1. The document defines pharmaceutical analysis as a branch of chemistry involving identification, determination, quantification, purification, and separation of substances or mixtures. It discusses various techniques used in pharmaceutical analysis.
2. Several applications of pharmaceutical analysis are discussed, including in pharmaceutical, food, and cosmetic industries as well as for disease diagnosis, geology, environmental science, and agriculture.
3. The document discusses different types of quantitative analysis including volumetric, gravimetric, gasometric, electrical, spectroscopic, thermal, separation, microbiological, and biological methods. It also discusses expressing concentration using terms like molarity, molality, normality, and others.
This document provides an overview of pharmaceutical analysis techniques. It discusses qualitative and quantitative analysis, various analytical methods including chemical, physical and biological methods. It describes different techniques for expressing concentration such as molarity, normality, percent solutions. It also discusses primary and secondary standards used for standardization of analytical methods and preparation of common standard solutions like hydrochloric acid, sodium hydroxide and sodium thiosulfate. The document aims to introduce fundamental concepts of pharmaceutical analysis.
This document discusses pharmaceutical analysis and errors. It begins by defining pharmaceutical analysis as methods for identification, quantitation, and purification of samples. It describes the scope of pharmaceutical analysis, which includes identifying and analyzing active pharmaceutical ingredients, determining drug stability and efficacy, and mixture analysis. Various techniques of analysis are also discussed, including qualitative and quantitative methods, as well as volumetric, gravimetric, electrochemical, instrumental, and biological techniques. Methods for expressing concentration like molarity, normality, and percentage are also defined. The document concludes by discussing primary and secondary standards used in preparing standardized solutions.
This document discusses various precipitation titration methods involving silver ions (Ag+). It describes three main methods:
1) Mohr's method uses silver ions as the titrant and chromate ions as the indicator for titrating halide ions like chloride. Silver halide precipitates first, followed by silver chromate at the endpoint.
2) Volhard's method titrates silver ions with thiocyanate ions in acidic medium using ferric ions as the reddish-brown thiocyanate complex indicator.
3) Fajan's method, or indicator adsorption method, involves adsorption of anionic dye indicators onto the precipitated silver halide particles. The intense color change at the
This document describes the Schnoiger's oxygen flask method, also known as the oxygen flask combustion method, for identifying halogens produced by combusting organic compounds. The method involves combusting samples containing halogens, like iodine, fluorine, chlorine, bromine or sulfur, in an oxygen-filled flask. The inorganic products produced are soluble in water. Halogens are then determined by titration. The method can be used to determine halogens, sulfur, phosphorus and other elements in medicines, organic compounds, polymers, coal and soil samples.
Different Techniques of Pharmaceutical AnalysisSapan Shah
The document discusses different techniques of analytical chemistry. It defines analytical chemistry as applying processes to identify, quantify, or determine the structure of substances or chemical compounds. The document outlines various types of analytical chemistry based on sample size, including macro, meso, micro, submicro, and ultramicro analysis. It also distinguishes between qualitative analysis, which provides information on species or functional groups, and quantitative analysis, which determines the relative amount of analytes numerically. Several analytical methods are described such as chemical, physicochemical, microbiological, and biological methods. The document emphasizes the importance of pharmaceutical analysis for identification, determination of impurities, drug stability, strength, concentration, and structure elucidation.
This document discusses various analytical methods used in pharmaceutical analysis including titration, spectroscopy, chromatography, and calibrations. Titration methods covered include acid-base, redox, complexometric, and potentiometric titrations. Spectroscopy techniques discussed are UV-visible spectroscopy, infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectroscopy. Chromatography methods covered are paper chromatography, gas chromatography, liquid chromatography, and high performance liquid chromatography. The document also discusses good manufacturing practices, quality assurance, quality control, and the importance of pharmaceutical analysis.
This document discusses acid-base titration and indicators. It defines acid-base titration as a quantitative analysis that involves neutralizing an acid or base of unknown concentration with an acid or base of known concentration. The equivalence point occurs when the titrant has exactly neutralized the analyte and allows calculating the concentration of the unknown acid or base. It also describes the Ostwald and quinonoid theories for how acid-base indicators work by changing color depending on their state of ionization or structural form under acidic or basic conditions.
Limt test Pharmaceutical Inorganic chemistry UNIT-I (Part-III) Limit Test.
Limit tests:- Factors affecting limit tests:
Specificity of the tests
Sensitivity
Control of personal errors (Analyst errors)
Test in which there is no visible reaction
Comparison methods
Quantitative determination
Limit test for Chloride: Principle, Procedure, observation and result.
Limit test for Sulphate: Principle, Procedure, observation and result
Limit test for Iron: Principle, Procedure, observation and result.
Limit test for Heavy metal: Principle, Procedure, observation and result.
Limit test for Lead: Principle, Procedure, observation and result.
Limit test for Arsenic: Principle, Gutzet test Procedure, detail in Gutzet Apparatus. observation and result.
Modifies Limit test for Chloride: Principle, Procedure, observation and result.
Modified Limit test for sulphate: Principle, Procedure, observation and result.
This document provides an overview of pharmaceutical analysis techniques. It discusses qualitative and quantitative analysis, various analytical methods including chemical, physical and biological methods. It describes different techniques for expressing concentration such as molarity, normality, percent solutions. It also discusses primary and secondary standards used for standardization of analytical methods and preparation of common standard solutions like hydrochloric acid, sodium hydroxide and sodium thiosulfate. The document aims to introduce fundamental concepts of pharmaceutical analysis.
This document discusses pharmaceutical analysis and errors. It begins by defining pharmaceutical analysis as methods for identification, quantitation, and purification of samples. It describes the scope of pharmaceutical analysis, which includes identifying and analyzing active pharmaceutical ingredients, determining drug stability and efficacy, and mixture analysis. Various techniques of analysis are also discussed, including qualitative and quantitative methods, as well as volumetric, gravimetric, electrochemical, instrumental, and biological techniques. Methods for expressing concentration like molarity, normality, and percentage are also defined. The document concludes by discussing primary and secondary standards used in preparing standardized solutions.
This document discusses various precipitation titration methods involving silver ions (Ag+). It describes three main methods:
1) Mohr's method uses silver ions as the titrant and chromate ions as the indicator for titrating halide ions like chloride. Silver halide precipitates first, followed by silver chromate at the endpoint.
2) Volhard's method titrates silver ions with thiocyanate ions in acidic medium using ferric ions as the reddish-brown thiocyanate complex indicator.
3) Fajan's method, or indicator adsorption method, involves adsorption of anionic dye indicators onto the precipitated silver halide particles. The intense color change at the
This document describes the Schnoiger's oxygen flask method, also known as the oxygen flask combustion method, for identifying halogens produced by combusting organic compounds. The method involves combusting samples containing halogens, like iodine, fluorine, chlorine, bromine or sulfur, in an oxygen-filled flask. The inorganic products produced are soluble in water. Halogens are then determined by titration. The method can be used to determine halogens, sulfur, phosphorus and other elements in medicines, organic compounds, polymers, coal and soil samples.
Different Techniques of Pharmaceutical AnalysisSapan Shah
The document discusses different techniques of analytical chemistry. It defines analytical chemistry as applying processes to identify, quantify, or determine the structure of substances or chemical compounds. The document outlines various types of analytical chemistry based on sample size, including macro, meso, micro, submicro, and ultramicro analysis. It also distinguishes between qualitative analysis, which provides information on species or functional groups, and quantitative analysis, which determines the relative amount of analytes numerically. Several analytical methods are described such as chemical, physicochemical, microbiological, and biological methods. The document emphasizes the importance of pharmaceutical analysis for identification, determination of impurities, drug stability, strength, concentration, and structure elucidation.
This document discusses various analytical methods used in pharmaceutical analysis including titration, spectroscopy, chromatography, and calibrations. Titration methods covered include acid-base, redox, complexometric, and potentiometric titrations. Spectroscopy techniques discussed are UV-visible spectroscopy, infrared spectroscopy, nuclear magnetic resonance spectroscopy, and mass spectroscopy. Chromatography methods covered are paper chromatography, gas chromatography, liquid chromatography, and high performance liquid chromatography. The document also discusses good manufacturing practices, quality assurance, quality control, and the importance of pharmaceutical analysis.
This document discusses acid-base titration and indicators. It defines acid-base titration as a quantitative analysis that involves neutralizing an acid or base of unknown concentration with an acid or base of known concentration. The equivalence point occurs when the titrant has exactly neutralized the analyte and allows calculating the concentration of the unknown acid or base. It also describes the Ostwald and quinonoid theories for how acid-base indicators work by changing color depending on their state of ionization or structural form under acidic or basic conditions.
Limt test Pharmaceutical Inorganic chemistry UNIT-I (Part-III) Limit Test.
Limit tests:- Factors affecting limit tests:
Specificity of the tests
Sensitivity
Control of personal errors (Analyst errors)
Test in which there is no visible reaction
Comparison methods
Quantitative determination
Limit test for Chloride: Principle, Procedure, observation and result.
Limit test for Sulphate: Principle, Procedure, observation and result
Limit test for Iron: Principle, Procedure, observation and result.
Limit test for Heavy metal: Principle, Procedure, observation and result.
Limit test for Lead: Principle, Procedure, observation and result.
Limit test for Arsenic: Principle, Gutzet test Procedure, detail in Gutzet Apparatus. observation and result.
Modifies Limit test for Chloride: Principle, Procedure, observation and result.
Modified Limit test for sulphate: Principle, Procedure, observation and result.
1) The document describes acid-base titration techniques, including defining terms like equivalence point and end point.
2) It discusses different types of titrations including strong acid-strong base, weak acid-strong base, and constructing titration curves.
3) Key points are made about calculating pH values before, at, and after the equivalence point for different titration scenarios. The document provides examples of constructing titration curves step-by-step.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Redox titration is a laboratory method to determine the concentration of an analyte by causing a redox reaction between a titrant and analyte. In redox titration, the titrant is prepared as a standard solution and acts as an oxidizing or reducing agent. It reacts with the analyte until the equivalence point is reached. The endpoint is detected using indicators or sensors that change color upon fully reacting with the analyte. Redox titration has various applications in fields like agriculture, water quality testing, and hydrometallurgy to analyze inorganic compounds. It provides methods for drug formulation and standardization of materials in drug synthesis.
This document describes the limit test for iron according to the Indian Pharmacopoeia. The test involves comparing the color produced by reacting a sample with thioglycolic acid in an ammonical citrate buffer to the color produced by a standard iron solution under the same conditions. If the color produced by the sample is less than the standard, it passes the limit test for iron. If the color is greater than the standard, it fails the limit test. The test is sensitive and uses citric acid to eliminate interference from other metal cations.
Volumetric Analysis
Types of titration
Acid- Base Theory
Reaction, End Point & Indicators
Acid- Base titration
Titration curve
Non- Aqueous Titration
Precipitation Titration
Complexometric Titration
Oxidation- Reduction Titration,
Calculation. Errors
General Informations,
Introduction of pharmaceutical analysis and their scoperamtripathi16
Pharmaceutical analysis involves identifying, quantifying, and purifying chemical substances and components in mixtures. There are two main types: qualitative analysis, which identifies whether a substance is present; and quantitative analysis, which determines the amount of a substance present. Common analytical techniques include volumetric analysis like titrations, electrochemical methods, spectroscopy, and chromatography. Pharmaceutical analysis is used in industries like pharmaceuticals, food, cosmetics, and for disease diagnosis to ensure quality, purity, safety and accurate diagnosis.
This document discusses acid-base titration and theories of acids and bases. It introduces acid-base titration as involving the neutralization reaction between an acid and base. Three theories of acids and bases are described: Arrhenius acid-base theory defines acids as producing H+ ions and bases as producing OH- ions. Bronsted-Lowry proton theory defines acids as proton donors and bases as proton acceptors. Lewis electron theory defines acids as electron pair acceptors and bases as electron pair donors. The document also discusses acid-base indicators and their use in determining the endpoint of a titration, as well as Ostwald and resonance theories of indicators.
Volumetric analysis is a quantitative method to determine the concentration of an unknown substance by measuring the volume of a standard solution required for a complete chemical reaction. It involves titrating a solution of known concentration against the analyte until the endpoint is reached, as indicated by an indicator. This allows the concentration of the analyte to be calculated. The document discusses the different types of volumetric titrations including acid-base, redox, precipitation and complexometric titrations. It also covers key concepts such as standard solutions, titration curves, and methods to determine the endpoint of the reaction.
Introduction to Pharmaceutical Analysis.pptxAkilMahmud2
The document provides an introduction to pharmaceutical analysis, including:
- Pharmaceutical analysis involves identification, determination, quantitation, and purification of chemical compounds from mixtures.
- Analytical methods include classical techniques like titrimetry and instrumental methods like chromatography and spectroscopy.
- Factors like sample properties, required precision/accuracy, and available facilities determine the suitable analytical method.
- Titrimetry involves quantitative determination of a sample by reacting it with a standard solution until an endpoint is reached.
Preparation and Evaluation of Aspirin tabletsSanket Kapadne
PREPARATION AND EVALUATION OF ASPIRIN TABLETS
Aim - Preparation and Evaluation of Aspirin Tablets.
Requirement –
Chemicals - Aspirin, HPMC, PVP, Sodium
Stearate, Talc
Glasswares - Granulating sieve, standard sieve set, etc.
Equipment - Tablet press
Principle
Aspirin tablet is prepared by wet granulation method. Aspirin belonging to the class of NSAID having analgesic, antipyretic, anti-inflammatory and antiplatelet activity at systematic standard doses. In this Lubricants in combination leads to better drug release kinetic. Aspirin tablets are obtained by wet Compression Method. The particles to be compressed consist of one or more medicaments, with or without excipients substance such as diluents, binders, and disintegration agents, lubricant, glidants.
Formula
Sr. No. Ingredients Quantity (1 Tab.)
1. Aspirin 250 mg
2. HPMC 50 mg
3. Microcrystalline Cellulose 70 mg
4. Polyvinyl Pyrrolidone Q.S.
5. Sodium Stearate+ Talc 1 mg + 5 mg
Method
Wet granulation forms the granulation by binding the powders together with an adheshive instead of by compaction.
Stages of granule development :
A. Pendular B. Funicular
C. Capillary D. Droplet Steps involved :
Step 1: Weighing and mixing of formulation ingredients.
Step 2: Preparing the damp mass.
Step 3: Screening the dampened powder into pellets or granules.
Step 4: Drying of moist granules.
Procedure
1. Tablets were prepared using wet granulation technique as per the composition given earlier.
2. The calculated amount which was required to prepare 400 mg aspirin tablets, containing 250 mg drug, HPMC polymer and PVP as a binder were mixed uniformly.
3. An enough granulating agent (water) was added slowly to prepare wet mass. Granules were prepared by sieving method using a 20# sieve.
4. Further, granules were dried at 35-45ºC for six hours. The dried granules were stored in desiccators until compression of tablets.
5.The required amounts of granules were weighed and compressed using automatically operated tablet punching machine having 12mm flat faced punch diameter and during the tablet preparation to maintain the low resistance between the solid and die wall, lubricants added in granules. Lubricant combinations are agents added in small quantities to the tablet during the tablet preparation.
6. The compressed tablets were stored in airtight container at room temperature for further evaluation.
Evaluation
1. Assay : Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about 0.5 g of Aspirin, add 30.0 ml of 0.5M sodium hydroxide, boil gently for 10 minutes, cool and titrate the excess of alkali with 0.5 M hydrochloric acid using phenol red solution as indicator. Repeat the operation without the substance under examination. The difference
This document describes the limit test for arsenic using the Gutzeit method. Arsenic in a sample is converted to arsine gas, which reacts with mercuric chloride paper to produce a stain that is compared to a standard stain. The test uses an apparatus with two glass tubes, where the sample is placed below zinc and hydrochloric acid to produce arsine gas, which passes through mercuric chloride paper to produce a stain after 40 minutes. By comparing the intensity of this test stain to the standard stain produced in the same way from a solution of known arsenic concentration, the document determines if the sample passes or fails the limit test for arsenic.
This document discusses non-aqueous titration including reasons for using non-aqueous solvents, common solvent types, and examples of acidimetry and alkalimetry titrations. Protogenic, protophilic, and aprotic solvents are described. Acidimetry involves titrating weak bases like ephedrine HCl with perchloric acid in glacial acetic acid. Alkalimetry involves titrating weak acids like sodium benzoate with sodium methoxide in DMF. The document provides procedures for standardizing a perchloric acid solution and estimating the percentage of ephedrine HCl and sodium benzoate in samples.
This document describes the Gutzeit test for detecting arsenic. The test works by first converting any arsenic in a sample into arsenious acid, then reducing it to arsine gas. Mercuric chloride paper placed in the apparatus will turn yellow if arsine gas is present, indicating the presence of arsenic in the original sample. The document provides details of the test apparatus, reagents used, procedure, and precautions to get accurate results and avoid contamination.
Pharmaceutical suspension can be classified based on the dispersed phase, vehicle used, proportion of solid particles, particle size, etc. They can be stabilized using suspending agents, viscosity increasing agents, surface charge, etc. Recent advances include nano suspensions to improve solubility, taste masked suspensions to improve palatability, and sustained release suspensions to reduce dosing frequency. Evaluation methods include sedimentation studies, rheological measurements, and zeta potential determination.
Complexometric TITRATION FOR PG IST SEM prakash64742
This document discusses complexometric titration, which involves titrating a metal ion with a complexing agent or chelating agent. It provides examples of different types of complexometric titrations including direct titration, back titration, and replacement titration. Assays for several substances using complexometric titration methods are described, such as magnesium sulfate using EDTA as the titrant, and calcium carbonate where the carbonate is dissolved using acid prior to titration.
This document discusses precipitation titration methods. It describes Mohr's method, Volhard's method and Fajan's method. Mohr's method uses potassium chromate as an indicator. Volhard's method indirectly titrates excess silver ions with thiocyanate using ferric ammonium sulfate as an indicator. Fajan's method uses adsorption indicators like fluorescein that change color upon adsorption to the precipitate formed at the endpoint. Key factors that influence precipitation titrations like solubility products, common ion effect and temperature are also discussed.
The document discusses two options for describing limits of Class 2 solvents such as acetonitrile in pharmaceutical products. Option 1 uses set concentration limits from guidelines that are acceptable if the daily dose is below 10g. Option 2 involves calculating the total daily exposure of a solvent by summing the amounts from all components, which must be below the permitted daily exposure level. An example shows how the limits are calculated and applied to determine if a product meets the requirements.
PA 1.pptx introduction to Pharmaceutical AnalysispriyankaRamugade
pharmaceutical analysis -
Pharmaceutical analysis is branch of practical chemistry deals with identification,determination,quantification,and purification of substances
pharmaceutical analysis devided into two types i.e.
1)Qualitative analysis
2)Quantitative Analysis
pharmaceutical analysis have various methods
1) Chemical method
2)Electrical method
3)Instrumental method
4)Biological method
Introduction to Error-Error is define as mistake
errors are categorized into two parts i.e.Absolute error and relative error
Absolute error is the difference between experimental mean value and true value
Relative errors is
This document discusses various concepts related to pharmaceutical analysis including assay, analyte, titrant, titration, equivalence point, and standardization. It defines assay as a qualitative or quantitative assessment of an analyte using a titrant. Titration involves measuring the volume of titrant used to reach the equivalence point, as indicated by a color change from an indicator. The document also discusses different types of quantitative analysis techniques including volumetric (titrimetric), gravimetric, gasometric, and instrumental methods. It provides examples of concentration units used in pharmaceutical analysis such as molarity, molality, and normality.
1) The document describes acid-base titration techniques, including defining terms like equivalence point and end point.
2) It discusses different types of titrations including strong acid-strong base, weak acid-strong base, and constructing titration curves.
3) Key points are made about calculating pH values before, at, and after the equivalence point for different titration scenarios. The document provides examples of constructing titration curves step-by-step.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
Redox titration is a laboratory method to determine the concentration of an analyte by causing a redox reaction between a titrant and analyte. In redox titration, the titrant is prepared as a standard solution and acts as an oxidizing or reducing agent. It reacts with the analyte until the equivalence point is reached. The endpoint is detected using indicators or sensors that change color upon fully reacting with the analyte. Redox titration has various applications in fields like agriculture, water quality testing, and hydrometallurgy to analyze inorganic compounds. It provides methods for drug formulation and standardization of materials in drug synthesis.
This document describes the limit test for iron according to the Indian Pharmacopoeia. The test involves comparing the color produced by reacting a sample with thioglycolic acid in an ammonical citrate buffer to the color produced by a standard iron solution under the same conditions. If the color produced by the sample is less than the standard, it passes the limit test for iron. If the color is greater than the standard, it fails the limit test. The test is sensitive and uses citric acid to eliminate interference from other metal cations.
Volumetric Analysis
Types of titration
Acid- Base Theory
Reaction, End Point & Indicators
Acid- Base titration
Titration curve
Non- Aqueous Titration
Precipitation Titration
Complexometric Titration
Oxidation- Reduction Titration,
Calculation. Errors
General Informations,
Introduction of pharmaceutical analysis and their scoperamtripathi16
Pharmaceutical analysis involves identifying, quantifying, and purifying chemical substances and components in mixtures. There are two main types: qualitative analysis, which identifies whether a substance is present; and quantitative analysis, which determines the amount of a substance present. Common analytical techniques include volumetric analysis like titrations, electrochemical methods, spectroscopy, and chromatography. Pharmaceutical analysis is used in industries like pharmaceuticals, food, cosmetics, and for disease diagnosis to ensure quality, purity, safety and accurate diagnosis.
This document discusses acid-base titration and theories of acids and bases. It introduces acid-base titration as involving the neutralization reaction between an acid and base. Three theories of acids and bases are described: Arrhenius acid-base theory defines acids as producing H+ ions and bases as producing OH- ions. Bronsted-Lowry proton theory defines acids as proton donors and bases as proton acceptors. Lewis electron theory defines acids as electron pair acceptors and bases as electron pair donors. The document also discusses acid-base indicators and their use in determining the endpoint of a titration, as well as Ostwald and resonance theories of indicators.
Volumetric analysis is a quantitative method to determine the concentration of an unknown substance by measuring the volume of a standard solution required for a complete chemical reaction. It involves titrating a solution of known concentration against the analyte until the endpoint is reached, as indicated by an indicator. This allows the concentration of the analyte to be calculated. The document discusses the different types of volumetric titrations including acid-base, redox, precipitation and complexometric titrations. It also covers key concepts such as standard solutions, titration curves, and methods to determine the endpoint of the reaction.
Introduction to Pharmaceutical Analysis.pptxAkilMahmud2
The document provides an introduction to pharmaceutical analysis, including:
- Pharmaceutical analysis involves identification, determination, quantitation, and purification of chemical compounds from mixtures.
- Analytical methods include classical techniques like titrimetry and instrumental methods like chromatography and spectroscopy.
- Factors like sample properties, required precision/accuracy, and available facilities determine the suitable analytical method.
- Titrimetry involves quantitative determination of a sample by reacting it with a standard solution until an endpoint is reached.
Preparation and Evaluation of Aspirin tabletsSanket Kapadne
PREPARATION AND EVALUATION OF ASPIRIN TABLETS
Aim - Preparation and Evaluation of Aspirin Tablets.
Requirement –
Chemicals - Aspirin, HPMC, PVP, Sodium
Stearate, Talc
Glasswares - Granulating sieve, standard sieve set, etc.
Equipment - Tablet press
Principle
Aspirin tablet is prepared by wet granulation method. Aspirin belonging to the class of NSAID having analgesic, antipyretic, anti-inflammatory and antiplatelet activity at systematic standard doses. In this Lubricants in combination leads to better drug release kinetic. Aspirin tablets are obtained by wet Compression Method. The particles to be compressed consist of one or more medicaments, with or without excipients substance such as diluents, binders, and disintegration agents, lubricant, glidants.
Formula
Sr. No. Ingredients Quantity (1 Tab.)
1. Aspirin 250 mg
2. HPMC 50 mg
3. Microcrystalline Cellulose 70 mg
4. Polyvinyl Pyrrolidone Q.S.
5. Sodium Stearate+ Talc 1 mg + 5 mg
Method
Wet granulation forms the granulation by binding the powders together with an adheshive instead of by compaction.
Stages of granule development :
A. Pendular B. Funicular
C. Capillary D. Droplet Steps involved :
Step 1: Weighing and mixing of formulation ingredients.
Step 2: Preparing the damp mass.
Step 3: Screening the dampened powder into pellets or granules.
Step 4: Drying of moist granules.
Procedure
1. Tablets were prepared using wet granulation technique as per the composition given earlier.
2. The calculated amount which was required to prepare 400 mg aspirin tablets, containing 250 mg drug, HPMC polymer and PVP as a binder were mixed uniformly.
3. An enough granulating agent (water) was added slowly to prepare wet mass. Granules were prepared by sieving method using a 20# sieve.
4. Further, granules were dried at 35-45ºC for six hours. The dried granules were stored in desiccators until compression of tablets.
5.The required amounts of granules were weighed and compressed using automatically operated tablet punching machine having 12mm flat faced punch diameter and during the tablet preparation to maintain the low resistance between the solid and die wall, lubricants added in granules. Lubricant combinations are agents added in small quantities to the tablet during the tablet preparation.
6. The compressed tablets were stored in airtight container at room temperature for further evaluation.
Evaluation
1. Assay : Weigh and powder 20 tablets. Weigh accurately a quantity of the powder containing about 0.5 g of Aspirin, add 30.0 ml of 0.5M sodium hydroxide, boil gently for 10 minutes, cool and titrate the excess of alkali with 0.5 M hydrochloric acid using phenol red solution as indicator. Repeat the operation without the substance under examination. The difference
This document describes the limit test for arsenic using the Gutzeit method. Arsenic in a sample is converted to arsine gas, which reacts with mercuric chloride paper to produce a stain that is compared to a standard stain. The test uses an apparatus with two glass tubes, where the sample is placed below zinc and hydrochloric acid to produce arsine gas, which passes through mercuric chloride paper to produce a stain after 40 minutes. By comparing the intensity of this test stain to the standard stain produced in the same way from a solution of known arsenic concentration, the document determines if the sample passes or fails the limit test for arsenic.
This document discusses non-aqueous titration including reasons for using non-aqueous solvents, common solvent types, and examples of acidimetry and alkalimetry titrations. Protogenic, protophilic, and aprotic solvents are described. Acidimetry involves titrating weak bases like ephedrine HCl with perchloric acid in glacial acetic acid. Alkalimetry involves titrating weak acids like sodium benzoate with sodium methoxide in DMF. The document provides procedures for standardizing a perchloric acid solution and estimating the percentage of ephedrine HCl and sodium benzoate in samples.
This document describes the Gutzeit test for detecting arsenic. The test works by first converting any arsenic in a sample into arsenious acid, then reducing it to arsine gas. Mercuric chloride paper placed in the apparatus will turn yellow if arsine gas is present, indicating the presence of arsenic in the original sample. The document provides details of the test apparatus, reagents used, procedure, and precautions to get accurate results and avoid contamination.
Pharmaceutical suspension can be classified based on the dispersed phase, vehicle used, proportion of solid particles, particle size, etc. They can be stabilized using suspending agents, viscosity increasing agents, surface charge, etc. Recent advances include nano suspensions to improve solubility, taste masked suspensions to improve palatability, and sustained release suspensions to reduce dosing frequency. Evaluation methods include sedimentation studies, rheological measurements, and zeta potential determination.
Complexometric TITRATION FOR PG IST SEM prakash64742
This document discusses complexometric titration, which involves titrating a metal ion with a complexing agent or chelating agent. It provides examples of different types of complexometric titrations including direct titration, back titration, and replacement titration. Assays for several substances using complexometric titration methods are described, such as magnesium sulfate using EDTA as the titrant, and calcium carbonate where the carbonate is dissolved using acid prior to titration.
This document discusses precipitation titration methods. It describes Mohr's method, Volhard's method and Fajan's method. Mohr's method uses potassium chromate as an indicator. Volhard's method indirectly titrates excess silver ions with thiocyanate using ferric ammonium sulfate as an indicator. Fajan's method uses adsorption indicators like fluorescein that change color upon adsorption to the precipitate formed at the endpoint. Key factors that influence precipitation titrations like solubility products, common ion effect and temperature are also discussed.
The document discusses two options for describing limits of Class 2 solvents such as acetonitrile in pharmaceutical products. Option 1 uses set concentration limits from guidelines that are acceptable if the daily dose is below 10g. Option 2 involves calculating the total daily exposure of a solvent by summing the amounts from all components, which must be below the permitted daily exposure level. An example shows how the limits are calculated and applied to determine if a product meets the requirements.
PA 1.pptx introduction to Pharmaceutical AnalysispriyankaRamugade
pharmaceutical analysis -
Pharmaceutical analysis is branch of practical chemistry deals with identification,determination,quantification,and purification of substances
pharmaceutical analysis devided into two types i.e.
1)Qualitative analysis
2)Quantitative Analysis
pharmaceutical analysis have various methods
1) Chemical method
2)Electrical method
3)Instrumental method
4)Biological method
Introduction to Error-Error is define as mistake
errors are categorized into two parts i.e.Absolute error and relative error
Absolute error is the difference between experimental mean value and true value
Relative errors is
This document discusses various concepts related to pharmaceutical analysis including assay, analyte, titrant, titration, equivalence point, and standardization. It defines assay as a qualitative or quantitative assessment of an analyte using a titrant. Titration involves measuring the volume of titrant used to reach the equivalence point, as indicated by a color change from an indicator. The document also discusses different types of quantitative analysis techniques including volumetric (titrimetric), gravimetric, gasometric, and instrumental methods. It provides examples of concentration units used in pharmaceutical analysis such as molarity, molality, and normality.
Introduction of Pharmaceutical Analysis.pdfKeval80
The document provides an introduction to pharmaceutical analysis, discussing topics like volumetric analysis, the scope of pharmaceutical analysis, classification of quantitative analysis methods, and sources of error. Primary standards like benzoic acid and secondary standards prepared in the lab are used to standardize solutions. Various methods like titration, spectroscopy, and chromatography are used in pharmaceutical analysis.
This document outlines the topics to be covered in a chemistry course, including analytical chemistry concepts and methods. It will introduce fundamental analytical vocabulary, qualitative and quantitative analysis techniques, and methods for evaluating analytical data. Specific topics include different concentration expressions, principles of qualitative analysis involving solubility and pH, and the types of errors that can occur during analysis. The course will provide numerical problems to reinforce these analytical chemistry concepts.
Mrs. Poonam Sunil Aher discusses different analytical techniques including quantitative methods like solubility, melting point, and boiling point as well as qualitative methods like color, odor, and identification tests. She focuses on titrimetric techniques like acid-base titration using indicators, redox titration, iodimetry titration using starch, and precipitation titration. She also covers gravimetric analysis techniques like volatilization and precipitation, and discusses aqueous versus non-aqueous titration.
This document provides an overview of analytical chemistry chapter 24. It discusses classical combustion analysis methods for determining empirical and molecular formulas. Combustion analysis involves burning a sample and collecting and measuring the CO2 and H2O products. The masses of C, H, and O in the sample can be calculated from these measurements. Modern spectroscopy methods are also covered, including infrared spectroscopy, UV-visible spectroscopy, NMR spectroscopy, atomic emission spectroscopy, atomic absorption spectroscopy, and mass spectrometry. These techniques analyze electromagnetic radiation absorbed or emitted by molecules to determine their structure.
Conventional methods of quantitative analysisHimanshu Saxena
1) Analytical chemistry deals with methods for identification, structural determination, quantification, qualitative analysis, and separation of molecules and mixtures.
2) Quantitative analysis provides numerical information on the exact amount or concentration of an analyte and can be done through volumetric or gravimetric methods.
3) Volumetric analysis involves titrating a solution of known volume and concentration (titrant) with an analyte until the endpoint of the reaction is reached to determine the unknown concentration. Gravimetric analysis involves precipitating, filtering, drying, and weighing an analyte to obtain its mass concentration.
Chemistry can be classified into general chemistry, analytical chemistry, physical chemistry, organic chemistry, inorganic chemistry, and biochemistry. Analytical chemistry involves the separation, identification, and quantification of substances in a sample. It can be divided into classical and instrumental analysis, with classical analysis including solid tests, wet tests, volumetric analysis, and gravimetric analysis. Volumetric analysis determines unknown concentrations by titrating a solution with a standard solution until an indicator shows the reaction is complete.
Pharmaceutical analysis involves analytical procedures to determine the purity, safety, and quality of drugs and chemicals. It is a branch of practical chemistry that identifies, quantifies, and purifies substances or separates mixtures. The objectives of the pharmaceutical analysis course are to understand principles of volumetric and electrochemical analysis and develop analytical skills. The course covers topics like sources of errors, primary and secondary standards, acid-base titrations, precipitation titrations, complexometric titration, and electrochemical methods of analysis. Pharmaceutical analysis is important for applications like quality control, clinical analysis, forensic analysis, and environmental analysis.
This document discusses quantitative analysis techniques used in pharmaceutical analytical chemistry. It describes three main types of quantitative analysis: volumetric (titration), gravimetric, and instrumental analysis. Titration is discussed in detail, including definitions of equivalence point and endpoint, types of titration reactions and methods, and requirements for primary standard substances and solutions used in titration. Equivalent weights and how they are calculated for different reaction types are also covered.
This document provides an overview of pharmaceutical analysis. It defines pharmaceutical analysis as involving processes to identify, quantify, and purify substances in mixtures. It then describes several common analytical techniques including titration, which involves reacting a sample with a solution of known concentration to determine the sample amount. The document outlines different types of analysis like qualitative to identify substances and quantitative to measure amounts. It also categorizes various instrumental and non-instrumental methods used in pharmaceutical analysis like titrimetry, gravimetry, spectroscopy, chromatography, and more. In closing, it discusses applications of analysis in manufacturing and research.
The document provides guidelines on standardizing herbal medicines according to WHO parameters. It discusses the need for standardization due to biological and geographical variations in herbal drugs. Various physical, chemical, biological and microscopic parameters are described for evaluating the identity, purity, quality and strength of herbal medicines. Parameters like ash value, extractive value, thin layer chromatography, chemical tests etc. are used to develop a chemical fingerprint of each herbal drug. The guidelines aim to promote the safe and effective use of herbal medicines.
This document provides an overview of analytical chemistry and instrumentation. It defines pharmaceutical chemistry and analytical chemistry. It discusses qualitative and quantitative analysis and describes common analytical instruments like pH meters, ORP meters, gas chromatographs, mass spectrometers, and spectrometers. It also outlines the analytical methodology and lists some applications of instrumental methods in fields like bioanalysis, environmental analysis, materials science, and forensic science.
Analytical Chemistry & Role in pharmaceutical industry
Different techniques of analysis
Significant Figures
Errors - Types & Minimization
Calibration of glasswares - pipette, burette & Volumetric flask
Pharmaceutical analysis involves techniques to identify, quantify, and purify substances as well as separate mixture components. [1] It uses qualitative and quantitative methods like chemical, physicochemical, microbiological, and biological analyses. [2] Common chemical techniques include volumetric (e.g., acid-base titration), gasometric, and gravimetric analysis. [3] Instrumental methods rely on measuring properties like electrical conductance and optical density. Microbiological analysis examines microbial growth inhibition. Biological analysis estimates potency using animal or tissue samples. Pharmaceutical analysis has applications in quality control, research, pollution monitoring, and more.
Pharmaceutical analysis involves techniques to identify, quantify, and purify chemical substances and separate mixtures. It can be qualitative, determining presence/absence, or quantitative, determining concentration. Techniques include chemical methods like volumetric titration, gasometry, and gravimetry. Physicochemical methods use instruments to detect changes in physical properties. Microbiological analysis tests antibiotic efficacy by microbial growth inhibition. Biological analysis estimates potency by comparing biological effects in tissues/animals to standards. Pharmaceutical analysis has applications in quality control/assurance, analytical research, environmental surveys, and pollution monitoring.
Introduction to Pharmaceutical analysis - I (HRB)Harshadaa bafna
This document discusses pharmaceutical analysis, which involves identifying, quantifying, and purifying substances and mixtures. It describes various analytical techniques like volumetric, electrochemical, spectroscopic, and chromatographic methods. It also discusses primary and secondary standards, methods of expressing concentration such as molarity and molality, sources of errors and how to minimize them, and pharmacopoeias which establish drug standards.
Quantitative method of analysis and instrumentation.pptxBharatKumarHumagai
Here are the key points about flame photometry:
Instrumentation:
- Flame photometer consists of an atomizer to convert the sample into an aerosol, a burner to produce a flame, an optical system to focus the light from the flame onto a photomultiplier tube, and an electronic circuit to amplify and measure the signal.
Principle:
- When an element is aspirated into the flame, electrons in the atoms get excited to higher energy levels. As they fall back to ground state, they emit light of characteristic wavelengths.
- Sodium emits yellow light at 589 nm, potassium emits violet light at 766.5 nm, lithium emits red light at
Asthma is a chronic inflammatory lung disease that causes narrowing of the airways. It affects over 300 million people worldwide. The hallmark symptoms of asthma include wheezing, coughing, chest tightness, and shortness of breath. Asthma is caused by a combination of genetic and environmental factors that lead to airway inflammation and constriction. Common triggers include allergens, viruses, exercise, and air pollution. Diagnosis involves lung function tests to measure airflow limitation and its improvement with bronchodilator medication. Treatment focuses on reducing symptoms with bronchodilators and preventing exacerbations with anti-inflammatory drugs like corticosteroids.
Asthma is a chronic disease characterized by inflammation of the airways causing coughing, wheezing, chest tightness, and difficulty breathing. It is usually caused by allergic triggers like pollen, dust mites, or animal dander that lead to bronchospasms and airway obstruction. Diagnosis involves patient history, physical exam, pulmonary function tests, and allergy testing. Treatment includes bronchodilators, corticosteroids, leukotriene modifiers, and monoclonal antibodies to reduce inflammation and prevent symptoms.
Ischaemic heart disease is caused by an imbalance between the heart's supply and demand for oxygenated blood, usually due to atherosclerosis narrowing the coronary arteries. The main symptoms are chest pain or discomfort known as angina. There are different types of angina that vary based on their triggers and patterns. Diagnosis involves tests like ECG, echocardiogram, stress tests and angiography. Treatment options include medications to reduce demands on the heart like nitrates, beta-blockers, and calcium channel blockers, as well as interventions like angioplasty, stents and bypass surgery.
Atherosclerosis is a disease where plaque builds up in the arteries. Over time, the plaque hardens and narrows the arteries, limiting blood flow. Risk factors include age, family history, smoking, high blood pressure, high cholesterol, diabetes, and obesity. Complications arise when blood flow is reduced to organs like the heart, brain, kidneys, and limbs, potentially causing heart attacks, strokes, chronic kidney disease, or poor circulation. Treatment focuses on lifestyle changes and medications to control risk factors and symptoms.
This document provides an outline for a lecture on hypertension. It begins with objectives to understand hypertension's etiology, risk factors, and complications. It then covers definitions of hypertension, classifications based on cause and clinical features, risk factors, pathogenesis, regulation of blood pressure, vascular changes in hypertension, and complications affecting the heart, blood vessels, kidneys, eyes, and brain. The lecture topics include primary and secondary causes, benign vs malignant hypertension, endocrine factors influencing blood pressure, and target organ damage.
Hypertension and its pathophysiology.pptxImtiyaz60
The document discusses hypertension and the heart. It provides details on:
- The structure and layers of the heart, including the myocardium and pericardium.
- The path of blood through the heart, from the vena cava and atria to the ventricles, valves, and out the aorta to the body.
- Additional details are given on heart size, location in the thoracic cavity, and the double-walled pericardium surrounding and protecting the heart.
This document discusses various appetite stimulants, digestants, and carminatives. It describes how appetite is influenced by several factors in the hypothalamus and gut-brain pathways. Common appetite stimulants mentioned include lemon pickles, bitter orange peel, and soups containing aromatic oils. Some medications can increase appetite but also have side effects. The document also discusses various digestive enzymes and bile acids that may aid digestion, though evidence for their efficacy is limited. Finally, it outlines several common carminative herbs and spices that can relieve gas and bloating.
Anti Ulcer drugs pharmacology and classificationImtiyaz60
This document summarizes drugs used to treat peptic ulcers. It discusses the anatomy and physiology of gastric acid secretion regulated by histamine, acetylcholine, and gastrin. It describes prostaglandins' protective role in the stomach and how H2 receptor blockers and proton pump inhibitors work to suppress acid secretion. H2 blockers competitively inhibit histamine receptors, while PPIs irreversibly inactivate the proton pump. Common medications discussed include cimetidine, ranitidine, famotidine, omeprazole, and lansoprazole. The goals of anti-ulcer therapy are relieving pain, promoting healing, and preventing complications and relapse.
Ginger and asafoetida are plants with medicinal properties. Ginger is native to Southeast Asia and cultivated in many tropical regions. It has buff-colored rhizomes with an aromatic odor and taste. Chemical constituents include volatile oils and phenolic compounds that give ginger its flavor and pharmacological effects. Asafoetida is an oleo-gum-resin obtained from Ferula plants. It occurs in tear or mass forms, has an intense odor, and chemical tests detect umbelliferone. Both ginger and asafoetida have traditional uses as carminatives, expectorants, and to treat conditions like nausea, flatulence, and asthma. They can be subject to adulteration
Leprosy is caused by Mycobacterium leprae. It primarily affects the skin and peripheral nerves, causing hypopigmented patches and thickening of nerves. There are two main forms - tuberculoid leprosy, which causes localized lesions, and lepromatous leprosy, which involves multiple organs. Diagnosis involves skin smears and biopsies to identify acid-fast bacilli. Treatment involves multidrug chemotherapy regimens containing dapsone, rifampicin, and clofazimine. Prevention focuses on contact tracing, chemoprophylaxis, isolation during reactions, and rehabilitation.
Tuberculosis (TB) is a chronic bacterial infection caused by Mycobacterium tuberculosis that typically forms granulomas in the lungs. It is treatable with a combination of anti-TB drugs over a 6-12 month period to kill both actively replicating and dormant bacilli. Diagnosis involves physical exam, chest x-ray, tuberculin skin test, and sputum culture. Risk factors include HIV infection, poverty, and crowded living conditions.
Stroke is the 5th leading cause of death in the US. There are three main types of stroke: ischemic, hemorrhagic, and transient ischemic attacks (TIAs). Ischemic strokes, which account for 85% of cases, occur when a blood clot blocks an artery supplying blood to the brain. Hemorrhagic strokes occur when a brain artery ruptures due to conditions like hypertension. TIAs are temporary and cause no permanent damage but indicate risk for future strokes. Symptoms of stroke appear suddenly and include face drooping, arm weakness, speech difficulties, and severe headache. Diagnostic tests help determine the type and location of stroke. Lifestyle changes and medical treatment can help prevent strokes.
The thyroid gland is located in the neck below the larynx. It produces thyroid hormones including thyroxine (T4) and triiodothyronine (T3) which increase metabolism in nearly every organ system. Iodine is necessary for thyroid hormone production. Disorders include hypothyroidism, where thyroid hormone production is inadequate, and hyperthyroidism, where production is excessive. Graves' disease is an autoimmune cause of hyperthyroidism. Cretinism results from untreated congenital hypothyroidism and causes severe physical and mental impairment.
Inflammatory bowel disease (IBD) represents a group of chronic disorders that cause prolonged inflammation of the digestive tract. The two main types are ulcerative colitis, which causes inflammation and ulcers in the lining of the large intestine, and Crohn's disease, which is a chronic inflammatory disease that can affect any part of the gastrointestinal tract from mouth to anus. IBD is treated through a combination of medications, dietary changes, and sometimes surgery, with the goals of inducing and maintaining remission of symptoms, preventing complications, and avoiding surgery if possible. Treatments include aminosalicylates, corticosteroids, immunosuppressants, biologics that target tumor necrosis factor, and antimicrobial agents.
Tannins are polyphenolic compounds found in many plants. They are classified as hydrolysable tannins, condensed tannins, or pseudo-tannins. Hydrolysable tannins are hydrolyzed by acids into gallic acid or ellagic acid, while condensed tannins are more resistant to hydrolysis. Tannins are extracted using mixtures of polar and non-polar solvents due to their high molecular weight. Identification tests for tannins include the gelatin test, Goldbeater's skin test, and reactions with ferrous sulfate or ferric chloride that produce colors. Pterocarpus marsupium, or Bijasal, is a plant source of k
This document discusses various drug classes used in the treatment of heart failure, including their mechanisms and effects. Diuretics reduce preload on the heart by reducing extracellular fluid volume through natriuresis. Vasodilators such as nitroglycerin and ACE inhibitors reduce preload and afterload by dilating blood vessels. Nesiritide is a natriuretic peptide that causes vasodilation and natriuresis. β-blockers improve outcomes in heart failure by inhibiting the deleterious effects of sympathetic activation on the heart.
Tuberculosis (TB) is a bacterial infection caused by Mycobacterium tuberculosis that most commonly infects the lungs. It can be treated with antibiotics. TB is spread through airborne droplets when an infected person coughs or sneezes. While latent TB means the immune system has contained the infection and the person is not infectious, active TB means the person is sick and can spread the disease. Standard TB treatment involves a combination of antibiotics like isoniazid, rifampin and ethambutol over a period of 6-9 months.
The document discusses infectious diseases and infectious agents. It covers host barriers to infection like the skin, respiratory system, gastrointestinal tract, and urogenital tract. It describes how these barriers can fail and allow infection. It also discusses the different classes of infectious agents including bacteria, viruses, fungi and parasites. The document outlines the different types of inflammatory responses infections can cause like suppurative inflammation, granulomatous inflammation, and cytopathic responses. It covers how microbes can evade the immune system and the various ways infections can be transmitted.
The document defines key terms related to the electrophysiology of the heart such as action potential, membrane potential, refractory period, and threshold potential. It then describes the four phases of the cardiac action potential: Phase 0 involves stimulation and sodium/calcium influx causing depolarization; Phase 1 involves partial repolarization through ion efflux; Phase 2 involves a plateau phase through continued ion fluxes; Phase 3 involves full repolarization through ion efflux slower than depolarization. Phase 4 is the interval between repolarizations. The cardiac action potential triggers mechanical contraction. An electrocardiogram detects and records the summed action potentials to analyze patterns like the P, QRS, and T waves related to atrial depolarization, ventricular depolarization
These simplified slides by Dr. Sidra Arshad present an overview of the non-respiratory functions of the respiratory tract.
Learning objectives:
1. Enlist the non-respiratory functions of the respiratory tract
2. Briefly explain how these functions are carried out
3. Discuss the significance of dead space
4. Differentiate between minute ventilation and alveolar ventilation
5. Describe the cough and sneeze reflexes
Study Resources:
1. Chapter 39, Guyton and Hall Textbook of Medical Physiology, 14th edition
2. Chapter 34, Ganong’s Review of Medical Physiology, 26th edition
3. Chapter 17, Human Physiology by Lauralee Sherwood, 9th edition
4. Non-respiratory functions of the lungs https://academic.oup.com/bjaed/article/13/3/98/278874
NVBDCP.pptx Nation vector borne disease control programSapna Thakur
NVBDCP was launched in 2003-2004 . Vector-Borne Disease: Disease that results from an infection transmitted to humans and other animals by blood-feeding arthropods, such as mosquitoes, ticks, and fleas. Examples of vector-borne diseases include Dengue fever, West Nile Virus, Lyme disease, and malaria.
Adhd Medication Shortage Uk - trinexpharmacy.comreignlana06
The UK is currently facing a Adhd Medication Shortage Uk, which has left many patients and their families grappling with uncertainty and frustration. ADHD, or Attention Deficit Hyperactivity Disorder, is a chronic condition that requires consistent medication to manage effectively. This shortage has highlighted the critical role these medications play in the daily lives of those affected by ADHD. Contact : +1 (747) 209 – 3649 E-mail : sales@trinexpharmacy.com
Basavarajeeyam is an important text for ayurvedic physician belonging to andhra pradehs. It is a popular compendium in various parts of our country as well as in andhra pradesh. The content of the text was presented in sanskrit and telugu language (Bilingual). One of the most famous book in ayurvedic pharmaceutics and therapeutics. This book contains 25 chapters called as prakaranas. Many rasaoushadis were explained, pioneer of dhatu druti, nadi pareeksha, mutra pareeksha etc. Belongs to the period of 15-16 century. New diseases like upadamsha, phiranga rogas are explained.
micro teaching on communication m.sc nursing.pdfAnurag Sharma
Microteaching is a unique model of practice teaching. It is a viable instrument for the. desired change in the teaching behavior or the behavior potential which, in specified types of real. classroom situations, tends to facilitate the achievement of specified types of objectives.
Ozempic: Preoperative Management of Patients on GLP-1 Receptor Agonists Saeid Safari
Preoperative Management of Patients on GLP-1 Receptor Agonists like Ozempic and Semiglutide
ASA GUIDELINE
NYSORA Guideline
2 Case Reports of Gastric Ultrasound
Rasamanikya is a excellent preparation in the field of Rasashastra, it is used in various Kushtha Roga, Shwasa, Vicharchika, Bhagandara, Vatarakta, and Phiranga Roga. In this article Preparation& Comparative analytical profile for both Formulationon i.e Rasamanikya prepared by Kushmanda swarasa & Churnodhaka Shodita Haratala. The study aims to provide insights into the comparative efficacy and analytical aspects of these formulations for enhanced therapeutic outcomes.
Recomendações da OMS sobre cuidados maternos e neonatais para uma experiência pós-natal positiva.
Em consonância com os ODS – Objetivos do Desenvolvimento Sustentável e a Estratégia Global para a Saúde das Mulheres, Crianças e Adolescentes, e aplicando uma abordagem baseada nos direitos humanos, os esforços de cuidados pós-natais devem expandir-se para além da cobertura e da simples sobrevivência, de modo a incluir cuidados de qualidade.
Estas diretrizes visam melhorar a qualidade dos cuidados pós-natais essenciais e de rotina prestados às mulheres e aos recém-nascidos, com o objetivo final de melhorar a saúde e o bem-estar materno e neonatal.
Uma “experiência pós-natal positiva” é um resultado importante para todas as mulheres que dão à luz e para os seus recém-nascidos, estabelecendo as bases para a melhoria da saúde e do bem-estar a curto e longo prazo. Uma experiência pós-natal positiva é definida como aquela em que as mulheres, pessoas que gestam, os recém-nascidos, os casais, os pais, os cuidadores e as famílias recebem informação consistente, garantia e apoio de profissionais de saúde motivados; e onde um sistema de saúde flexível e com recursos reconheça as necessidades das mulheres e dos bebês e respeite o seu contexto cultural.
Estas diretrizes consolidadas apresentam algumas recomendações novas e já bem fundamentadas sobre cuidados pós-natais de rotina para mulheres e neonatos que recebem cuidados no pós-parto em unidades de saúde ou na comunidade, independentemente dos recursos disponíveis.
É fornecido um conjunto abrangente de recomendações para cuidados durante o período puerperal, com ênfase nos cuidados essenciais que todas as mulheres e recém-nascidos devem receber, e com a devida atenção à qualidade dos cuidados; isto é, a entrega e a experiência do cuidado recebido. Estas diretrizes atualizam e ampliam as recomendações da OMS de 2014 sobre cuidados pós-natais da mãe e do recém-nascido e complementam as atuais diretrizes da OMS sobre a gestão de complicações pós-natais.
O estabelecimento da amamentação e o manejo das principais intercorrências é contemplada.
Recomendamos muito.
Vamos discutir essas recomendações no nosso curso de pós-graduação em Aleitamento no Instituto Ciclos.
Esta publicação só está disponível em inglês até o momento.
Prof. Marcus Renato de Carvalho
www.agostodourado.com
Novas diretrizes da OMS para os cuidados perinatais de mais qualidade
Pharmaceutical Analysis [Autosaved].pptx
1. By Imtiyaz Bagban
M. Pharm. (Pharmacology)
Assistant Professor
Department of Pharmacology
Krishna School of Pharmacy & Research (KSP)
Drs. Kiran & Pallavi Patel Global University
(KPGU)
1
Introduction to
Pharmaceutical Analysis
B. Pharm. Semester I
Subject – Pharmaceutical Analysis
Subject Code- BP102T
UNIT 1
2. Contents
• Definition and Scope Pharmaceutical Analysis.
• Different techniques of analysis.
• Methods of expressing concentration.
• Primary and secondary standards.
• Preparation and standardisation of various molar and normal solution:
Oxalic acid, sodium hydroxide, hydrochloric acid, sodium
thiosulphate, sulphuric acid, potassium permanganate and ceric
ammonium sulphate
• Errors : Sources of errors, types of errors, methods of minimizing
errors.
2
3. Pharmaceutical analysis
• Pharmaceutical analysis is a branch of practical chemistry that involves a
series of process for identification, determination, quantification and
purification of a substance, separation of the components of a solution or
mixture, or determination of structure of chemical compounds
3
4. 1. In pharmaceutical industry- There are different sectors in pharmaceutical industry as
research and development (R&D) and Quality control (QC) in which pharmaceutical analysis
utilizes regularly.
2. In Food industry- As we all know packed food which consumed by consumer should have
all parameters like quality, purity and safety which enhance acceptability by consumer. For
this it is require analyzing all these parameters for packed food.
Different kind of preservatives, coloring, flavouring and sweetening agents are used in packed
food which can natural or synthetic chemical ingredient so these should analyze qualitatively
and quantitatively, for this various kind of analytical techniques can be applicable.
3. In Cosmetic Industry- Preparation of cosmetics, as lipsticks, creams nail paints, lotion
shampoo and conditioners etc play with two things as colour and odour and these colouring
agents and fragrances are also build by different chemical ingredients so the quality and
quantity of these ingredients should be known which can be analyse by different techniques of
analysis.
4. In Disease diagnosis- Different disease can be diagnosed by pharmaceutical analysis
techniques like HIV is observed by ELISA method 4
Scopes of analysis
5. 5.Geology- Geologist uses analytical procedure for analyzing ground water, minerals,
soil sample etc.
6. Environmental science- Many industrial process give raise to pollutants which can
present health problem. Quantitative analysis of air, water and some times soil sample
carried out to determine the level of pollution and establish safe limits for pollutants.
7. Agriculture science- In farming the nature and level of fertilizer application is based
on information obtained by anlayzing soil to determine its content of essential plant
nutrients, nitrogen, phosphorus, potassium and trace elements required for healthy plant
growth.
8. Government legislation can only be enforced by the work of analytical chemist, e.g
national and international agreements on water pollution and atmospheric pollution,
regulation on substances hazardous to health and laws governing the misuse of drugs.
5
6. There are main two types of chemical analysis
• Qualitative analysis- These tests are performed to indicate whether
the substance or compound is present in the sample or not.
• Various qualitative tests are detection of evolved gas, formation of
precipitates, limit tests, color change reaction, melting point and
boiling point test etc.
• Quantitative analysis- Techniques are mainly used to quantify any
compound or substance in the sample. 6
1. Qualitative analysis ( identification )
2. Quantitative analysis ( estimation )
7. Quantitative analysis are classified as
1. Chemical Methods
A. Volumetric Method- In volumetric methods assay is
based on the measurement of volume of solution of
known strength that is required to react completely
with the substance to be analyse
• Neutralization- Neutralisation reaction between acid
and base
• Precipitation titration- The reaction between titrate and
titrant result in formation of precipitates.
• Complexometric titration- it include complex
formation between the analyte and titrant.
• Redox titration- The titration based on redox reaction
7
8. B. Gravimetric Methods- Gravimetric analysis is a quantitative
analysis by weight and is a process of isolating and weighing
the compound of known composition. i.e. purest form
• The separation of compound is affected by number of ways
like precipitation, volatilization etc
C. Gasometric Methods- These methods involve measurement
of the volume of gases
• These measure gas liberated in the given chemical reaction
under the conditions that are described in the process.
• The volume measured is corrected to standard conditions of
temperature and pressure.
• Decrease in the volume of gas when a suitable agent is placed
to absorb one of the gases present and reduced to standard
conditions of temperature and pressure.
• Cyclopropane, CO2, Nitrous oxide, O2, octyle nitrate, amyl
nitare and nitrogen gases are determined by these method
• Gas Burettes and Nitrometer
9. 2. Instrumental Methods
A) Electrical Methods
• Voltametry- measurement of current at a microelectrode
• Coulometry-measurement of current and time to complete
electrochemical reaction
• Potentiometry- measurement of potential of an electrode
• Condutometry- measurement of electrical conductivity
• Electrogravimetry- electrolysis is carried out and material deposit on electrode is weighed
B) Spectroscopic Methods
a) Absorption Methods-
Visible spectroscopy, Infrared spectroscopy,
UV spectroscopy,
Nuclear Magnetic Resonance Spectroscopy,
Mass spectrometry
b) Emission Methods- Flame photometry, Fluorimetry
9
10. c) Thermal Methods
I. Thermogravimetry
II. Differential thermal analysis
III. Differential scanning calorimetry
d) Separation Methods
a) Chromatographic Methods-
HPLC, TLC, HPTLC,
Paper chromatography,
Gel chromatography,
Ion exchange chromatography
II. Electrophoretic Methods
10
11. 3) Microbiological Method-
• The microbiological assay is based upon comparison of the inhibition of growth of
bacteria by measured conc. of antibiotics to be examined with that produced by known
conc. of standard preparation of antibiotics having known activity.
I. Cylinder plate method ( cup plate)
II. Turbidimetric method
4) Biological Method-
• Biological analysis are carried out to observe biological effect of drug on some living
matter they also called bioassay.
• This method carried out by comparing biological effect of sample to be tested with
biological effect produced by standard compound in identical test condition.
• Bioassay involves measurements of various parameters including tissue of organ,
weight of organ, blood parameters such as blood glucose, cholesterol urea, enzyme
conc.etc
11
12. Methods of expressing concentration
• Concentration is a general term that expresses the quantity of solute contained in a given
amount of solution.
• Solute - Substances that are dissolved
• Solvents- Substance in which solutes are dissolved (usually water)
• Titrant- A solution of known concentration
• Analyte- A solution of substance which is titrated
• Indicator- it is an auxiliary reagent used in all stoichiometric reactions to detect end point
of the reaction.
• Equivalence point- a point at which the reaction just completed.
• End Point-when the reaction between titrant and analyte just complete and the indicator
gives a visual color change in the liquid.
• Stoichiometric end point- equivalent quantity of titrant and analyte has reacted is called
Stoichiometric end point 12
13. Concentration can be express in
1. Molarity (M)
2. Molality (m)
3. Normality (N)
4. Formality (F)
5. Parts per million (ppm)
6. Mole fraction
7. By Percentage
14. • Molar Concentration /Molarity (M) – It is the number of moles of solute dissolved in
1 lit of solution
Molarity (M) = Number of moles of solute
Volume of solution in L
• Volume temperature dependent – Molarity can change with temperature
• Example - 1 mole (40g) of NaOH dissolved in 1 litere solution said to be 1M
• Half mole (20g) of NaOH dissolved in 1 litter solution said to be 0.5M
• Half mole (20g) of NaOH dissolved in 500ml solution said to be 1M
Molal concentration /Molality (m) – Although rarely practice It is defined as number of
moles of solute dissolved in 1000g of solvent
Molality (m) = weight of solute × 100
Weight of solvent × Mol. wt. of solvent 14
15. • Equivalent Weight – The equivalent weight of a substance is defined as the
parts by weight of that substance which is chemically equivalent to 1.008 parts
by weight of hydrogen.
• Equivalent Weight = Molecular Weight
Acidity/Basicity
• EX 1) HCL Eq. Wt = 36.5/1=36.5
• 2) H2SO4 Eq.Wt = 98/2=49
15
Equivalent
Acid
Base
Salt
16. Equivalent Mass of Acid (Neutralization Reaction)
• Equivalent mass of acid =
Molecular mass acid
Number of replaceable OH-(Basicity)
Example
Equivalent mass of HCL and H2SO4
HCl
H
CL
H2SO4
2H
SO4
--
Equivalent mass of HCl = 1+35.5 = 36.5
1
Equivalent mass of H2SO4 = 32 + 4 × 16 + 2 × 1 = 49
2
16
17. Equivalent Mass of Base (Neutralization Reaction)
• Equivalent mass of base =
Molecular mass
Number of replaceable OH-(Acidity)
Example
Equivalent mass of NaOH and Ca(OH)2
NaOH
Na
OH
Ca(OH)2
Ca
2OH
Equivalent mass of NaOH = 23+16+1 = 40
1
Equivalent mass of Ca(OH)2 = 40+2 × 16 + 2 × 1 = 37
2 17
18. Equivalent Mass of Salt ( Complexometric and Precipitation Reaction)
• Equivalent mass of salt =
Molecular mass
Total number of positive or negative charge
Example
Equivalent mass of NaCl and MgCl2
AgNO3 Cl
AgCl ↓ NO3
NaCl Ag
NA
AgCl
Equivalent mass of AgNO3 = 169.9/1 = 169.9 g/mol
Equivalent mass of NaCl = 58.44/1 = 58.44 g / mol
18
19. Equivalent weight in Oxidation and Reduction Reaction
a) Ion Electron Method
• Ascertain the reactants and products of the reaction.
• Write partial equation for oxidising and reducing agent.
• Example:
• Reduction:- Mno4
- → Mn
• The balance atomically and electrically
Mno4
- + 8H+ + 5e → Mn
2H2O
• Equivalent weight =
Molecular weight
Number of electron transferred
Equivalent weight of KMnO4 = 158/5 = 31.6
19
20. • Oxidation:
• Example
Fe+2 → Fe+3
The balance electrically
Fe+2 -e → Fe+3
• Equivalent weight =
Molecular weight
Number of electron transferred
Equivalent weight of FeSO4 = 278/1 = 278
b) Oxidation Reduction Method
• Oxidation and reduction method are the process involving the changes in the valency.
• Oxidation Number (O.N) indicates the amount of oxidation or reduction required to
convert on atom of the element from free state to that in the compound.
• If oxidation takes place O.N is positive and If reduction takes place O.N is negative.
20
21. • O.N of free or uncombined element is zero.
• O.N of hydrogen ( except hydrides ) is +1
• O.N of Oxygen (except peroxides) is -2
• Equivalent weight =
Molecular weight
change in O.N
Example:
(I) K+Mn+7O4
-8 → Mn+2S+6O4
−8
change in oxidation number of manganese is from +7 to +2
Equivalent weight = 158/5= 31.6
(II) 2Fe+2S-2O4 → Fe2
+6(SO4
-6)3
Change in O.N of iron is from +2 to +3 hence
Equivalent weight = 151.90/1= 159.90
(III) K2
+2Cr2
+12O7
-14 → Cr2
+6(SO4
-6)2
Change in O.N of iron is from +12 to +6 hence
Equivalent weight = 294/6 = 49
21
22. Normality (N) - it is the number of equivalent weight of solute dissolved in 1
litter of solution
Normality (N) = Weight of solute
Equivalent Weight × Volume of solution in liter
• Normality varies according to the reaction as the equivalent weight of a
substance may very according to the reaction in which the solute precipitates.
Formality / Formal solution
• Some substances do not exist in molecular form whether in solid or solution
form they remain in ionic form in solid state as well as in solution
• In such cases instead of mol. wt. formula weight used in preparation and its
conc. expressed in terms of formality
Formality (F) = Weight of solute Formula weight
• Volume of solvent
Parts per Million – Parts per Million is frequently used to express the conc.
Of vary solution and is expressed as “ppm”
22
23. Mole fraction (X)- it is defined as moles of component divided by total
number of moles making up solution
Mole fraction (x) = Moles of of component
total number of moles making up solution
• Example- A solution is prepared by dissolving 1 mole of ethyl alcohol
C2H5OH in 3 moles of water where nA and nB represent the number of moles
of ethyl alcohol and water respectively
• Mole fraction of ethyl alcohol = XA= nA/nA+nB
=1/1+3=1/4=0.2
• Mole fraction of water =XB= nB/nA+nB=3/1+3=3/4=0.75
23
24. 24
By Percentage
Volume Percentage (v/v)
• It is defined as the volume of solute in mL present in 100 mL solution.
Volume % = (volume of solute/ total volume of solution) X 100
• For example:
• 10% solution of HCl by volume means that 10 mL of liquid HCl is present in 100 mLof the solution.
Mass by Volume Percentage (w/v)
• It is defined as the mass of solute present in 100 mL of solution.
Mass by Volume % = (mass of solute/ total volume of solution) X 100
• For example:
• A10% mass by volume solution means that 10 gm solute is present in 100 mL of solution.
Mass by Mass Percentage (w/w)
• It is defined as the mass of solute present in 100 gm of solution.
Mass % = (mass of solute / total mass of solution) X 100
• For example:
• A10% mass by volume solution means that 10 gm solute is present in 100 gm of solution.
25. 1.Calculate the masspercentageofaspirin(C9H8O4)inacetonitrile(CH3CN) when 6.5 gofC9H8O4 is
dissolvedin450 gof CH3CN.
Ans.Mass of solution = 6.5g + 450g = 456.5g
Mass% of aspirin= Mass of aspirin X 100
Mass of solution
= 6.5/456.5 X 100 = 1.424%
2. Calculatethe molarityofa solutioncontaining5 gofNaOHin450 mL.
Ans. Moles of NaOH =5 g/40 g /mol (molar mass of NaOH=40 g /mol)
= 0.125 mol
Volume of the solution in liters = 450 mL / 1000mL/L
=0.45L
Molarity(M)= Moles of NaOH / Volume of the solution in liters
= 0.125 mol / 0.45L
= 0.278 mol /L
NUMERICALS ON CONCENTRATION
26. 3. Calculate the mole fraction of ethylene glycol (C2H6O2) in a solution containing 20%
of C2H6O2 by mass.
Ans. Solution will contain 20 g of ethylene glycol and 80 g of water.
Molar mass of C2H6O2 = 12 × 2 + 1 × 6 + 16 × 2 = 62 g /mol
Moles of C2H6O2 = 20 g/62 g mol = 0.322 mol
Moles of water = 80 g/18 g mol = 4.444 mol
Mole fraction of C2H6O2 = (moles of C2H6O2 /moles of C2H6O2+moles of water)
= 0.322/0.322+4.444 = 0.068
Mole fraction of water = 1-0.068 (mole fraction of C2H6O2 + mole fraction of water=1) = 0.932
4. Calculatemolalityof2.5 gofethanoicacid(CH3COOH)in 75 gof benzene.
Ans. Molar mass of CH3COOH : 12 × 2 + 1 × 4 + 16 × 2 = 60 g /mol
Moles of CH3COOH = 2.5 g/60 g /mol = 0.0417 mol
Mass of benzene(solvent) in kg =75 g/1000 g/ kg =0.075kg
Molality(m)of CH3COOH = Moles of CH3COOH
Mass of benzene(solvent) in kg
= 0.0417 mol/0.075kg
= 0.556 mol/kg
27. 5. Calculate the mass percentage of Benzene (C6H6) and Carbon Tetrachloride (CCl4) if
22g of Benzene is dissolved in 122g of Carbon Tetrachloride.
Ans.
Mass percentage of benzene = Mass of benzene X 100
Mass of solution
=22g X100 /144g = 15.28%
Mass percentage of carbon tetrachloride=100-15.28 = 84.72
6. Calculate the mole fraction of Benzene in solution containing 30% by mass in Carbon
tetrachloride.
Mole fraction of benzene= No. of moles of benzene
(No. of moles of benzene + No. of moles of carbon tetrachloride)
No. of moles of benzene= mass of benzene/molar mass of benzene
= 30g/78g/mol(molar mass of benzene 78g/mol)
=0.385
No. of moles of carbon tetrachloride= mass of carbon tetrachloride/molar mass of carbon tetrachloride
=70g/154g/mol =0.455
Mole fraction of benzene=0.385/(0.385+0.455) = 0.458
Mole fraction of carbon tetrachloride=1-0.458 = 0.542
28. 7. CALCULATE THE MOLARITY OF EACH OF THE FOLLOWING SOLUTIONS:
(A) 30 g OF CO(NO3)2. 6H2O IN 4.3 L OF SOLUTION (B) 30 ML OF 0.5 M H2SO4
DILUTED TO 500 ML.
Ans.
(A)Molarity of solution = No. of moles of solute
Volume of solution in L
No. of moles of solute = Mass of Co(NO3)2. 6H2O
Molar mass of Co(NO3)2.6H2O
=30g/310.7g/mol = 0.0966
Volume of solution in L=4.3L
Molarity of solution=0.0966/4.3=0.022M
(B) M1V1=M2V2
M1=0.5M,V1=30ML, V2=500ML, M2=?
M2=0.5X30/500
=15/500
=0.03M
29. 8. Calculate (A) Molality (B) Molarity and (C) Mole fraction of KI if the density 20%
(mass/mass) aqueous KI is 1.202 g/mL.
Ans. Here Mass of KI=20g,
Mass of solution=100g,
Mass of solvent=80g
(A)Molality(m)=0.12/0.080=1.5m
(B) Molarity(M)=0.12/0.0832=1.44M
(volume of solution=mass of solution/density)
=100/1.202=83.2ml=0.0832L)
(c) Mole fraction of KI= No.of moles of KI
Total no. of moles in solution
= 0.12/(0.12+4.44)
=0.0263
30. 30
Primary Standard
These are extremely pure, stable, it not a hydrate/has no water of hydration, and has a high molecular weight.
Ex. Potassium hydrogen phthalate, Benzoic Acid, Arsenious Oxide, Sodium Carbonate, Sodium Oxalate, Potassium
Iodide, Potassium dichromate, Potassium hydrogen iodate
Properties:
It is extremely pure,
Highly stable
It is anhydrous
It is less hygroscopic
Has very high molecular weight
Can be weighed easily
Should be ready to use and available
Should be preferably non toxic
Should not be expensive
31. Secondary Standard:
Don’t meet requirements for a primary standard but are available with sufficient
purity and properties to be generally acceptable. It is usually standardized against a
primary standard.
• EX. - NaOH , KOH , Ba(OH)2, HCl , HNO3 , HClO4 Sulfamic Acid, KMnO4 , Na2S2O3
• Properties:
Prepared from primary standard
Stable
Reacts rapidly and completely with analyte
31
32. Quality Control
• Quality control is powerful productivity technique for effective diagnosis of lack of
quality or conformity to settle standards in any of the material.
• The science of quality control is largely statistical in nature. The statistical quality
control technique is based on theory of probability and sampling and is extensively used
in pharmaceutical industries and quality control laboratory.
• Statistical quality control is classified into two part:
• Process control- To maintain satisfactory quality level in production.it ensure that the
product confirms to the specified quality standards.it is achieved through technique of
control chart.
• Product Control- Controlling the quality of product by critical examination at strategic
points which achieved through sampling inspection plans.
• Random samples of work in process are taken and inspected. data collected and
presented in chart from which is essential part of quality control system.
32
33. • Improve quality and uniformity level.
• Better use of raw material.
• Efficient utilisation of equipment.
• Batter inspection.
• Batter specification.
• Improve consumer and manufacturer relation.
33
Objective of statistical quality control
34. QC functions and responsibilities
• This department is staffed with scientist and technicians responsible
for sampling of raw material and inspection of packaging components
, including labelling.
• They conduct in process testing, environment monitoring and inspect
operation for compliances. test on finished dosage form
• QC is responsible for monitoring product quality through
distribution, including testing of product complaint sample,
evaluating product stability etc.
• QC play important in the selection and qualification of vendors from
whom these materials are purchased.
• QC is responsible, as part of its testing and inspection for monitoring
the environmental conditions under which products are
manufactured and held. different level of control are established
depending on intended use of dosage form. Ex Parenteral Product
(sterile condition).
34
35. • Another major element of quality is Non sterile Products such as
liquids, tablets, and capsules. The objective here is to determine an
acceptable level of particulates and microbial contaminates and then to
control them to this level.
• If particulates are found to be excessive steps must be taken to bring
them within acceptable limits. So as not to compromise the quality of
product.
• Control of Packing components especially those that come into direct
contact with a product. These materials must be inspected and tested
against rigid specifications to ensure they meet functional standard.
• Labelling is understandably a critical component not just in original
design and acceptance but also with regard to secure storage and to
ensure accountability. Final product labelling must be inspected to
ensure that it is correct.
35
36. Quality Assurances
• Quality assurance system involves a set of procedure put in place to
ensure that quality control activities are performed.
• QA system permit certain level of confidence to be assigned to result
that are obtained from an analytical procedure.
• QA system normally involves accreditation with an outside
independent organisation within many countries numerous analytical
procedures may now be accredited via for example the International
standards organization.
36
37. Importance of QA
• The Pharmaceutical industry as avital segment of the health care
system.
• Conduct research
• Manufacture and market pharmaceutical and biological products and
medical devices use for acute and chronic treatment and diagnosis of
disease.
• Recent advances in drug discovery are presenting new challenges to
QC and the system that operate internally in the industry.
• The external regulations established by the food and drug
Administration and other regulatory bodies also added to these
challenges.
• Quality must be built into a drug product during product and process
design and it is influenced by physical plant design, space, ventilation,
and sanitation during routine production.
37
38. QA Function and Responsibilities
• QA has to play a major role in the identification and preparation of the
necessary policies and standard operating procedures. (SOPs)
relative to control quality.
• Specification and test for active ingredients, the excipients, and the
product itself,
• Specific stability procedures for the product,
• Freedom from microbial contamination,
• Proper storage of the product and containers, packaging, and
labelling to ensure that container closure systems provide functional
protection of the product against factor like moisture, oxygen, light,
volatility, and drug /package interaction.
• Quality Monitoring – this activity is able to determine if operation
have adequate system facilities and written procedure to control the
quality of product produced.
38
39. • Establish control or checkpoints to monitor the quality of the product
as it is proceed and upon completion of manufacture.
• Raw material and component testing
• In process , packaging, labelling, and finished product testing
• Batch auditing and stability monitoring
• Responsibility for final product release- It must determine that the
product meets all the applicable specification and it was manufactured
according to internal standard an cGMPs.
• Audit Function: QA department combine this reviews of SOPs with
an audit of facilities and operations.
• Then it give company management an inside report on its level of
compliances and will allow the necessary changes or correction to be
made prior to either causing product failure or as a deficiency during
inspection by FDA
39
40. Preparation and standardization of various Molar and Normal solution
• For the preparation of standard solution a known quantity of standard
substances depending upon the requirement is dissolved in known amount of
water and desired volume is made.
• These substances have a constant weight, high purity, non hygroscopic, the
solution is of known and definite concentration.
• Example- Prepare 0.1N Oxalic acid
1) Oxalic acid – (COOH)2.H2O
• Mol.weight – 126
• Acidity – 2
• Equivalent weight – 63
• Therefor weight 6.3gm of oxalic acid (COOH)2.H2O and transfer it in to
volumetric flask and make up to the mark.
40
41. 2) Sodium Hydroxide
Preparation of 0.1N NaOH solution=40
Mol. weight of NaOH= 40
Acidity ( number acceptable Oh groups) = 1
Equivalent Weight of NaOH= 40
Therefor 4g of NaOH dissolved in 1 lit of solution will give 0.1N solution
Procedure
weigh accurately 4 g of NaOH in a beaker and dissolve it in distilled water.
weighing should be performed quickly as it is hygroscopic. Transfer the contents
and the washings to a 1 lit volumetric flask. Cool and then make volume up to the
mark. Shake well.
Standardization
The 0.1N NaOH prepared as per above mentioned procedure is standardized by
titrating against 0.1N Oxalic Acid using Phenolphthalein as an indicator. 10 ml
0.1 N oxalic acid is taken in a conical flask to which 2 – 3 drops of
Phenolphthalein is added and mixed well. 41
42. • This solution is titrated slowly with constant stirring against 0.1N NaOH
taken in burette. Titration is continued till the appearance of permanent pale
pink colour as the end point.
• Calculation of normality of NaOH using formula
• N1V1=N2V2 where N1= Normality of NaOH ?
V1= Volume of NaOH Solution used
N2= Normality of standard oxalic acid solution
V2= Volume of standard oxalic acid solution
3) Potassium Permanganate:
Preparation of 0.1N KMnO4 Solution
Mol.weight of KMnO4 = 158g/mol
Equivalent weight of KMnO4= 31.6
42
43. • Equivalent weight of KMnO4 is reaction specific. In acidic medium
KMnO4 is used as an oxidiser. So there will be 5 electron gained by Mn
atom. Hence the Equivalent weight of KMnO4 = Molecular weight /
Number of electrons gained in redox reaction = 158/5= 31.6 so 3.16 or
3.2 g of KMnO4 is weighed and dissolved in 1 lit of distilled water to get
0.1N KMnO4 solution.
• In alkaline or neutral medium, reaction of KMnO4 is different and Mn
gains 3 electrones in redox reaction. So for alkaline medium redox
titration, Equivalent weight of KMnO4=158/3 =52.6 So 5.26 g of KMnO4
is weighed and dissolved in 1 lit of distilled water to get 0.1N KMnO4
solution.
• Procedure
• 3.2 g of KMnO4 is weighed and dissolved in 1 lit of distilled water to get
0.1N KMnO4 solution. the solution is boiled for 10-15 minutes and then
allowed to stand for few days and filtered through glass wool.
43
44. • Standaradization
• 10ml of 0.1N oxalic acid taken in conical flask. Add 5ml dilute sulphuric
acid warm it to 60-70⸰C and titrate against KMnO4 from the burette till light
pinkish colour appears. Repeat the titration until concomitant result are
obtained the strength of KMnO4 is calculated using the formula
N1V1=N2V2 where N1= Normality of KMnO4 ?
V1= Volume of KMnO4 Solution used
N2= Normality of standard oxalic acid solution
V2= Volume of standard oxalic acid solution
• Note: Ordinary or even pure distilled water contains traces of organic
matter which reduces the KMnO4 solution. That is why the solution is
boiled and kept for some time before standardization. In the absence of
sufficient amount of dilute H2SO4 or due to the time rapid addition of
KMnO4 in titration brown turbidity may appear.
44
45. 4) Sulphuric Acid:
Preparation of 0.1N H2SO4
Equivalent weight of H2SO4= 49
Specific gravity = 1.84 g/ml
So volume of 49 g H2SO4 = 26.6 ml
Concentrated H2SO4 is about 97% pure
Therefore actual amount of Concentrated H2SO4 required for 1 lit of 1N
H2SO4 solution is = (100/97)×26.6 = 27.42
For 1 lit 0.1N H2SO4 solution, 2.74 ml of Concentrated H2SO4 required
Procedure
Take 2.74ml sulphuric acid in beaker filled with small amount of
distilled water. Transfer the contents of beaker to volumetric flask of 1
lit capacity and make volume up to the mark with distilled water. Shake
well.
45
46. Standardization
• 0.1N H2SO4 is titrated with 10ml of 0.1N Na2CO3 using methyl orange as
an indicator. Repeat the titration until at least three concordant readings
are obtained
• Suppose 10ml of 0.1N Na2CO3 = 9.5 ml of H2SO4
N1V1=N2V2
10×0.1=9.5×N2
N2 = 0.1052
To prepare 1 lit 0.1N H2SO4 the volume of 0.1052 N acid required is
1000×0.1= 950ml
0.1052
Take 950ml 0.1052 N acid and dilute to 1 lit.
46
47. 5) Hydrochloric Acid:
Molar mass of HCl is 36.46g/mol, since HCl has only one hydrogen, the
equivalent mass will be 36.46. Specific gravity for 1 lit. volume of HCl is
1.189
For 1 lit. volume, grams of compound needed = (0.1N)(36.46)(1lit)=3.6461
Volume of concentrated (37.5%) needed= 3.6461 =8.1774ml
0.375×1.189
Procedure
Transfer exactly 20ml of the 0.1M HCl solution into 250ml conical flask. Add
3 drops of phenolphthalein as indicator. Titrate against standard 0.1N NaOH
solution until a permanent pale pink colour is appeared. Using the volume of
NaOH, the strength HCl is calculated.
HCL can be standardized by titrating with standard 0.1N Na2CO3 using
methyl orange as indicator, colour change yellow to reddish orange.
47
48. Standardization
• HCl is standardized against 0.1N NaOH which is already standardized
against 0.1N oxalic acid using phenolphthalein indicator.
HCl + NaOH → NaCl + H2O
6) Sodium Thiosulphate:
Preparation of 0.1M Sodium Thiosulphate Solution (Na2S2O3.5H2O):
Dissolve 24.8gm of sodium thiosulphate crystal in previously boiled and
cooled distilled water and make the volume to 1000ml.
Store the solution in a cool place in a dark colored bottle.
After storing the solution for about two weeks, filter if necessary and
standardize as follows:
48
49. Standardization
• Weigh accurately about 5 gm of finely ground potassium
dichromate which has been previously dried to a constant weigh
about at 105+2⸰C into a clean 1 lit. volumetric flask.
• Add distilled water to dissolve the content of volumetric flask and
make up to the mark with distilled water shake thoroughly and
keep in dark place.
• Pipette 25 ml of this solution into 250ml conical flask. Add 5ml
concentrated HCl and 15ml of 10% potassium iodide solution.
Allow to stand for 5 min and titrate the mixture with the solution
of sodium thiosulphate using starch solution as an indicator
towards the end point.
• The end point taken when blue colour changes to green. Calculate
the Normality of the Sodium thiosulphate.
49
50. 7) Ceric Ammonium Sulphate:
Preparation of 0.1M Ceric Ammonium Sulphate:
Dissolve 66gm of ceric ammonium sulphate with gentle heat in a mixture of 30ml of
sulphuric acid and 500ml of water. Cool the mixture, filter and dilute to 1000ml with
water.
Standardization of 0.1M ceric Ammonium sulphate:
Arsenic trioxide is allowed to dry for an hour. From this weigh about 20.2gm of arsenic
trioxide accurately and transfer into 500ml conical flask. Wash the inner walls with of
conical flask with 100ml of water and mix thoroughly. To this , add 300ml of dilute
sulphuric acid ,0.15ml of osmic acid and 0.1ml of ferroin sulphate indicator.
Titrate this solution with ceric ammonium sulphate which has taken in burette. Continue
the titration till the pink colour of solution changed to pale blue or yellowish green
colour.
Each ml of 0.1n ceric ammonium sulphate≅ 0.6326 gm of ceric ammonium sulphate
≅4.946 gm of arsenic trioxide
50
51. DEFINITION:
• Errors may be defined as the difference between a measured value and its true value.
• True value of a measurement is determined by taking the mean value of a series of repeated
measurements.
TYPES OF ERRORS:
• Errors are classified in two types
I. Systemic (Determinate) errors
II. Random (Indeterminate) errors
A) DETERMINATE ERRORS:
• Errors which can be avoided or whose magnitude can be determined is called as systemic
errors. It can be determinable and presumably can be either avoided or corrected.
ERRORS
51
52. 52
Systemic errors further classified as:
1. Operational and personal error
2. Instrumental error
3. Errors of method
4. Additive or proportional error
1. Operational and personal error:
• Errors for which the individual analyst is responsible and are not connected with the method
or procedure is called as personal errors.
• We can assign indeterminate errors to several sources, including collecting samples,
manipulating samples during the analysis, and making measurements.
e.g. unable to judge colour change when errors occur during operation is called as operational
error e.g. transfers of solution, effervescence, incomplete drying, underweighting of precipitates,
overweighing of precipitates, and insufficient cooling of precipitates.
These errors are physical in nature and occur when sound analytical techniques is not followed
53. 53
2.Instrumental and Reagent errors:
Errors occur due to faulty instrument or reagent containing impurities.
e.g. un-calibrated weights, un-calibrated burette, pipette and measuring flasks.
3.Errors of Method:
When errors occur due to method, it is difficult to correct. In gravimetric analysis, error
occurs due to Insolubility of precipitates, co- precipitates, post-precipitates, decomposition,
and volatilization.
In titrimetric analysis errors occur due to failure of reaction, side reaction, reaction of
substance other than the constituent being determined, difference between observed end
point and the stoichiometric equivalence point of a reaction.
54. 54
4. Additive or proportional errors:
• Additive error does not depend on constituent present in the determination e.g. loss in weight
of a crucible in which a precipitate is ignited.
• Proportional error depends on the amount of the constituent e.g. impurities in standard
compound.
B)INDETERMINATE ( Random )ERRORS :
• These errors are also called accidental errors. Indeterminate errors arise from uncertainties in
a measurement that are unknown and which cannot be controlled by the analyst.
• Random error is caused by unpredictable fluctuations in the readings of a measurement
apparatus or experimenters interpretation of the instruments reading.
55. MINIMIZATION OF ERRORS:
Analyst has no control on random errors but systemic errors can be reduced by following
methods.
(I) Calibration of Instruments, Apparatus and Applying Necessary Corrections:
• Most of the instruments, commonly used in an analytical laboratory, such as : UV-
Spectrophotometer-meter, IR- Spectrophotometer, single—pan electric balance, pH-meter,
turbidimeter and nephelometer, Polari meter, refractometer and the like must be calibrated
duly, before use so as to eliminate any possible errors.
• In the same manner all apparatus, namely : pipettes, burettes, volumetric flasks,
thermometers, weights etc., must be calibrated duly, and the necessary corrections
incorporated to the original measurements in some specific instances where an error just
cannot be avoided it may be convenient to enforce an appropriate correction for the effect
that it ultimately causes for instance : the inherent impurity present in a weighed precipitate
can be estimated first and then deducted duly from its weight.
56. II) Performing a Parallel Control Determination:
• It essentially comprises of performing an altogether separate estimation under almost
identical experimental parameters with a quantity of a standard substance that consists of
exactly the same weight of the component as is present in the unknown sample.
• Thus, the weight of the component present in the unknown sample may be calculated with
the help of the following expression :
Result found for standard
× Weight of constituent in standard
Result found for unknown X
Where, X = Weight of the component present in the Unknown sample.
57. (III) Blank Determination :
• In order to ascertain the effect of the impurities present in the reagents employed and reaction
vessels used, besides establishing exactly the extent to which an excess of standard solution
required to locate the exact end-point under the prevailing experimental parameters of the
unknown sample—a blank determination is an absolute necessity.
• It may be accomplished by performing a separate parallel estimation, without using the sample
at all, and under identical experimental parameters as employed in the actual analysis of the
given sample.
• Note : Always avoid using an appreciably large blank correction which gives rise to a vague
and uncertain ‘exact value’ thereby minimizing the precision of the analysis.
58. (IV) Cross-checking Results by Different Methods of Analysis:
In certain specific cases the accuracy of a result may be cross-checked by performing another
analysis of the same substance by an altogether radically different method.
Examples :
(a) HCl-Solution : It may be assayed either by titration with a standard solution of a strong
alkali (NaOH), or by precipitation
(b) In water hardness the calcium and the magnesium conc. Determine by atomic absorption
may be compared with the results obtained by complexometric titration (EDTA titration )
In short, the results thus obtained by the two fundamentally different techniques must be
concordant thereby justifying and ascertaining the fact that the values obtained are fairly
small limits of error.
59. (V)Method of Standard Addition:
• Here, a small known quantity of the component under estimation is added to the sample, which
is subsequently subjected to analysis for the total amount of component present.
• The actual difference in the quantity of components present in samples with or without the
added component ultimately gives the recovery of the amount added component.
• A goods at is factory recovery builds up the confidence in the accuracy of the method of
analysis.
Note : The method of ‘standard addition’ is particularly useful to physicochemical techniques
of analysis, for instance : Spectrophotometry, Turbidimetry.
(VI) Method of Internal Standards:
• The specific method is of immense value both in chromatographic as well as spectroscopic
determinations.
• Here, a fixed quantity of a reference substance (i.e., the ‘internal standard’) is added to a series
of known concentrations of the material to be assayed.
• The ratio of the peak size of the internal standard and the series of known conc are plotted
against the conc. values. This should give straight line.
60. Absolute Error
The absolute error is the difference between the measured value and the actual
value. (The absolute error will have the same unit label as the measured quantity)
E absolute = I X(measured) – X(accepted) I
Relative Error:
Relative error is the ratio of the absolute error of the measurement to the accepted
measurement.
E relative = [measured value- actual value]/actual value
Percent of Error:
Error in measurement may also be expressed as a percent of
error. The percent of error is found by multiplying the relative error by 100%.
E % = [measured value- actual value]/actual value x 100
61. 61
Sources of Impurities in Pharmaceuticals
Impure Chemical Compound:
• Acompound is said to be impure if it is having foreign matter i.e. Impurities.
Pure Chemical Compound:
• A pure chemical compound refers to that compound which is having no foreign matter
i.e. impurities.
• Chemical purity means freedom from foreign matter.
• Analytically 100 % pure substances are not available and traces of impurities must be present.
• Impurity is any material that affects the purity of the material of interest.
• Presence of Impurities in the pharmaceutical substances may produce toxic effects on the
body and may also lower down the active strength of the pharmaceutical substance.
• Impurities commonly in chemical substances include small quantities of lead, Arsenic,, Iron,
Chloride and sulphate.
62. 62
Sources of Impurities in Pharmaceuticals
The different sources of impurities in pharmaceuticals are listed below:
1)Raw material used in manufacture
2)Reagents used in manufacturing process
3)Method/ process used in manufacture or method of manufacturing
4)Chemical processes used in the manufacture
5)Atmospheric contamination during the manufacturing process
6)Intermediate products in the manufacturing process
7)Defects in the manufacturing process
8)Inadequate Storage conditions
9)Decomposition of the product during storage
10) Accidental substitution or deliberate adulteration with spurious or useless
materials
63. 63
1) Raw materials employed in manufacture
• When substances or chemicals are manufactured the raw materials from
which these are prepared often contain impurities. These impurities get
incorporated in final product
• Example – Impurities like arsenic, lead, heavy metal etc., are present in
raw material and are found in final product.
• Impurities such as Arsenic, Lead and Heavy metals are present in raw
materials and hence are found in substances. So, it is necessary to use
pure chemicals and substances as raw materials for the manufacturing
process.
64. 64
HgCl2+ 2NH4OH-------------NH2HgCl + NH4Cl + 2 H2O
Soluble soluble Ammoniated mercury (ppt) (soluble)
2) Reagents used in the manufacturing process:
• If reagents used in the manufacturing process are not completely removed by
washing, these may find entry into the final products.
• Example:
Ammoniated mercury may be prepared by adding a solution of Mercuric chloride to dilute
ammonia solution.
The precipitate ofAmmoniated mercury (Final Product)contains ammonium hydroxide.Thus,
this precipitate is washed with cold water to remove ammonium hydroxide.
If it is not removed completely by washing with water, the final product may
contain in it Ammonium hydroxide as impurity.
65. 65
3) Method or the process used in the manufacture:
• Many drugs and chemicals (usually organic) are manufactured from different raw
materials, by using different methods or processes.
• Some impurities are incorporated into the materials during the manufacturing process.
• The type and amount of impurity present in the drug/ chemical varies.
• In certain drugs , a multiple-step-synthesis procedure is used , which produces
• intermediate compounds.
• The purification of intermediates is also important, otherwise the impurities present in
the intermediate will get incorporated in the final product.
• Usually side reactions occur during the synthesis. Impurities of the product side
reactions also occur in the substances.
66. • This may introduce new impurities due to contamination by reagents and solvents at various
stages of the process as described below:
Reagents employed in the process:
i.e. Calcium carbonate is obtained by interaction of a soluble calcium salt and a soluble carbonate and
therefore the product will contain traces of soluble alkali, which the washing process has failed to remove.
Reagents added to remove other impurities
i.e. Potassium bromide contains traces of Barium, which is added in the manufacturing process to remove
excess of sulphate.
Solvents
i.e. Water is the cheapest solvent available and has been used wherever possible
Action of solvents and reagents on reaction vessels
• During manufacturing process, some of the solvents and reagent may undergo reaction with metals of
reaction vessel and may dissolve these metals, which appear as impurities in the final product.
• i.e. The inorganic compounds manufactured in Iron vessel will containArsenic and Iron as impurities.
• Thus IP has prescribed limit test forArsenic and Iron for most inorganiccompounds
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67. 4) Chemical process used in the manufacture:
For the synthesis of drugs, many chemical reactions such as Nitration,
Halogenation, Oxidation, reduction, hydrolysis are involved.
In these chemical processes, different chemicals are used.
Tap water is generally used in the various processes and it is often having
Cl-,Mg+2, Ca+2 ions, which are generally found in the substance which is
being manufactured.
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68. 5)Atmospheric contamination during the manufacturing process:
• In the industrial areas, the atmosphere is contaminated with dust particles and
• some gases like Hydrogen sulphide, Sulphur dioxide, and black smoke.
• During the manufacture or purification of the pharmaceutical products, these
impurities enter the final products.
• There are many pharmaceutical products which when manufactured are
contaminated with atmospheric CO2 and water vapour.
Example - NaOH absorbs atmospheric CO2.
• 2NaOH + CO2 -------------------------------- Na2CO3 + H2O
• Due to this reaction, NaOH should not be kept open for a longer time during its
• manufacture.
• Therefore, IP has prescribed that Sodium hydroxide should not contain more than 3% of
sodium carbonate.
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69. 6) Defects in the manufacturing process:
• In many manufacturing processes, there are defects like imperfect mixing,
incompleteness, non-adherence to proper temperature, pressure, pH or reaction
conditions, which may give chemical compounds with impurities in them.
• Example:
• Zinc oxide may be prepared by heating metallic zinc to bright redness in a current of
air. The vapours of Zinc burn to form Zinc oxide which is collected as a fine white
powder.
• But if there is less heat or air or both, zinc metal is not completely converted to
zinc oxide.
• Thus the final product, Zinc oxide may still contain metallic zinc as impurity.
• So, IP has prescribed a test for Zinc metal in zinc oxide.
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70. 7) Intermediate products in the manufacturing process:
• There are some intermediates which are produced during the manufacturing
process.
• Sometimes these intermediates may be carried through to the final product as
impurity.
Example:
Potassium iodide is prepared by reacting Iodine with Potassium hydroxide.
6KOH+ 3I2--------------------5KI + KIO3 + 3H2O
• The resulting solution is first evaporated and then heated with charcoal.
KIO3 + 3C-------------------KI + 3CO
• In this process if the intermediate product (KIO3) is not completely converted into
KI, then it may be carried through to the final product as an impurity.
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71. 8) Storage conditions:
• The chemical substances when prepared have to be stored in different types of containers
depending upon:
Nature of the material
Batch size
Quantity
• Many types of materials are used for storage purpose like plastic, polythene, iron vessels,
stainless steel and aluminum copper etc.
• Reaction of these substances with the material of the storage vessel takes place and the
products formed occur as impurities in the stored material.
Examples-
• Leaching out effect: Alkalis stored in ordinary glass containers extract lead from it, which
in found as impurity in the final product.
• Strong chemicals react with iron containers and extract Iron an impurity in final product.
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72. 10) Decomposition of the product during storage:
• Chemical decomposition, analysis or breakdown is the separation of a chemical
compound into elements or simpler compounds.
• It is sometimes defined as the exact opposite of a chemical synthesis. Chemical
decomposition is often an undesired chemical reaction.
• Some substances decompose on storing due to presence of air, light and oxygen. So,
the final product is contaminated.
• Deliquescent substances, absorb water from the atmosphere and get liquefied.
• Crude vegetable drugs are especially susceptible to decomposition.
• A number of organic substances get spoiled because of decomposition on exposure to
the atmosphere. e.g. amines, phenols potent drug etc.
• Decomposition products appear as impurities in the substances.
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73. 11)Accidental substitution or deliberate adulteration with spurious or
useless materials:
• It is possible to avoid accidental substitution by storing the toxic
substances together
• separately or in a locked cupboard.
• Many pharmaceutical chemicals are adulterated with cheaper substances.
• E.g The expensive potassium may be adulterated with sodium bromide
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74. Effect of Impurities
The impurities present in the substances may give following effects:
1. Impurities having toxic effects may be injurious to health, if present above
certain limits.
2. Traces of impurities may exert a cumulative toxic effect after a certain time.
3. Impurities may lower the active strength of the substance.
4. Impurity may decrease shelf life of substance.
5. Impurity may cause incompatibility with other substances.
6. Impurities may cause a physical or chemical change in the properties of the
substance, so making the substance medicinally useless.
7. May cause change in color, odour and taste.
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75. Pharmacopoeia of various countries prescribe “Test for purity” for substances
which are to be used for medical purpose. The so called tests for purity are as a
matter of fact tests for detecting impurities in the substances.
Pharmacopoeia will decide and fix the limit of tolerance for these impurities.
For certain common impurities for which pharmacopoeia prescribes the test of
purity are:
Colour, odour, taste:- Along with other test for purity, description of test, odour,
colour, etc., are given in pharmacopoeias.
Physicochemical constants :- Solubility of the substances in various solvents ,
determination of melting and boiling points for organic substances, optical rotation
for optically active substances and refractive index for liquids are some values which
tell us about the purity of substances.
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Test for purity:
76. Acidity, alkalinity, pH:- Substances that are prepared from chemical reaction involving
acids and alkalis often contain considerable amount of the acid or alkali, as an impurity.
So the tests for acidity and alkalinity are of a great help to estimate the extent of the
impurity.
• Solution of certain substances have a definite pH at a given conc. The presence of an
impurity will bring change in pH and it can be detected.
Cations and anions:- A large number of synthetic drugs both inorganic and organic is
prepared using strong acids like hydrochloric, nitric, sulphuric, etc.
• The presence of chloride and sulphate ions are common impurities. Test for these ions
(anions) generally carried out.
• Test for sodium , ammonium (cations) are often carried out to detect impurities in
inorganic compounds.
• Tests for heavy metals like lead, iron, copper and mercury are also carried out as these
are very common impurities in substances.
Ash:- Determination of ash in crude vegetable drugs , organic compound and some
inorganic compounds give good indication about the extent of impurities of heavy
metals or minerals in nature.
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77. Validation Parameters of analytical methods
Validation: A process involving confirmation of establishing by laboratory studies that a
method/procedure/system/analyte give accurate and reproducible result for intended analytical
application in a proven and established range is called validation.
Analytical parameters to be validated:
1) Accuracy
2) Precision
3) Repeatability
4) Reproducibility
5) Intermediate precision
6) Selectivity (specificity)
7) Linearity and range
8) Sensitivity
9) Limit of detection
10) Limit of quantitation
11) Ruggedness
12) Robustness
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78. • Accuracy:
• It relates to the closeness of test results to true ( actual ) value. i.e measure of
exactness of analytical method.
• It is expressed as % recovery by the assay of known added amount of analyte in the
linearity range. This is probably most difficult parameter to validate.
• Accuracy of the method can be determine in one of three ways
a) Recovery study
b) Comparison with results using another method known to be accurate
C) Analysis of reference material
• Recovery studies are performed by adding a known amount of the analyte either to
blank matrix or by adding a sample in which the background analyte is measured
by the same procedure and subtracting from the total value to obtain recovery.
• A better validation is to perform the analysis by two independent methods in which
the second method is known to be accurate for the sample matrix of interest
• The ideal way to validate a method is to analyse a reference material in composition
to given sample.
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79. • Precision:
• Precision may be defined as the degree of agreement between the replicate
measurements of the same quantity.
• The precision is usually expressed as
• Standard deviation
• Relative standard deviation
• Repeatability: Repeatability is the precision of the method when repeated by the same
analyst using same test method and under same set of laboratory conditions within a
short interval of time, deference being the sample analysed.
• Reproducibility: when the subject method is carried out by different analyst in
different laboratories, using different equipments, reagents and laboratory setting
and on different days using the sample for same then the study carried out is
reproducibility study.
• Intermediate precision: Precision of the method when repeated in same laboratory.
Different days, different analyst, different equipment, different reagent lots etc.
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81. • Selectivity (specificity):
• Selectivity is the extent that the method can measure the analyte of interest in the matrices of
the sample being analysed without interference from matrix (including other analyte)
• The method must allow distinct analytical measurement of analyte of interest and exclusion of
all other relevant interferences.
• Linearity and range:
• The linearity of an analytical method is its ability to obtain test result that are directly
proportional to the concentration of analyte in samples.
• Range: Lowest and highest level of analyte that the method can determine with reasonable
accuracy and precision in the range of 80/100/120% of the claim.
• Linearity and range may be demonstrated directly one the test substance and or by using separate
weighing or synthetic mixture of the test product components, using proposed procedure.
• Sensitivity:
• The sensitivity is the ability to differentiate two different concentration and is determined by
the slop of the calibration curve.
• Sensitivity is the slop of the calibration curve that is obtained by the response against the
analyte concentration.
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82. • Limit of detection (LOD): it is defined as the lowest conc. of analyte in sample that can
be detected but not necessarily quantify under stated experimental condition.
• Limit of quantitation (LOQ): it is defined as the lowest conc. of the analyte in a
sample that can be estimated quantitively with acceptable precision, accuracy and
reliability by a given method under stated experimental condition.
• Ruggedness: refer to the precision of test result obtain by analyse the same sample
under Varity of normal test condition such as laboratories, analysts, instruments,
days, reagents.
• Ruggedness is a measure reproducibility of test results under normal expected
operational conditions from laboratory to laboratory and from analyst to analyst.
• Study will identify those factor that will contribute to variability of the results and should
not be changed.
• Robustness: Robustness or reliability refer to how sensitive the method is to control
small change in parameters such as the size of sample, temperature, pH of the
solution, reagent of concentration, time of reaction.
• It is the measure the capacity of the analytical method to remain unaffected by small but
deliberate variation in procedure.
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83. Sampling techniques:
• Sampling: Sampling is withdrawal of small portion from bulk which is
truly representative of whole bulk material.
• Sample Preparation: the problem involves obtaining a sample that is
representative of the whole. This sample is called the gross sample.
• Its size very from a few gram or less to several pound, depending of the
type of bulk material.
• Once gross sample is obtained it may have to reduced to a sufficiently small
size to be handled. This is called sample.
• Once sample is obtained an aliquot, or portion of it will be analysed, this
aliquot is called the analytical sample.
• Several replicate analyses on the same sample may be performed by taking
separate aliquots.
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84. 1) Sampling techniques for solid compound:
• In homogeneity of the material, variation in particle size, and variation
within the particles make sampling of solid more difficult than other
material.
• The easiest but usually most unreliable way to sample a material is the grab
sample which is one sample taken at random and assumed to be
representative.
• The grab sample will be satisfactory only if the material from which it is
taken is homogeneous.
2) Sampling techniques for liquid compound:
• These material tend to be homogeneous and are much easier to sample.
Liquid must be shaken to obtain a homogeneous mixture.
• If mixture is indeed homogeneous a simple grab sample will suffice. For all
practical purpose this method is satisfactory for taking blood samples.
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85. • If liquid samples are not homogeneous and if they are small enough they can be
shaken and sample immediately. Example they may be particles in the liquid that
have tend to settle.
• Large stationary liquids can be sampled with thief sampler which is device for
obtaining aliquots at different levels.
• The separate aliquots of liquids can be analysed individually and the result obtained,
or the aliquots can be combined into one gross sample and replicate analyses
performed.
3) Sampling techniques for gaseous compounds:
• The usual method of sampling gases involves displacement of a liquid. The liquid
must be one in which the sample has little solubility and with which it does not
react.
• Mercury is the liquid is allowed to trickle from the bottom of the container,
whereupon the gas is pulled in at the top.
• A grab type sample is satisfactory in some cases. In the collecting of breath sample.
• Example- the subject could blow into an evacuated bag . Auto exhaust could be
collected in large evacuated plastic bag.
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86. Sampling error minimization:
1) By increasing the size of the sample:
The sampling error can be reduced by increasing the sample size. If the sample size n is
equal to the population size N, then the sampling error is zero.
2) By stratification:
When the population contains homogeneous units, a simple random sample is likely to
be representative of the population. But if the population contain dissimilar units, a
random sample may failed to be representative of all kinds of units, in the population.
To improve the result of the sample, the sample design is modified. The population is
divided into different groups containing similar units this groups are called strata.
From each group a sub sample is selected in a random manner. Thus all groups are
represented in the sample and sampling error is reduced. It is called stratified
random sampling.
The size of sub sample from each stratum is frequently in proportion to the size of
the stratum.
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87. 1) Define and classify errors? Describe the various methods to minimize theerrors.
2) What are different methods of expressing concentration?
3) What are primary and secondary standards? Give examples of primary standards used in different
types of titrations. Enlist the ideal properties ofthe primary standard.
4) How do you calculate the equivalent weight and molecular weight of asubstance. Give examples.
5) What is pharmaceutical analysis? Explain different types of analysis. What is its scope in
pharmacy?
6) What is sampling? Discuss sampling techniques.
7) Explain: Validation, Accuracy, Precision, Limit of Detection, Limit of Quantitation,
8) Explain: Specificity, Selectivity, Ruggedness, Robustness, Repeatability, Reproducibility,
Intermediate precision, Linearity and range.
9) Discuss various sources of impurities, effect of impurities, and test for purity.
10) What is analytical method validation? Enumerate validation parameters and define any four.
11)Give the importance of quality control and quality assurance in formulation analysis.
12)Define limit test. Write a principle and reaction of limit test for chloride, iron, arsenic, lead, and
sulphate
87