The document discusses various types of impurities that may be present in pharmaceuticals and medicinal preparations. It provides examples of different categories of impurities including foreign particles, impurities that cause toxicity, impurities that reduce drug activity, and impurities arising from the manufacturing process, raw materials, or storage conditions. The document also describes tests for purity that are used to identify and limit undesirable impurities according to pharmacopeia standards. Limit tests are discussed as quantitative or semi-quantitative methods to control small amounts of impurities and ensure the purity of pharmaceutical substances.
This document discusses pharmaceutical impurities. It defines impurity as unwanted foreign particles other than the active drug. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. The types and amounts of impurities depend on factors like purity of starting materials and purification methods. Limit tests are used to detect and limit specific impurities like chlorides, sulphates, and iron according to pharmacopeia limits. The tests use reactions like precipitation or color changes to compare a sample to a standard of a known impurity level. Maintaining low impurity levels is important for safety, efficacy, and stability of pharmaceutical products.
Quality control drugs and pharmaceuticalsSHIVANEE VYAS
The term quality control is the most important in pharmaceutical industries. It is essential that a good quality product should be available to the doctors for treating patient or for the actual users. The term quality is applied to drugs and drug products which contributing directly or indirectly to the purity, safety & effectiveness of the products.
Impurities in pharmaceutical substancesShaliniBarad
Impurities definition
Sources of impurities
Effect/ type of impurities
Limit test definition
Limit test Importance,
Principle & procedure of Limit test for iron, chloride, sulphate, arsenic & heavy metals.
The document provides an overview of limit tests that are performed on pharmaceutical products to ensure purity and quality. It discusses general impurity limit tests such as clarity of solution, color of solution, insoluble matter, moisture content, and ash values. It also describes specific limit tests for metallic and acid radical impurities. Limit tests are important to control unwanted chemicals and ensure pharmaceuticals are free of potentially harmful impurities within defined acceptable limits. Common methods used include loss on drying, Karl Fischer titration, and analysis of total ash, acid-insoluble ash, sulphated ash, and water-soluble ash. The document emphasizes that limit tests play a vital role in standardizing pharmaceutical chemicals and formulations to guarantee patients receive effective
The document discusses various types of impurities that can be present in pharmaceutical preparations and their sources. It describes six main types of impurities: 1) those that cause toxic or adverse reactions, 2) those that deteriorate the activity of the substance, 3) those that cause incompatibility, 4) those that cause technical problems, 5) those arising from humidity/temperature, and 6) those arising from coloring/flavoring substances. Potential sources of impurities discussed include raw materials, starting materials/reagents, solvents, equipment, intermediates generated during synthesis, and manufacturing defects. Proper control of sources like raw materials, processes, storage conditions, and packaging can help minimize impurities in pharmaceutical preparations.
Define Impurities, 3 Types of Impurities, 13 Sources of Impurities - Raw martials, Reagents used, Methods used, Chemical process, Solvent, Atmospheric contamination, Intermediate process, Defect in manufacturing process, Manufacturing hazards, Impurities due to Storage condition, Impurities due to Crystal packing, Decomposition of product, Adulteration.
This document discusses impurities in pharmaceutical products. It defines impurities as foreign substances present in small amounts that make a product dirty or unacceptable. Impurities can decrease shelf life, stability, therapeutic effects and increase toxicity. Sources of impurities include synthesis, formulation, storage, particulate matter, byproducts, microbial contamination and heavy metals. The quality and safety of pharmaceuticals is highly dependent on controlling impurities. Proper purification of raw materials and intermediates during synthesis is important to minimize synthesis-related impurities. Storage conditions must be suitable to prevent storage-related impurity formation. Water is a major source of heavy metal impurities so distilled or demineralized water is preferred. Overall, stringent control of all potential sources
This document discusses pharmaceutical impurities. It defines impurity as unwanted foreign particles other than the active drug. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. The types and amounts of impurities depend on factors like purity of starting materials and purification methods. Limit tests are used to detect and limit specific impurities like chlorides, sulphates, and iron according to pharmacopeia limits. The tests use reactions like precipitation or color changes to compare a sample to a standard of a known impurity level. Maintaining low impurity levels is important for safety, efficacy, and stability of pharmaceutical products.
Quality control drugs and pharmaceuticalsSHIVANEE VYAS
The term quality control is the most important in pharmaceutical industries. It is essential that a good quality product should be available to the doctors for treating patient or for the actual users. The term quality is applied to drugs and drug products which contributing directly or indirectly to the purity, safety & effectiveness of the products.
Impurities in pharmaceutical substancesShaliniBarad
Impurities definition
Sources of impurities
Effect/ type of impurities
Limit test definition
Limit test Importance,
Principle & procedure of Limit test for iron, chloride, sulphate, arsenic & heavy metals.
The document provides an overview of limit tests that are performed on pharmaceutical products to ensure purity and quality. It discusses general impurity limit tests such as clarity of solution, color of solution, insoluble matter, moisture content, and ash values. It also describes specific limit tests for metallic and acid radical impurities. Limit tests are important to control unwanted chemicals and ensure pharmaceuticals are free of potentially harmful impurities within defined acceptable limits. Common methods used include loss on drying, Karl Fischer titration, and analysis of total ash, acid-insoluble ash, sulphated ash, and water-soluble ash. The document emphasizes that limit tests play a vital role in standardizing pharmaceutical chemicals and formulations to guarantee patients receive effective
The document discusses various types of impurities that can be present in pharmaceutical preparations and their sources. It describes six main types of impurities: 1) those that cause toxic or adverse reactions, 2) those that deteriorate the activity of the substance, 3) those that cause incompatibility, 4) those that cause technical problems, 5) those arising from humidity/temperature, and 6) those arising from coloring/flavoring substances. Potential sources of impurities discussed include raw materials, starting materials/reagents, solvents, equipment, intermediates generated during synthesis, and manufacturing defects. Proper control of sources like raw materials, processes, storage conditions, and packaging can help minimize impurities in pharmaceutical preparations.
Define Impurities, 3 Types of Impurities, 13 Sources of Impurities - Raw martials, Reagents used, Methods used, Chemical process, Solvent, Atmospheric contamination, Intermediate process, Defect in manufacturing process, Manufacturing hazards, Impurities due to Storage condition, Impurities due to Crystal packing, Decomposition of product, Adulteration.
This document discusses impurities in pharmaceutical products. It defines impurities as foreign substances present in small amounts that make a product dirty or unacceptable. Impurities can decrease shelf life, stability, therapeutic effects and increase toxicity. Sources of impurities include synthesis, formulation, storage, particulate matter, byproducts, microbial contamination and heavy metals. The quality and safety of pharmaceuticals is highly dependent on controlling impurities. Proper purification of raw materials and intermediates during synthesis is important to minimize synthesis-related impurities. Storage conditions must be suitable to prevent storage-related impurity formation. Water is a major source of heavy metal impurities so distilled or demineralized water is preferred. Overall, stringent control of all potential sources
This document discusses sources and types of impurities that may be present in pharmaceutical substances. It identifies several potential sources of impurities including raw materials, manufacturing methods, reaction vessels, atmospheric contamination, and errors in manufacturing or packaging processes. The document also categorizes types of impurities as organic impurities, inorganic impurities, or residual solvents. Organic impurities can arise from starting materials, byproducts, intermediates, or degradation products. Inorganic impurities may come from reagents, ligands, catalysts, metals or other materials. Residual solvents are organic or inorganic liquids used in manufacturing that can remain in the final product.
This document discusses sources and types of impurities in pharmaceutical substances. It identifies several potential sources of impurities including raw materials, the manufacturing process, solvents, intermediate products, atmospheric contamination, and manufacturing hazards. Long term exposure to impurities can be harmful to the human body, causing issues like respiratory problems, gastrointestinal symptoms, cancer, and more. Careful control and monitoring of the manufacturing process is important to limit impurities in pharmaceutical drugs.
Pharmaceutical impurity and limit test_by_Raju_Yadav_M.S._Pharm_NIPER_2020RajYadav238
The document discusses various sources of impurities in pharmaceuticals such as raw materials, reagents, manufacturing processes, storage conditions, and defines an impurity as any undesired substance that affects the purity of the material. It explains the effects of impurities including toxicity, decreased potency, and incompatibility with other substances. Tests for purity are prescribed by pharmacopoeias to ensure freedom from undesirable impurities and establish limits of tolerance for common impurities.
Definition of Impurity
Types of Impurities
Sources of Impurity
foreign unwanted matter present in a compound which are differ from the actual molecular formula.
According to ICH “An impurity in a drug of the new drug substance that is not the substance”.
Chemically a compound is impure if it contains undesirable foreign matter i.e. impurities. Thus chemical purity is freedom from foreign matter
Impurities can have unwanted pharmacological or toxicological effect that seriously impact product quality and patient safety.
The International Conference on Harmonization (ICH) has formulated a workable guideline regarding the control of impurities.
Impurities in pharmaceutical are the unwanted chemicals that remains with the active pharmaceutical ingredient (API’s), or develop during formulation or upon aging of both API and formulated API’s to medicine.
The presence of the unwanted chemicals, even in small amount , may influence the efficacy and safety of pharmaceutical product
This document discusses pharmaceutical impurities, which are unwanted chemicals that remain with active pharmaceutical ingredients or develop during formulation or aging. Impurities can come from raw materials, intermediates, reagents, catalysts, solvents, reaction vessels, improper storage, cross contamination, manufacturing errors, packaging errors, microbial contamination, chemical instability, storage containers, or atmospheric contamination. The presence of impurities can affect the efficacy, safety, and purity of pharmaceutical products. Common impurities include metals, microbes, residual solvents, and degradation products. Strict controls are needed in manufacturing to minimize impurities.
Impurities in pharmaceuticals are the unwanted chemicals that remain with the active pharmaceutical ingredients (APIs), or develop during formulation, or upon aging of both API and formulated APIs to medicines.
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY AND LIMIT TESTSUJATA WANKHEDE
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY, INTRODUCTION TO LIMIT TESTS, LIMIT TEST OF IRON, CHLORIDE, SULPHATE, ARSENIC AND THERE DIAGRAMS WITHTHE PRINCIPAL AND PROCEDURE OF ALL THE LIMIT TEST WITH THEIR RESULTS
This document discusses impurities in pharmaceuticals and limit testing. It defines impurity as any undesired material that affects the purity of the substance. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. Limit tests are used to check pharmaceuticals for common toxic impurities like arsenic, lead, iron and ensure they are below safe levels. Proper testing of impurities is important to ensure pharmaceuticals are safe and effective.
The document discusses impurities in pharmaceutical substances and limit tests. It provides context on the history of pharmacopoeias and defines impurities as unwanted chemicals that can remain with active pharmaceutical ingredients or develop during formulation. Potential sources and types of impurities are discussed.
Key limit tests for common impurities like chloride, sulfate, iron, and heavy metals are described. The principles, reactions, procedures, observations and reasons for the tests are explained. Limit tests are designed to identify and control small quantities of impurities using quantitative or semi-quantitative comparisons. The document emphasizes that even small amounts of impurities can impact product quality, efficacy, and patient safety.
The document discusses argentometric titration methods. It provides context that these reactions have limited usage due to co-precipitation effects not providing accurate precipitate composition, a limited choice of indicators, and solubility product playing a major role. It then defines solubility product constant and lists ideal conditions for precipitation titrations. The document outlines two classes of argentometric titrations and provides context on silver nitrate and procedures for a titration experiment and calculations.
The document discusses sources of impurities in pharmaceuticals. Impurities can arise from raw materials, reagents used in manufacturing, the manufacturing process itself, storage conditions, and decomposition over time. Common impurities include heavy metals like arsenic and lead. The presence of impurities can negatively impact safety, efficacy, and shelf life of pharmaceutical products. Pharmacopoeias set limits for common impurities and prescribe tests to evaluate purity.
This document discusses limitations of Lewis acid-base reactions, properties of buffer solutions, buffer capacity, the Henderson-Hasselbalch equation, and applications of buffers in pharmacy. It also covers general principles for adjusting solutions to isotonicity and its importance, types of impurities found in pharmaceutical substances, sources of impurities, effects of impurities, and limit tests for chloride, sulfate, iron, heavy metals, lead, and arsenic. Limit tests are used to identify and control small quantities of impurities that may be present in substances.
1. The document discusses impurities that can be present in pharmaceutical substances, including sources of impurities from raw materials, reagents, manufacturing processes, storage conditions, and other factors.
2. Limit tests are described as quantitative or semi-quantitative tests used to identify and control small amounts of impurities that may be present. Specific examples of limit tests for sulfate, iron, and arsenic are provided.
3. The limit test for iron involves the reaction of iron in an ammonical solution with thioglycollic acid and citric acid to form a ferrous thioglycolate complex, producing a pale pink to deep reddish purple color in an alkaline medium.
The document discusses primary and secondary standards used in volumetric analysis. It defines primary standards as highly pure, stable chemicals that can be weighed easily and used directly for standardization. Secondary standards have lower purity and stability than primary standards but can be used indirectly after standardization against a primary standard. Common primary standards mentioned include potassium hydrogen phthalate and anhydrous sodium carbonate. Secondary standards discussed include sodium hydroxide solutions, which are standardized against primary acids due to their hygroscopic nature. The key requirements for a chemical to be used as a primary standard are that it is pure, stable, non-hygroscopic, and has a high molecular weight.
Topic 1 INTRODUCTION AND QUALITY CONTROL (1)PC.pptxVrushaliDesai7
This document provides an introduction to pharmaceutical chemistry and discusses sources of errors and impurities in pharmaceuticals. It describes how impurities can affect pharmacopoeial substances by making them toxic, decreasing therapeutic effects, or changing physical/chemical properties. Common impurity tests are outlined, including limit tests for chlorides, sulfates, arsenic, and iron which use chemical reactions to identify impurities and compare results to standards. Proper procedures and reasons for each test are explained in detail.
chemical oxygen demand -analysis using APHA manualSHERIN RAHMAN
This document provides details on methods for analyzing chemical oxygen demand (COD) using standards from the American Public Health Association (APHA) manual. It describes three common COD analysis methods: the open reflux method, closed reflux titrimetric method, and closed reflux colorimetric method. For each method, it outlines the key steps, including refluxing samples with dichromate and sulfuric acid, and then titrating or measuring color change to determine the amount of dichromate consumed and calculate the COD level. The document also discusses interferences, limitations, sampling, and analysis of COD values both above and below 50 mg O2/L.
Impurities can arise from various sources in pharmaceutical preparations including raw materials, equipment, reagents, solvents, and the manufacturing process itself. Raw materials may introduce impurities like heavy metals or other foreign particles. The equipment, reagents, and solvents used can also lead to impurities if not properly purified or washed. Additionally, the chemical reactions, intermediates, defects in process, and manufacturing hazards have the potential to result in impurities being carried through to the final product. Strict specifications and analytical testing are required to identify, quantify, and limit both known and unknown impurities for safety and efficacy.
Impurities can arise from various sources in pharmaceutical preparations including raw materials, equipment, reagents, solvents, and the manufacturing process itself. Raw materials may introduce impurities like heavy metals, chemicals used to eliminate other impurities can become impurities themselves if not removed properly. The equipment, intermediates generated during synthesis, chemical reactions used, and defects in manufacturing can all contribute to impurities being introduced. Proper specifications and analytical procedures are needed to identify, quantify, and limit both known and unknown impurities.
Unit 1 PHARMACEUTICAL INORGANIC CHEMISTRYSayali Powar
The document discusses various limit tests performed as per the Indian Pharmacopoeia to determine the presence of impurities below specified limits. It describes the principles, procedures and observations for limit tests of chloride, sulphate, iron, arsenic, heavy metals and lead. Limit tests involve comparing the color or turbidity developed in a test sample to a standard under defined reaction conditions. They provide a semi-quantitative analysis to check if impurity levels pass specified limits in the pharmacopoeia.
This document discusses sources and types of impurities that may be present in pharmaceutical substances. It identifies several potential sources of impurities including raw materials, manufacturing methods, reaction vessels, atmospheric contamination, and errors in manufacturing or packaging processes. The document also categorizes types of impurities as organic impurities, inorganic impurities, or residual solvents. Organic impurities can arise from starting materials, byproducts, intermediates, or degradation products. Inorganic impurities may come from reagents, ligands, catalysts, metals or other materials. Residual solvents are organic or inorganic liquids used in manufacturing that can remain in the final product.
This document discusses sources and types of impurities in pharmaceutical substances. It identifies several potential sources of impurities including raw materials, the manufacturing process, solvents, intermediate products, atmospheric contamination, and manufacturing hazards. Long term exposure to impurities can be harmful to the human body, causing issues like respiratory problems, gastrointestinal symptoms, cancer, and more. Careful control and monitoring of the manufacturing process is important to limit impurities in pharmaceutical drugs.
Pharmaceutical impurity and limit test_by_Raju_Yadav_M.S._Pharm_NIPER_2020RajYadav238
The document discusses various sources of impurities in pharmaceuticals such as raw materials, reagents, manufacturing processes, storage conditions, and defines an impurity as any undesired substance that affects the purity of the material. It explains the effects of impurities including toxicity, decreased potency, and incompatibility with other substances. Tests for purity are prescribed by pharmacopoeias to ensure freedom from undesirable impurities and establish limits of tolerance for common impurities.
Definition of Impurity
Types of Impurities
Sources of Impurity
foreign unwanted matter present in a compound which are differ from the actual molecular formula.
According to ICH “An impurity in a drug of the new drug substance that is not the substance”.
Chemically a compound is impure if it contains undesirable foreign matter i.e. impurities. Thus chemical purity is freedom from foreign matter
Impurities can have unwanted pharmacological or toxicological effect that seriously impact product quality and patient safety.
The International Conference on Harmonization (ICH) has formulated a workable guideline regarding the control of impurities.
Impurities in pharmaceutical are the unwanted chemicals that remains with the active pharmaceutical ingredient (API’s), or develop during formulation or upon aging of both API and formulated API’s to medicine.
The presence of the unwanted chemicals, even in small amount , may influence the efficacy and safety of pharmaceutical product
This document discusses pharmaceutical impurities, which are unwanted chemicals that remain with active pharmaceutical ingredients or develop during formulation or aging. Impurities can come from raw materials, intermediates, reagents, catalysts, solvents, reaction vessels, improper storage, cross contamination, manufacturing errors, packaging errors, microbial contamination, chemical instability, storage containers, or atmospheric contamination. The presence of impurities can affect the efficacy, safety, and purity of pharmaceutical products. Common impurities include metals, microbes, residual solvents, and degradation products. Strict controls are needed in manufacturing to minimize impurities.
Impurities in pharmaceuticals are the unwanted chemicals that remain with the active pharmaceutical ingredients (APIs), or develop during formulation, or upon aging of both API and formulated APIs to medicines.
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY AND LIMIT TESTSUJATA WANKHEDE
INTRODUCTION TO PHARMACEUTICAL CHEMISTRY, INTRODUCTION TO LIMIT TESTS, LIMIT TEST OF IRON, CHLORIDE, SULPHATE, ARSENIC AND THERE DIAGRAMS WITHTHE PRINCIPAL AND PROCEDURE OF ALL THE LIMIT TEST WITH THEIR RESULTS
This document discusses impurities in pharmaceuticals and limit testing. It defines impurity as any undesired material that affects the purity of the substance. Impurities can come from raw materials, reagents, manufacturing processes, storage conditions, or deliberate adulteration. Limit tests are used to check pharmaceuticals for common toxic impurities like arsenic, lead, iron and ensure they are below safe levels. Proper testing of impurities is important to ensure pharmaceuticals are safe and effective.
The document discusses impurities in pharmaceutical substances and limit tests. It provides context on the history of pharmacopoeias and defines impurities as unwanted chemicals that can remain with active pharmaceutical ingredients or develop during formulation. Potential sources and types of impurities are discussed.
Key limit tests for common impurities like chloride, sulfate, iron, and heavy metals are described. The principles, reactions, procedures, observations and reasons for the tests are explained. Limit tests are designed to identify and control small quantities of impurities using quantitative or semi-quantitative comparisons. The document emphasizes that even small amounts of impurities can impact product quality, efficacy, and patient safety.
The document discusses argentometric titration methods. It provides context that these reactions have limited usage due to co-precipitation effects not providing accurate precipitate composition, a limited choice of indicators, and solubility product playing a major role. It then defines solubility product constant and lists ideal conditions for precipitation titrations. The document outlines two classes of argentometric titrations and provides context on silver nitrate and procedures for a titration experiment and calculations.
The document discusses sources of impurities in pharmaceuticals. Impurities can arise from raw materials, reagents used in manufacturing, the manufacturing process itself, storage conditions, and decomposition over time. Common impurities include heavy metals like arsenic and lead. The presence of impurities can negatively impact safety, efficacy, and shelf life of pharmaceutical products. Pharmacopoeias set limits for common impurities and prescribe tests to evaluate purity.
This document discusses limitations of Lewis acid-base reactions, properties of buffer solutions, buffer capacity, the Henderson-Hasselbalch equation, and applications of buffers in pharmacy. It also covers general principles for adjusting solutions to isotonicity and its importance, types of impurities found in pharmaceutical substances, sources of impurities, effects of impurities, and limit tests for chloride, sulfate, iron, heavy metals, lead, and arsenic. Limit tests are used to identify and control small quantities of impurities that may be present in substances.
1. The document discusses impurities that can be present in pharmaceutical substances, including sources of impurities from raw materials, reagents, manufacturing processes, storage conditions, and other factors.
2. Limit tests are described as quantitative or semi-quantitative tests used to identify and control small amounts of impurities that may be present. Specific examples of limit tests for sulfate, iron, and arsenic are provided.
3. The limit test for iron involves the reaction of iron in an ammonical solution with thioglycollic acid and citric acid to form a ferrous thioglycolate complex, producing a pale pink to deep reddish purple color in an alkaline medium.
The document discusses primary and secondary standards used in volumetric analysis. It defines primary standards as highly pure, stable chemicals that can be weighed easily and used directly for standardization. Secondary standards have lower purity and stability than primary standards but can be used indirectly after standardization against a primary standard. Common primary standards mentioned include potassium hydrogen phthalate and anhydrous sodium carbonate. Secondary standards discussed include sodium hydroxide solutions, which are standardized against primary acids due to their hygroscopic nature. The key requirements for a chemical to be used as a primary standard are that it is pure, stable, non-hygroscopic, and has a high molecular weight.
Topic 1 INTRODUCTION AND QUALITY CONTROL (1)PC.pptxVrushaliDesai7
This document provides an introduction to pharmaceutical chemistry and discusses sources of errors and impurities in pharmaceuticals. It describes how impurities can affect pharmacopoeial substances by making them toxic, decreasing therapeutic effects, or changing physical/chemical properties. Common impurity tests are outlined, including limit tests for chlorides, sulfates, arsenic, and iron which use chemical reactions to identify impurities and compare results to standards. Proper procedures and reasons for each test are explained in detail.
chemical oxygen demand -analysis using APHA manualSHERIN RAHMAN
This document provides details on methods for analyzing chemical oxygen demand (COD) using standards from the American Public Health Association (APHA) manual. It describes three common COD analysis methods: the open reflux method, closed reflux titrimetric method, and closed reflux colorimetric method. For each method, it outlines the key steps, including refluxing samples with dichromate and sulfuric acid, and then titrating or measuring color change to determine the amount of dichromate consumed and calculate the COD level. The document also discusses interferences, limitations, sampling, and analysis of COD values both above and below 50 mg O2/L.
Impurities can arise from various sources in pharmaceutical preparations including raw materials, equipment, reagents, solvents, and the manufacturing process itself. Raw materials may introduce impurities like heavy metals or other foreign particles. The equipment, reagents, and solvents used can also lead to impurities if not properly purified or washed. Additionally, the chemical reactions, intermediates, defects in process, and manufacturing hazards have the potential to result in impurities being carried through to the final product. Strict specifications and analytical testing are required to identify, quantify, and limit both known and unknown impurities for safety and efficacy.
Impurities can arise from various sources in pharmaceutical preparations including raw materials, equipment, reagents, solvents, and the manufacturing process itself. Raw materials may introduce impurities like heavy metals, chemicals used to eliminate other impurities can become impurities themselves if not removed properly. The equipment, intermediates generated during synthesis, chemical reactions used, and defects in manufacturing can all contribute to impurities being introduced. Proper specifications and analytical procedures are needed to identify, quantify, and limit both known and unknown impurities.
Unit 1 PHARMACEUTICAL INORGANIC CHEMISTRYSayali Powar
The document discusses various limit tests performed as per the Indian Pharmacopoeia to determine the presence of impurities below specified limits. It describes the principles, procedures and observations for limit tests of chloride, sulphate, iron, arsenic, heavy metals and lead. Limit tests involve comparing the color or turbidity developed in a test sample to a standard under defined reaction conditions. They provide a semi-quantitative analysis to check if impurity levels pass specified limits in the pharmacopoeia.
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2. Impurities are defined as a foreign particle that affects the purity of a substance.
Usually, impurities occurring in many pharmaceutical or medicinal preparations may
be of the following types.
.
.
1. Foreign particle that bring about adverse or toxic reactions when present in
excess beyond their limits. Example: lead, heavy metals, arsenic etc.
2. Impurities which may not cause toxic effects but bring about deterioration of the
activity of chemical. Example: hard soap containing excess of water.
3. Impurities that cause incompatibility of active ingredient with other substance or
which reduce the properties of active ingredient
4. Impurities which may lead to technical problems in the applications of the
substance. Example: presence of carbonate in ammonia solution, presence of
KIO3 in KI solution
.
3. 5. Impurities arising due to humidity temperature.
Example: presence of very low amount of moisture may enable substance to get
oxidized easily or may reduce its free-flowing characteristics
.
.
6. Impurities arising due to colouring and flavoring substances. These impurities
can be detected by changes in colour, odour, taste and appearance
Examples: Presences of phenolic compounds decolourize sodium salicylat e,
presence of minute quantities of magnesium salt causes dampening of sodium
chloride.
7. Impurities which may alter the physical and chemical properties of the
substance.
8. Impurities which decrease the shelf – life
4.
5. Raw materials:
Method / process of manufacture:
Starting materials or reagents used:
Examples:
Calcium carbonate is prepared from the reagents calcium chloride and sodium
carbonate. Hence, calcium carbonate by this process is associated with alkali
(Na2CO3) and soluble chlorides. If the CaCO3 product is not washed properly to
remove excess of Na2CO3and chlorides, then they get carried as impurities. Due to
this reason, pharmacopeia has prescribed limits for soluble chlorides and alkali for
CaCO3
6. Reagents employed to eliminate other impurities:
Example:
Barium is employed to remove excess sulphate in the synthesis of potassium
bromide. Improper usage results in the presence of very small amounts of
barium in the final product.
Solvents or vehicles used in the manufacturing
Water is the most commonly used solvent in many preparations
8. Intermediates generated during the synthesis
Example: In the preparation of potassium iodide ( KI) from potassium
hydroxide and iodine, potassium iodate (KIO3) is formed as an intermediate.
KIO3 is evaporated to dryness and the residue obtained is heated with charcoal
to get KI. Incomplete or improper conversion of KIO3 is liable to be carried as
an impurity to the final preparation which is desirable.
Chemical methods used in the manufacturing process:
Example:
Potassium iodide is synthesized from kelp (ash of a sea weed). When sea weed
containing nitrogenous organic matter is heated at very high temperature in the
presence of alkli, cyanides are generated. These cyanides may get incorporated as an
impurity
9. Defects in the process of manufacturing
Examples:
Synthesis of calcium chloride involves addition of pure calcium carbonate to
slightly excess quantity of dilute hydrochloric acid with continuous stirring
followed by filtration and concentration of filtrate to give CaCl2 crystals. If the
ingredients are not mixed properly or if any amount of HCl passes through the filter
or if the concentration is not properly carried out, then it affects the final product.
Manufacturing hazards:
i. Arbitrary inclusion of particulate matter:
Eye ointments packed in metal tubes made up of tin, aluminum generally get
contaminated due to the extrusion of metal particles from the packing material.
The
extent of contamination depends upon the viscosity of the ointment. As the
viscosity of the ointment increases, the extent of extrusion increases.
10. ii. Arbitrary inclusion of microorganisms:
iii. Cross contamination:
Conditions of storage:
a) Carless storage:
Example:
Ferrous sulphate should be stored in air tight containers. Improper storage
leads to the conversion of soluble ferrous sulphate to insoluble ferric oxide in
the presence of air and moisture
11. b) Filthy matter:
c) Effect of container materials
Examples:
Salicylic acid reacts with metal tubes, therefore, it should not be stored in metal
tubes unless and until they are lacquered internally.
Atropine sulphate injection should be strictly packed in glass ampoules as it offers
hydrolytic resistance. Therefore, a container should be so selected such that it is
suitable for storing the preparation and does not contribute to its degradation.
There are grades of glass containers available.
Type I: it exhibits very high hydrolytic resistance. It is a neutral glass.
Type II: it is formed by the surface treatment of glass and exhibit very high
hydrolytic resistance. Type I and II glasses can be differentiated from each other by
crushed glass test.
Type III: it possesses very limited hydrolytic resistance.
Aqueous solutions of injections should be stored in either type I or II glass
containers while non – aqueous solutions as well as injectable solids are stored in
type III glass containers after complying with the test for hydrolytic resistance.
12. 4. Atmospheric / environmental conditions:
Example: if sodium hydroxide is exposed to air for very long periods during
the
process of manufacturing it reacts with carbon dioxide and gets converted
to
sodium carbonate. This sodium carbonate gets incorporated into NaOH and
serves
as an impurity
5. Packing Errors:
6. Deliberate adulteration or international substitution
13. Test for purity:
Pharmacopoeia prescribes the “Test for purity” for pharmaceutical substances to
check their freedom from undesirable impurities. 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
Physicochemical constants (Iodine value, saponification value, melting point,
refractive index etc.)
Acidity, alkalinity, pH
Humidity (Estimation of moisture)
14. Cations and anions
Ash
Arsenic or lead
Loss on drying
Loss on ignition
15. 1. Title of the Monograph
3.Formula &Molecular weight
4. Chemical name
5. Category
7.Description
10. Identification
11.Test for purity
12.Assay
13.Storage
14.Labelling
2.Synonyms
6.Doses
8.Solubility
9.Standards
16. Storage Condition Limit
Room Temperature 20° to 25°
Cool Storage Condition 8° to 15°
Cold Storage condition 2° to 8°
Fridge Storage condition -4° to 2°
17. Limit tests are quantitative or semi-quantitative tests designed to identify and
control small quantities of impurity, which are likely to be present in the
substance. The quantity of any one impurity in an official substance is often
small, and consequently the visible reaction response to any test for that impurity
is also small. The design of individual tests is therefore important if errors are to
be avoided in the hands of different operators.
Specificity of the test
Any test used as a limit test must, of necessity, give some form of selective
reaction with the trace impurity. Many tests used for the detection of inorganic
impurities in official inorganic chemicals are based upon the separations involved
in inorganic qualitative analysis.
Sensitivity of the test The degree of sensitivity required in a limit test varies
enormously according to the standard of purity demanded by the monograph.
The sensitivity of most tests is dependent upon a number of variable factors
concentration of the solute, precipitating reagent, duration of the reaction,
temperature, and the nature and concentration of other substances unavoidably
present in solution
18. Types of limit test
1. Test in which there is no visible reaction
2. Comparison methods
3. Quantitative determination
19.
20. General precaution
The liquid used must be clean and filtered if necessary
The Nessler cylinder must be made of colorless glass and of the same
inner diameter
Detecting opalescence or color development must be performed in
daylight
When comparing turbidity it should be done against black background
When comparing color it should be done against white background
21. Pharmacopoeia does not prescribe any numerical value of limit test for
chlorides, sulphate and iron because limit test is based on the simple
comparison of opalescence or colour between the test and standard solution
prescribed according to pharmacopoeia.
In this type of limit test, the extent of turbidity or opalescence or colour
produced in influenced by the presence of other impurities present in the
substance and also by variation in time and method of performance of test.
Thus the pharmacopoeia does not prescribe any numerical value of the limit
22. The limit test involve simple comparisons of opalescence, turbidity, or
colour with standard.
These are semi-qualitative reactions in which extent of impurities present
can be estimated by comparing visible reaction response of the test and
standard.
By this way, extent of reaction is readily determined by direct comparison
of test solution with standard. So pharmacopoeia prefers comparison
methods.
23. Chloride limit test :Limit test of chloride is based on the reaction of soluble
chloride with silver nitrate in presence of dilute nitric acid to form silver chloride,
which appears as solid particles (Opalescence) in the solution.
Soluble chloride present as impurity
The silver chloride produced in the presence of dilute Nitric acid makes the test
solution turbid, the extent of turbidity depending upon the amount of Chloride
present in the substance is compared with the standard opalescence produced by
the addition of Silver nitrate to a standard solution having a known amount of
chloride and the same volume of dilute nitric acid as used in the test solution.
24.
25.
26. Observation:
The opalescence produce in sample solution should not be greater than standard
solution. If opalescence produces in sample solution is less than the standard
solution, the sample will pass the limit test of chloride and visa versa.
Reasons:
Nitric acid is added in the limit test of chloride to make solution acidic and
helps silver chloride precipitate to make solution turbid at the end of process
as Dilute HNO3 is insoluble in AgCl.
Certain modification are required to be adopted for the preparation of the
solution depending upon the type of compound which is taken.
27.
28.
29.
30. Limit test for sulphate: The Sulfate Limit Test is designed to determine the
allowable limit of sulfate contained in a sample. Principle: Limit test of
sulphate is based on the reaction of soluble sulphate with barium chloride in
presence of dilute hydrochloric acid to form barium sulphate which appears as
solid particles (turbidity) in the solution.
Then comparison of turbidity is done with a standard turbidity obtained
from a known amount of Sulphate and same volume of dilute
Hydrochloric acid have been added to both solutions. The barium chloride
test solution in the IP has been replaced by Barium sulphate reagent which
is having barium chloride, sulphate free alcohol and a solution of
potassium sulphate. Potassium sulphate has been added to increase the
sensitivity of the test.
31.
32. Barium sulphate reagent contains barium chloride, sulphate free alcohol and
small amount of potassium sulphate.
Observation:
The turbidity produce in sample solution should not be greater than standard
solution. If turbidity produces in sample solution is less than the standard
solution, the sample will pass the limit test of sulphate and vice versa.
Reasons:
Hydrochloric acid helps to make solution acidic. Potassium sulphate is used to
increase the sensitivity of the test by giving ionic concentration in the reagent.
Alcohol helps to prevent super saturation and so produces a more uniform
opalescence
33. Limit test for Iron : Limit test of Iron is based on the reaction of iron in
ammonical solution with thioglycollic acid in presence of citric acid to form
iron thioglycolate (Ferrous thioglycolate complex) which produces pale pink
to deep reddish purple color in alkaline media. Thioglycolic acid is used as
reducing agent.
The color of the Ferrous thioglycolate complex fades in the presence of air due
to oxidation. Also, the color is destroyed in presence of oxidizing agents and
strong alkalis. The purple color is developed only in alkaline media. So
ammonia solution is used.
34. But ammonia reacts with iron, forms precipitate of ferrous hydroxide. Thus
citric acid is used which prevents the precipitate of iron with Ammonia by
forming a complex with iron as iron citrate.
35.
36. Observation: The purple color produce in sample solution should not be
greater than standard solution. If purple color produces in sample solution is
less than the standard solution, the sample will pass the limit test of iron and
vice versa.
Reasons:
Citric acid forms complex with metal cation and helps precipitation of iron by
ammonia by forming a complex with it.
Thioglycolic acid helps to oxidize iron (II) to iron (III).
37. Ammonia is added to make solution alkaline. The pale pink color is visible
only in the alkaline media. The color is not visible in acidic media as ferrous
thioglycolate complex decomposes in high acidic media.
38. Limit test for Arsenic:
Arsenic is a well-known undesirable and harmful impurity which is present in
medicinal substances. All pharmacopoeias prescribe a limit test for it.
Pharmacopoeial method is based on the Gutzeit test.
All the special reagents used in the limit test for Arsenic are marked and
distinguished by letter ‘As T’, which means that they all should be Arsenic free
and should themselves conform to the test forArsenic.
39. Principle: Limit test of Arsenic is based on the reaction of arsenic gas with
hydrogen ion to form yellow stain on mercuric chloride paper in presence of
reducing agents like potassium iodide. It is also called as Gutzeit test and
requires special apparatus.
Arsenic, present as arsenic acid ((H3AsO4) in the sample is reduced to
arsenious acid (H3AsO3) by reducing agents like potassium iodide, stannous
acid, zinc, hydrochloric acid, etc. Arsenious acid is further reduced to arsine
(gas) (AsH3) by hydrogen and reacts with mercuric chloride paper to give a
yellow stain
43. When the sample is dissolved in acid, the Arsenic present in the sample gets
converted to Arsenic acid.
By action of reducing agents like Potassium iodide, stannous acid etc., Arsenic
acid gets reduced to arsenious acid.
The nascent hydrogen formed during the reaction, further reduces Arsenious
acid to Arsine gas, which reacts with mercuric chloride paper, giving a yellow
stain.
44. Apparatus:
It is having a wide mouthed glass bottle of 120 mL capacity having mouth of
about 2.5 cm in diameter. This bottle is fitted with a rubber bung through which
passes a glass tube, 20 cm long. External diameter=0.8 cm &Internal
diameter=0.65 cm
The tube is constricted at its lower end extremity to about 1 mm diameter and
there is blown a hole, not less than 2 mm in diameter, in the side of the tube near
the constricted part.
The upper end of the glass tube is fitted with two rubber bungs(25 mm x 25 mm),
each having a hole bored centrally and exactly 6.5 mm in diameter.
45. One of the bungs has been fitted to the upper end of the tube, while the second
bung has to be fitted upon the first bung in such a way that the mercuric
chloride paper gets exactly sandwiched between the central perforation of the
two.
The bungs are kept in close contact by using rubber band or spring clip in such
a manner that the gas evolved from the bottle must have to pass through the
0.65 mm internal circle of mercuric chloride paper.
During the test, the evolved gases have been passing through the side hole, the
lower hole serving as an exit for water which condenses in the constricted part
of the tube.
An important feature has been the standardization of the area of Mercuric
chloride paper which is exposed to the reaction of arsine gas.
46.
47. Reasons: Stannous chloride is used for complete evolution of arsine. Zinc,
potassium iodide and stannous chloride is used as a reducing agent.
Hydrochloride acid is used to make the solution acidic Lead acetate paper are
used to trap any hydrogen sulphide which may be evolved along with arsine.
48. Use of stannated Hydrochloric acid: If pure zinc and HCl are used, the steady
evolution of gas does not occur. This produces improper stain (e.g slow
evolution produces short but intense stain while rapid evolution of gas
produces long but diffused stain.) So, to get steady evolution of gas, stannated
hydrochloric acid is used.
Use of Lead Acetate solution: H2Sgas may be formed during the experiment
as zinc contains sulphides as impurities. It gives black stain to HgCl2 paper
and so will interfere the test.
49. Hence, gases evolved are passed through cotton wool plug moistened with lead
acetate, where H2S gas is trapped as PbS. Use of Potassium iodide: KI is
converted to HI which brings about reduction of unreacted pentavalent arsenic
to trivalent Arsenic. Thus, reproducible results can be obtained. If it is not
used, then some pentavalent Arsenic may remain unreacted.
50. Limit test for heavy metals
The limit test for heavy metals is designed to determine the content of metallic
impurities that are coloured by hydrogen sulphide or sodium sulphide under
the condition of the test should not exceed the heavy metal limits given under
the individual monograph. The heavy metals (metallic impurities) may be
iron, copper, lead, nickel, cobalt, bismuth, antimony etc.. The limit for heavy
metals is indicated in the individual monograph in term of ppm of lead i.e. the
parts of lead per million parts of the substance being examined
51. In substances the proportion of any such impurity (Heavy metals) has been expressed
as the quantity of lead required to produce a color of equal depth as in a standard
comparison solution having a definite quantity of lead nitrate. The quantity is stated
as the heavy metal limit and is expressed as parts of lead (by weight) per million parts
of the test substance. The limit test for heavy metals has been based upon the
reaction of the metal ion with hydrogen sulphide, under the prescribed conditions of the
test causing the formation of metal sulphides.
• These remain distributed in colloidal state, and give rise to a brownish coloration.