The document discusses research conducted to optimize the lyophilization process for Drug-X, which has both stable and unstable polymorphic forms. Characterization of Drug-X and the excipient Mannitol was performed using DSC, TGA, and XRD. Freeze drying parameters were optimized using DSC. Six batches were produced varying freeze drying conditions and analyzed for water content and solid state using KF titration and XRD. Studies on the effect of relative humidity on Drug-X found that the monohydrate form is stable between 20-30% RH, with the anhydrous form forming at lower or higher humidity levels. Optimal storage conditions for the monohydrate were determined to be below 25°
This document summarizes an experiment to synthesize the sulfa drug sulfanilamide through a multi-step process involving the acetylation of aniline and other reactions. The experiment had a very low yield of less than 1% sulfanilamide, likely due to product loss during filtration and some reactions not going to completion. While the target compound sulfanilamide was produced, as confirmed by its melting point and IR spectroscopy, improvements to the technique are needed to increase the yield. The synthesis of sulfanilamide and other sulfa drugs provides opportunities to study their antimicrobial mechanisms and develop new therapeutic agents.
Disintegration Properties and Drug Release Profiles of Sodium Alginate Films ...CrimsonPublishersRDMS
Disintegration Properties and Drug Release Profiles of Sodium Alginate Films Modified with Additives in Yoshifumi Murata* in Crimson Publishers: Journal of Materials Science & Technology
QUANTITATIVE DETERMINATION OF PRESERVATIVES, EMULSIFIERS, AND COLOURING MATER...CARE COLLEGE OF PHARMACY
This document describes methods for quantitatively determining preservatives, emulsifiers, and colouring materials found in foods and pharmaceuticals. It discusses using thin-layer chromatography to identify common preservatives like methyl paraben and propyl paraben, and extracting and identifying emulsifiers like polysorbate 80. Gas chromatography methods are provided for determining mono- and diglycerides. Finally, it outlines extracting and identifying food dyes from candy coatings using yarn and ammonia.
1. The document discusses methods for determining loss on drying, weight per mL (density), and water content of substances through various techniques.
2. Loss on drying is determined by placing a sample in a drying apparatus under specified conditions until it reaches a constant mass, allowing the calculation of mass lost due to moisture.
3. Weight per mL (density) can be found using a pycnometer to measure the weight and volume of a liquid sample, or through other techniques like an oscillating transducer density meter.
The document describes various tests conducted on pharmaceutical samples, including:
- Weight/ml and density tests to determine the weight of a liquid per milliliter.
- Total solids tests to determine the residue left after drying a sample.
- Ash testing to determine acid soluble, acid insoluble, water soluble and sulphated ash contents.
- Toxicity tests conducted on finished drug products and packaging to assess safety.
- Loss on drying tests to determine volatile content lost after drying under specified conditions.
- Moisture content tests using thermogravimetric analysis or Karl Fischer titration.
This document outlines various physical evaluation tests performed on crude drugs, including moisture content, optical rotation, refractive index, melting point, viscosity, solubility, ash values, extractive values, and volatile oil content. These tests are used to standardize crude drugs and determine their composition and purity. Key tests mentioned include determining moisture content by heating to a constant weight, measuring viscosity and refractive index, identifying melting point ranges, assessing solubility in various solvents, calculating ash, water-soluble extract, and alcohol-soluble extract values, and quantifying volatile oil content. The results of these tests provide information about crude drug identity and quality.
This document summarizes an experiment to synthesize the sulfa drug sulfanilamide through a multi-step process involving the acetylation of aniline and other reactions. The experiment had a very low yield of less than 1% sulfanilamide, likely due to product loss during filtration and some reactions not going to completion. While the target compound sulfanilamide was produced, as confirmed by its melting point and IR spectroscopy, improvements to the technique are needed to increase the yield. The synthesis of sulfanilamide and other sulfa drugs provides opportunities to study their antimicrobial mechanisms and develop new therapeutic agents.
Disintegration Properties and Drug Release Profiles of Sodium Alginate Films ...CrimsonPublishersRDMS
Disintegration Properties and Drug Release Profiles of Sodium Alginate Films Modified with Additives in Yoshifumi Murata* in Crimson Publishers: Journal of Materials Science & Technology
QUANTITATIVE DETERMINATION OF PRESERVATIVES, EMULSIFIERS, AND COLOURING MATER...CARE COLLEGE OF PHARMACY
This document describes methods for quantitatively determining preservatives, emulsifiers, and colouring materials found in foods and pharmaceuticals. It discusses using thin-layer chromatography to identify common preservatives like methyl paraben and propyl paraben, and extracting and identifying emulsifiers like polysorbate 80. Gas chromatography methods are provided for determining mono- and diglycerides. Finally, it outlines extracting and identifying food dyes from candy coatings using yarn and ammonia.
1. The document discusses methods for determining loss on drying, weight per mL (density), and water content of substances through various techniques.
2. Loss on drying is determined by placing a sample in a drying apparatus under specified conditions until it reaches a constant mass, allowing the calculation of mass lost due to moisture.
3. Weight per mL (density) can be found using a pycnometer to measure the weight and volume of a liquid sample, or through other techniques like an oscillating transducer density meter.
The document describes various tests conducted on pharmaceutical samples, including:
- Weight/ml and density tests to determine the weight of a liquid per milliliter.
- Total solids tests to determine the residue left after drying a sample.
- Ash testing to determine acid soluble, acid insoluble, water soluble and sulphated ash contents.
- Toxicity tests conducted on finished drug products and packaging to assess safety.
- Loss on drying tests to determine volatile content lost after drying under specified conditions.
- Moisture content tests using thermogravimetric analysis or Karl Fischer titration.
This document outlines various physical evaluation tests performed on crude drugs, including moisture content, optical rotation, refractive index, melting point, viscosity, solubility, ash values, extractive values, and volatile oil content. These tests are used to standardize crude drugs and determine their composition and purity. Key tests mentioned include determining moisture content by heating to a constant weight, measuring viscosity and refractive index, identifying melting point ranges, assessing solubility in various solvents, calculating ash, water-soluble extract, and alcohol-soluble extract values, and quantifying volatile oil content. The results of these tests provide information about crude drug identity and quality.
Pharmaceutical Quality Management of Dexamethasone tablets BP
Dexamethasone tablets USP
DEXAMETHSONE OPTHALMIC SUSPENSION BP
DEXAMETHSONE OPTHALMIC SUSPENSION USP
Dexamethasone is a synthetic (man-made) corticosteroid.
Corticosteroids are naturally-occurring chemicals produced by the adrenal glands located above the kidneys.
Vitamins A and E are fat-soluble vitamins that play important roles in vision, antioxidant activity, and other metabolic functions. Vitamin A is found in foods like carrots, green vegetables and fruits, and helps with night vision. Vitamin E sources include nuts, seeds, and vegetable oils, and it acts as an antioxidant to repair tissues. Both vitamins can be quantified using chromatographic methods by measuring absorption peaks - vitamin A is measured using UV spectrophotometry while vitamin E uses gas chromatography to separate and measure peaks from standards.
This document summarizes a study on solvent deasphalting (SDA) of various vacuum residues from an Iranian crude oil using a bench-scale unit. The key findings are:
1) SDA with pentane or butane solvents significantly reduced metals, sulfur, and carbon content in the deasphalted oils (DAOs) produced, with butane giving greater reductions.
2) Higher molecular weight solvents and lower feed boiling points increased DAO yields, though yields leveled off for feeds over 500°C. Higher temperatures decreased yields.
3) DAO quality, as indicated by lower contaminant levels, improved with higher temperatures and lower feed boiling points. SDA is effective for upgrading vacuum
Purpose: Quantitative analysis of steroidal saponin „Diosgenin‟ from methanol extract of Moringa oleifera Lam (Drumstick) by HPTLC technique.
Approach: The approach of the study was to find out the presence of Diosgenin from Moringa and then its quantity.
Method: HPTLC analysis was performed with methonolic extract of seeds. Standard Diosgenin curve was used to detect the availability of the steroidal saponin Diosgenin.
Results: 20 μL of sample was applied which showed 159.4084 ng of Diosgenin. About 0.797 % w/v of Diosgenin was estimated form seeds of Moringa in methonolic extract. It was compared with the standard Diosgenin curve.
Conclusions: Moringa oleifera Lam seeds are the source of steroidal saponin- Diosgenin which can be used as female contraceptive to control human population.
Preparation and Properties of Oxidized Starch with High degree of OxidationIqbal Prawira
Corn starch had the highest degree of oxidation of 45% compared to pea and sweet potato starch. Oxidation of starch using 0.02% CuSO4 as a catalyst at 55°C for 60 minutes resulted in a degree of oxidation of 53.8%. Infrared spectroscopy showed that hydroxyl groups were successfully oxidized to carbonyl and carboxyl groups. The intrinsic viscosity and thermal stability of oxidized starch decreased with increasing degree of oxidation.
This document discusses various physical parameters and methods used to evaluate crude drugs, including ash values, swelling factor, extractive values, and bioassay. It describes determining total ash value, acid insoluble ash value, sulphated ash value, and water soluble ash value. Methods are provided for measuring swelling factor and water soluble, alcohol soluble, and ether soluble extractive values. Finally, it outlines using bioassay to evaluate drug activity through tests on living organisms.
Phytochemical Investigation of Caralluma lasiantha: Isolation of Stigmasterol...Ratnakaram Venkata Nadh
This document summarizes the isolation and identification of stigmasterol from Caralluma lasiantha. Stigmasterol was isolated using a sequence of steps including saponification, fractional crystallization, and column chromatography. Structural identification was confirmed through spectral data including IR, 1H NMR, 13C NMR, and mass spectrometry, as well as by comparing data to literature values. Stigmasterol is a phytosterol that was isolated for the first time from this plant species.
The document describes the Folch method for extracting lipids. It involves homogenizing tissue in a 2:1 chloroform/methanol mixture. The homogenate is then filtered or centrifuged to separate the liquid phase. This phase is washed with water or saline solution and centrifuged to separate the mixture into upper and lower phases. The upper methanol phase is removed by siphoning and contains polar molecules. The lower chloroform phase contains lipids and is evaporated, leaving only lipids.
Determination of pesticides residue in grains,fruits, vegetables,milk and mil...ShameerAbid
This document discusses the determination of pesticide residues in commodities. It covers the classification of different types of pesticides, factors that affect compatibility of samples for analysis, extraction methods, cleanup techniques, and general guidelines for preparing different types of samples for extraction and analysis. The key points are:
- Pesticides are classified into organochlorines, organophosphates, carbamates, pyrethroids, neonicotinoids, and miscellaneous pesticides.
- Sample preparation depends on characteristics like moisture content, with methods for high moisture, dry, and whole egg samples.
- Extraction separates pesticide residues from the matrix using solvents like acetonitrile or hexane.
Standardization of herbal drugs involves physical, chemical, biological, and toxicological methods. Physical methods include determining viscosity, melting point, solubility, moisture content, and ash values. Chemical methods involve detecting compounds like alkaloids, carbohydrates, and oils. Biological assays test for effects on microbes, tissues, or animals. Toxicological analysis checks for pesticide, heavy metal, and radioactive contamination as well as aflatoxins. Together, these techniques provide a standardized profile for identifying herbal drugs and ensuring their quality and purity.
Ijpar 14 618 ashaSynthesis and screening of new 2-(2-oxoindoline-3-ylidene)-n...pharmaindexing
This document describes the synthesis and characterization of new 2-(2-oxoindoline-3-ylidene)-N-phenyl hydrazine carbothioamide derivatives and evaluation of their antimicrobial activity. It involves a three step synthesis of the derivatives from aryl amines, including purification and characterization of intermediates and final compounds. The compounds were characterized using physical methods like melting point and spectroscopy. The compounds were evaluated for antibacterial activity against four bacteria and antifungal activity against two fungi using disk diffusion assays. Some of the compounds showed good antimicrobial activity.
Standardization of herbal drugs involves using morphological, microscopic, physical, chemical, and biological methods to determine identity, quality, purity and detect adulterants. Macroscopic and microscopic analysis examines physical characteristics. Microscopic methods include determining stomatal number, palisade ratio, and vein-islet number. Physical methods involve measuring properties like viscosity, melting point, solubility, moisture content, optical rotation, and refractive index. Chemical analysis comprises determining extractive values, ash values, bitterness, and hemolytic activity. Together, these techniques allow for confirmation of herbal drug identity and quality.
This document discusses the thermal and rheological properties of Povidone (PVP) and Copovidone polymers for use in hot melt extrusion. It finds that all PVP polymers show some degradation above 180°C, so that temperature is recommended as the upper limit for melt extrusion. PVP K-12 and S-630 are found to have ideal rheological properties for melt extrusion, with melt viscosities between 700-100,000 Pa.s. The other grades may require plasticization to be successfully melt extruded below 180°C.
This document presents information on analyzing organophosphorus and organochlorine pesticides. It describes the effects of pests and insects on various foods, the history of pesticide use in agriculture, and provides details on multi-residue methods for determining these pesticides. The methods involve extracting samples using solvents like acetone and dichloromethane, clean up using chromatography columns, and analyzing extracts using gas chromatography with detectors like FPD or ECD. Calibration is done against standard solutions to quantify residues in samples.
This document describes experiments to extract and analyze lipids from serum. In the first part, lipids were extracted from serum using chloroform-methanol and separated via centrifugation. The organic phase containing lipids was evaporated, redissolved in chloroform, and observed as a yellow liquid, indicating the presence of lipids. In the second part, thin layer chromatography was used to separate lipids in the extract on silica plates developed in two solvent systems, revealing at least two lipid components with different polarities. The experiments demonstrated techniques for lipid extraction and separation.
Development and Validation of Stability Indicating Assay Method of Montelukas...ijtsrd
Background A simple, precise cost effective stability indicating assay method of Montelukast by RP HPLC. Material Chromatographic separation was achieved on a Meteoric core C18 column 100mm x 4.6 mm, 2.7µm using a mobile phase 2 ml Trifluroacetic acid mixture of acetonitrile 250ml and methanol 400ml 350 650 at a flow rate of 1.5ml per minute. Wavelength was detection at 255nm. The retention time of Montelukast was 4 minutes. Results The method was found linear concentration the range of 120.39 802.57µg ml, tablet analysis of RSD 0.403, accuracy range 30 , 50 , 100 , and 200 , Precision RSD 0.3. The proposed method was validated as per the ICH guidelines. Conclusion The HPLC method was validated and demonstrated good linearity, precision, accuracy, specificity, robustness and stability indicating. The development HPLC method can be utilized for routine analysis stability studies for Montelukast. Miss. Harshada Ravindra Patil | Mr. Pavan Nathu Patil "Development and Validation of Stability Indicating Assay Method of Montelukast Tablet by RP-HPLC" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-1 , December 2019, URL: https://www.ijtsrd.com/papers/ijtsrd29809.pdf Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/29809/development-and-validation-of-stability-indicating-assay-method-of-montelukast-tablet-by-rp-hplc/miss-harshada-ravindra-patil
The document discusses the use of accelerated stability studies conducted at higher temperatures than intended storage conditions to quickly identify degradation processes in drug formulations. It defends this approach by stating that using elevated temperatures increases degradation rates, allowing stable formulations to be developed more quickly through identifying conditions and excipients that slow degradation over long periods at lower temperatures. While this approach does not guarantee detecting all events, it has generally proven reliable.
identification and quantitative determination of additives in pharmaceutical ...Sharath Hns
This document discusses the identification and quantification of various additives that are commonly found in pharmaceutical formulations and cosmetics. It provides an overview of different classes of additives such as preservatives, colors, antioxidants, emulsifiers, stabilizers, thickeners and flavors. It then describes various analytical techniques like titrimetric methods, spectrophotometry, HPLC and chromatography that can be used to separate, identify and determine the concentration of specific additives like benzoic acid, synthetic colors, antioxidants and emulsifiers.
This document describes methods for analyzing fermentation products such as wine, spirits, and beer. It discusses determining various analytes including tannins, extracts, sulphur dioxide, ethyl alcohol content, total acidity, and methyl alcohol. Spectrophotometric and gas chromatography methods are provided for measuring methyl alcohol. The document also outlines procedures for common assays such as using a spectrophotometer to generate a standard curve for tannin quantification and titrating samples with sodium hydroxide to determine total acidity.
Mucilage of basil seed can be employed as a potential ingredient in suspensions, emulsions, gels and tablets especially as viscosity enhancing agents, thickening agent, emulsifier or gelling agent and release retardant because of its good hydrophilic nature, physical stability, barrier properties, efficient control of release profile, extrudability and good spreadability.
Extensive characterisation of natural polymer in dosage form development for subsequent commercialisation has given rise to a new term “Naturapolyceutics”.
The document discusses preformulation, which involves determining the physicochemical properties of a new drug substance to aid in developing a stable dosage form. Key goals are to formulate a safe, effective dosage form with good bioavailability. The document outlines areas studied in preformulation including solubility, polymorphism, hygroscopicity, and particle characterization. Understanding these properties helps ensure the drug will perform as intended.
Pharmaceutical Quality Management of Dexamethasone tablets BP
Dexamethasone tablets USP
DEXAMETHSONE OPTHALMIC SUSPENSION BP
DEXAMETHSONE OPTHALMIC SUSPENSION USP
Dexamethasone is a synthetic (man-made) corticosteroid.
Corticosteroids are naturally-occurring chemicals produced by the adrenal glands located above the kidneys.
Vitamins A and E are fat-soluble vitamins that play important roles in vision, antioxidant activity, and other metabolic functions. Vitamin A is found in foods like carrots, green vegetables and fruits, and helps with night vision. Vitamin E sources include nuts, seeds, and vegetable oils, and it acts as an antioxidant to repair tissues. Both vitamins can be quantified using chromatographic methods by measuring absorption peaks - vitamin A is measured using UV spectrophotometry while vitamin E uses gas chromatography to separate and measure peaks from standards.
This document summarizes a study on solvent deasphalting (SDA) of various vacuum residues from an Iranian crude oil using a bench-scale unit. The key findings are:
1) SDA with pentane or butane solvents significantly reduced metals, sulfur, and carbon content in the deasphalted oils (DAOs) produced, with butane giving greater reductions.
2) Higher molecular weight solvents and lower feed boiling points increased DAO yields, though yields leveled off for feeds over 500°C. Higher temperatures decreased yields.
3) DAO quality, as indicated by lower contaminant levels, improved with higher temperatures and lower feed boiling points. SDA is effective for upgrading vacuum
Purpose: Quantitative analysis of steroidal saponin „Diosgenin‟ from methanol extract of Moringa oleifera Lam (Drumstick) by HPTLC technique.
Approach: The approach of the study was to find out the presence of Diosgenin from Moringa and then its quantity.
Method: HPTLC analysis was performed with methonolic extract of seeds. Standard Diosgenin curve was used to detect the availability of the steroidal saponin Diosgenin.
Results: 20 μL of sample was applied which showed 159.4084 ng of Diosgenin. About 0.797 % w/v of Diosgenin was estimated form seeds of Moringa in methonolic extract. It was compared with the standard Diosgenin curve.
Conclusions: Moringa oleifera Lam seeds are the source of steroidal saponin- Diosgenin which can be used as female contraceptive to control human population.
Preparation and Properties of Oxidized Starch with High degree of OxidationIqbal Prawira
Corn starch had the highest degree of oxidation of 45% compared to pea and sweet potato starch. Oxidation of starch using 0.02% CuSO4 as a catalyst at 55°C for 60 minutes resulted in a degree of oxidation of 53.8%. Infrared spectroscopy showed that hydroxyl groups were successfully oxidized to carbonyl and carboxyl groups. The intrinsic viscosity and thermal stability of oxidized starch decreased with increasing degree of oxidation.
This document discusses various physical parameters and methods used to evaluate crude drugs, including ash values, swelling factor, extractive values, and bioassay. It describes determining total ash value, acid insoluble ash value, sulphated ash value, and water soluble ash value. Methods are provided for measuring swelling factor and water soluble, alcohol soluble, and ether soluble extractive values. Finally, it outlines using bioassay to evaluate drug activity through tests on living organisms.
Phytochemical Investigation of Caralluma lasiantha: Isolation of Stigmasterol...Ratnakaram Venkata Nadh
This document summarizes the isolation and identification of stigmasterol from Caralluma lasiantha. Stigmasterol was isolated using a sequence of steps including saponification, fractional crystallization, and column chromatography. Structural identification was confirmed through spectral data including IR, 1H NMR, 13C NMR, and mass spectrometry, as well as by comparing data to literature values. Stigmasterol is a phytosterol that was isolated for the first time from this plant species.
The document describes the Folch method for extracting lipids. It involves homogenizing tissue in a 2:1 chloroform/methanol mixture. The homogenate is then filtered or centrifuged to separate the liquid phase. This phase is washed with water or saline solution and centrifuged to separate the mixture into upper and lower phases. The upper methanol phase is removed by siphoning and contains polar molecules. The lower chloroform phase contains lipids and is evaporated, leaving only lipids.
Determination of pesticides residue in grains,fruits, vegetables,milk and mil...ShameerAbid
This document discusses the determination of pesticide residues in commodities. It covers the classification of different types of pesticides, factors that affect compatibility of samples for analysis, extraction methods, cleanup techniques, and general guidelines for preparing different types of samples for extraction and analysis. The key points are:
- Pesticides are classified into organochlorines, organophosphates, carbamates, pyrethroids, neonicotinoids, and miscellaneous pesticides.
- Sample preparation depends on characteristics like moisture content, with methods for high moisture, dry, and whole egg samples.
- Extraction separates pesticide residues from the matrix using solvents like acetonitrile or hexane.
Standardization of herbal drugs involves physical, chemical, biological, and toxicological methods. Physical methods include determining viscosity, melting point, solubility, moisture content, and ash values. Chemical methods involve detecting compounds like alkaloids, carbohydrates, and oils. Biological assays test for effects on microbes, tissues, or animals. Toxicological analysis checks for pesticide, heavy metal, and radioactive contamination as well as aflatoxins. Together, these techniques provide a standardized profile for identifying herbal drugs and ensuring their quality and purity.
Ijpar 14 618 ashaSynthesis and screening of new 2-(2-oxoindoline-3-ylidene)-n...pharmaindexing
This document describes the synthesis and characterization of new 2-(2-oxoindoline-3-ylidene)-N-phenyl hydrazine carbothioamide derivatives and evaluation of their antimicrobial activity. It involves a three step synthesis of the derivatives from aryl amines, including purification and characterization of intermediates and final compounds. The compounds were characterized using physical methods like melting point and spectroscopy. The compounds were evaluated for antibacterial activity against four bacteria and antifungal activity against two fungi using disk diffusion assays. Some of the compounds showed good antimicrobial activity.
Standardization of herbal drugs involves using morphological, microscopic, physical, chemical, and biological methods to determine identity, quality, purity and detect adulterants. Macroscopic and microscopic analysis examines physical characteristics. Microscopic methods include determining stomatal number, palisade ratio, and vein-islet number. Physical methods involve measuring properties like viscosity, melting point, solubility, moisture content, optical rotation, and refractive index. Chemical analysis comprises determining extractive values, ash values, bitterness, and hemolytic activity. Together, these techniques allow for confirmation of herbal drug identity and quality.
This document discusses the thermal and rheological properties of Povidone (PVP) and Copovidone polymers for use in hot melt extrusion. It finds that all PVP polymers show some degradation above 180°C, so that temperature is recommended as the upper limit for melt extrusion. PVP K-12 and S-630 are found to have ideal rheological properties for melt extrusion, with melt viscosities between 700-100,000 Pa.s. The other grades may require plasticization to be successfully melt extruded below 180°C.
This document presents information on analyzing organophosphorus and organochlorine pesticides. It describes the effects of pests and insects on various foods, the history of pesticide use in agriculture, and provides details on multi-residue methods for determining these pesticides. The methods involve extracting samples using solvents like acetone and dichloromethane, clean up using chromatography columns, and analyzing extracts using gas chromatography with detectors like FPD or ECD. Calibration is done against standard solutions to quantify residues in samples.
This document describes experiments to extract and analyze lipids from serum. In the first part, lipids were extracted from serum using chloroform-methanol and separated via centrifugation. The organic phase containing lipids was evaporated, redissolved in chloroform, and observed as a yellow liquid, indicating the presence of lipids. In the second part, thin layer chromatography was used to separate lipids in the extract on silica plates developed in two solvent systems, revealing at least two lipid components with different polarities. The experiments demonstrated techniques for lipid extraction and separation.
Development and Validation of Stability Indicating Assay Method of Montelukas...ijtsrd
Background A simple, precise cost effective stability indicating assay method of Montelukast by RP HPLC. Material Chromatographic separation was achieved on a Meteoric core C18 column 100mm x 4.6 mm, 2.7µm using a mobile phase 2 ml Trifluroacetic acid mixture of acetonitrile 250ml and methanol 400ml 350 650 at a flow rate of 1.5ml per minute. Wavelength was detection at 255nm. The retention time of Montelukast was 4 minutes. Results The method was found linear concentration the range of 120.39 802.57µg ml, tablet analysis of RSD 0.403, accuracy range 30 , 50 , 100 , and 200 , Precision RSD 0.3. The proposed method was validated as per the ICH guidelines. Conclusion The HPLC method was validated and demonstrated good linearity, precision, accuracy, specificity, robustness and stability indicating. The development HPLC method can be utilized for routine analysis stability studies for Montelukast. Miss. Harshada Ravindra Patil | Mr. Pavan Nathu Patil "Development and Validation of Stability Indicating Assay Method of Montelukast Tablet by RP-HPLC" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-4 | Issue-1 , December 2019, URL: https://www.ijtsrd.com/papers/ijtsrd29809.pdf Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/29809/development-and-validation-of-stability-indicating-assay-method-of-montelukast-tablet-by-rp-hplc/miss-harshada-ravindra-patil
The document discusses the use of accelerated stability studies conducted at higher temperatures than intended storage conditions to quickly identify degradation processes in drug formulations. It defends this approach by stating that using elevated temperatures increases degradation rates, allowing stable formulations to be developed more quickly through identifying conditions and excipients that slow degradation over long periods at lower temperatures. While this approach does not guarantee detecting all events, it has generally proven reliable.
identification and quantitative determination of additives in pharmaceutical ...Sharath Hns
This document discusses the identification and quantification of various additives that are commonly found in pharmaceutical formulations and cosmetics. It provides an overview of different classes of additives such as preservatives, colors, antioxidants, emulsifiers, stabilizers, thickeners and flavors. It then describes various analytical techniques like titrimetric methods, spectrophotometry, HPLC and chromatography that can be used to separate, identify and determine the concentration of specific additives like benzoic acid, synthetic colors, antioxidants and emulsifiers.
This document describes methods for analyzing fermentation products such as wine, spirits, and beer. It discusses determining various analytes including tannins, extracts, sulphur dioxide, ethyl alcohol content, total acidity, and methyl alcohol. Spectrophotometric and gas chromatography methods are provided for measuring methyl alcohol. The document also outlines procedures for common assays such as using a spectrophotometer to generate a standard curve for tannin quantification and titrating samples with sodium hydroxide to determine total acidity.
Mucilage of basil seed can be employed as a potential ingredient in suspensions, emulsions, gels and tablets especially as viscosity enhancing agents, thickening agent, emulsifier or gelling agent and release retardant because of its good hydrophilic nature, physical stability, barrier properties, efficient control of release profile, extrudability and good spreadability.
Extensive characterisation of natural polymer in dosage form development for subsequent commercialisation has given rise to a new term “Naturapolyceutics”.
The document discusses preformulation, which involves determining the physicochemical properties of a new drug substance to aid in developing a stable dosage form. Key goals are to formulate a safe, effective dosage form with good bioavailability. The document outlines areas studied in preformulation including solubility, polymorphism, hygroscopicity, and particle characterization. Understanding these properties helps ensure the drug will perform as intended.
Seminar on solid state stability and shelf life by ranjeet singhRanjeet Singh
This seminar discusses the stability of solid drug substances and techniques for determining shelf life. Stability is defined as a drug substance remaining within specified limits of identity, strength, quality and purity during storage and use. Solid drugs can undergo physical transformations like polymorphic transitions, formation of hydrates or amorphous forms. Analytical techniques are used to identify these changes. Shelf life studies involve real time testing at recommended storage conditions or accelerated testing at elevated temperatures to estimate shelf life under normal conditions. Factors like temperature, moisture, pH and light exposure can influence drug degradation and must be considered.
The document discusses the formulation and characterization of cubosomes for controlled drug delivery. Cubosomes are nanostructured liquid crystalline particles that can encapsulate drugs. The study formulated cubosomes using lipids and block copolymers to encapsulate dextromethorphan for controlled release. Various formulations were tested in vitro and using cryo-TEM. The results showed that cubosomes can provide controlled release of drugs and balance structure, charge and viscosity is important to achieve this.
This document outlines preformulation studies conducted on the drug metronidazole, including characterization of its physical properties, solubility, stability, and compatibility with excipients. Key aspects that were evaluated include particle size, bulk density, angle of repose, pH, partition coefficient, stability under various conditions like temperature, humidity and light. Drug-excipient compatibility was also studied by storing mixtures at elevated temperature and observing for physical or chemical changes. The goal of these studies is to understand the drug's characteristics and behavior to aid in rational formulation design and selection of appropriate excipients and storage conditions.
In this slide, you will learn about what is polymorphism, types, and properties of polymorphism, the application of polymorphism in pharmaceutical industries, polymorphism of several drugs. Hope you will like it.
This document discusses drug stability and stabilization techniques. It defines drug stability and outlines the various types of instability drugs may experience, including physical, chemical, and microbial changes. It also discusses techniques for assessing stability through studies of solid state stability, compatibility with excipients, and solution phase stability. Specific degradation pathways like hydrolysis, oxidation, and photolysis are examined. Methods for establishing shelf life through accelerated stability testing and the Arrhenius equation are also covered. The document emphasizes the importance of stability studies in ensuring drug quality throughout storage and use.
Dissolution enhancement of glimepiride by solid dispersion technique.Santosh Adhikari
Dissolution Enhancement of Glimepiride by Solid Dispersion Technique.
Priyanka Shrestha1*, Shiva Kumar Bhandari1, SM Ashraful Islam1, and Santosh Adhikari2.
1Department of Pharmacy, University of Asia Pacific, Dhanmondi, Dhaka-1209, Bangladesh.
2Department of Pharmacy, Rajiv Gandhi University of Health Science, Banglore-560 041.
Colloidal particles ranging in size between 10 & 1000 nm are known as nanoparticles.
SLNs are new generation of submicron sized lipid emulsion where the liquid lipid(oil) has been substituted by a solid lipid.
Example: Capture - Dior
Preformulation studies characterize the physical and chemical properties of new drug molecules to aid in developing safe, effective, and stable dosage forms. The objectives are to establish physico-chemical parameters, determine kinetics and stability, and establish compatibility with excipients. Major areas of investigation include organoleptic properties, bulk characterization like crystallinity and polymorphism, solubility analysis including pH effects, and stability analysis of solutions and solids. Understanding these properties provides insights for processing and storage to ensure drug quality.
Stability_Considerations_In_Formulation_Development.pptRavi Kumar G
The document discusses the importance of stability considerations in pharmaceutical development. It states that stability is a key attribute and integral part of drug and dosage form development. The aim of pharmaceutical development is to design stable products and control factors preventing quality and stability issues. Stability evaluations start early in drug development and cover various stages. The physical state of drugs can influence stability, dissolution, and bioavailability. Factors like polymorphism, hydration, and processing need to be controlled. Excipient selection and manufacturing processes also impact stability and should be considered during formulation development.
This document provides an overview of preformulation studies for a new drug. It discusses characterizing the physical and chemical properties of the drug molecule to develop a safe, effective, and stable dosage form. Key aspects of preformulation studies that are described include salt formation, prodrug design, polymorphism, crystallinity, hygroscopicity, particle characterization, bulk density, powder flow properties, solubility analysis, stability analysis, and drug-excipient compatibility testing. The goal of preformulation is to obtain essential information to guide formulation development and design robust evaluation of the new drug candidate.
FORMULATION AND EVALUATION OF GLIBENCLAMIDE MICROSPHERE DRUG DELIVERY SYSTEMArindam Chakraborty
The document discusses the formulation and evaluation of glibenclamide microsphere drug delivery system. The objective was to increase the drug's self-life by developing a microsphere delivery system. Two batches of glibenclamide microspheres were prepared using different polymers and manufacturing methods. Batch 2, prepared via spray congealing with agar polymer, showed more sustained release over 12 hours compared to Batch 1 and was considered the optimized formulation. In vitro drug release studies found Batch 2 followed zero-order kinetics. The microspheres were characterized and evaluated for properties like particle size, drug entrapment efficiency, and in vitro drug release kinetics. The study achieved sustained drug release to improve bioavailability and patient compliance.
Shraddha roll no- 7 -m. pharm final presentation ---rbvrr college of pharmacysaathiyaa
The document describes the development and validation of an analytical method for ziprasidone using reverse phase high performance liquid chromatography. The method utilizes a Sunsil C18 column with a mobile phase of water and methanol (55:45) at a flow rate of 1 mL/min. Ziprasidone was detected at 261 nm with a retention time of 3.082 minutes. The method was validated for specificity, precision, linearity, accuracy, limit of detection, limit of quantification and robustness as per ICH guidelines. The developed and validated method can be used for the analysis of ziprasidone in bulk and pharmaceutical formulations.
The document discusses ICH stability testing guidelines for drug substances and products, outlining the types of studies required including long term, intermediate, and accelerated studies under various storage conditions. Key aspects that are evaluated include physical, chemical, and microbial changes that may occur over time and factors that influence stability such as temperature, humidity, and light exposure. The purpose of stability testing is to establish a product's shelf life and ensure it remains safe and effective when stored as recommended.
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EFFECT OF VARIOUS FREEZE DRYING
PARAMETERS ON THE STABILITY OF DRUG-X
R. Deepak Chandra
M.Pharm (Pharm Analysis)+MBA
Roll no:15
Under the Guidance of
Dr. Dipti Gatne
Professor & HOD of Pharm Analysis
SPP SPTM
NMIMS University
Under the Guidance of
Dr. Subash gore
General Manager, R&D Formulations
Dr. Ajeet K singh
Sr. Manager, R&D Formulations
Mylan laboratories limited, Hyderabad
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Background
Drug-X has the stable forms among its polymorphs, it available in the form of
lyophilized injection, stable form-Monohydrate & unstable form- Anhydrous
form.
During the process of lyophilization it converts monohydrate form of Drug-X to
anhydrous form where complete water is removed there by, monohydrate form of
Drug-X to anhydrous which is unstable not suitable for the formulation.
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Aim & Objective of the Work
To differentiate stable and unstable forms of Drug-X .
To characterize solid state of monohydrate form of Drug-X in freeze drying
formulation.
Determine the effects of various relative humidity conditions on Drug-X & ideal
storage conditions for stable Drug-X monohydrate form i.e. Temperature and
humidity conditions.
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S. no Materials Category, mechanism of action & use
1 Drug-X (API) Alkylating agent; Nitrogen Mustards, synthetic antineoplastic drug. Very
Narrow Therapeutic Index.
Prodrug; Activation requires cytochrome P450 enzyme.
Reactive carbonium ion intermediates transfer alkyl groups by forming
covalent bonds results in cross linking/ abnormal base pairing/ scission of
DNA strand.
Current Therapies:
1. Regulatory T-cell modulation
2. Treatment of Multiple Sclerosis.
3. Choice for acute & chronic leukaemias, myeloid leukaemia, Breast
Cancer
2 Mannitol
(Excipient)
In lyophilized preparations-Mannitol as a carrier to produce a stiff,
homogeneous cake that improves the appearance of the lyophilized cake
Improved dissolution rates; Improved thermal stability
Bulking agent
Materials
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S. No Equipment Purpose of Use
1. Differential Scanning Calorimeter
Determine the freeze drying parameters, and
characterization of API and Excipient.
2. Thermo Gravimetric Analysis To determine the weight loss in API.
3. X-Ray Diffraction D-8 Advance
Characterization of API & Mannitol, solid state
characterization of API, Lyophilized cakes, polymorphs of
API
4.
Gravimetric sorption Analyzer
(Intelligent gravimetric analysis)
Study the humidity effect on API
(Sorption-Desorption studies)
5. Karl Fisher Titration Determine the water content
6. Lyophilizer Perform the process of lyophilization/freeze drying.
Methods
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The project was planned as follows-
Characterization of Drug-X :
Determination of Melting point by Differential scanning calorimeter.
Determination of Powder Characteristics by Powder X-ray diffraction.
Determination of Water content by Thermogravimetric analyzer.
Characterization of Mannitol:
Determination of Melting point by Differential scanning calorimeter.
Determination of Powder Characteristics by Powder x-ray diffraction.
Lyophilization of Drug-X Formulation:
Drug-X for Injection, USP.
Optimization of lyophilization conditions in stable lyophilized Drug-X formulation by Differential Scanning
Calorimetry.
Lyophilization process
Characterization of Freeze Dried Formulations:
Determination of Water content by Karl fischer Titration
Characterization of Freeze Dried Formulations by Powder X-ray Diffraction
Effect of Relative humidity on Drug-X:
Effect of Relative humidity on Drug-X by Gravimetric sorption analyzer
Effect of Relative humidity on Drug-X by Powder x-ray diffraction.
Research Envisaged &Plan of Work
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Melting point at 49.3°C.
characteristic for monohydrate form of Drug-X
wrt the reference in the USP monograph
specifications. (49°C-52°C)
Peaks for at 6.973°, 14.755° and 17.785,
which are the characteristic for Drug-X.
Characterization of Drug-X - DSC, XRD & TGA
DSC Thermogram of Drug-X Diffractogram of Drug-X
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Loss of weight as 6.15% which is characteristic for Drug-X
TGA Thermogram of Drug-X
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Melting point at 170.9°C which is
characteristic wrt the reference in the USP
monograph (165°C-170°C)
Observed peaks for at, 9.402°, 13.659°,
and 17.263° which are characteristic
Mannitol
Characterization of Mannitol - DSC & XRD
DSC Thermogram of Mannitol Diffractogram of Mannitol
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Dissolving
Drug and
excipients in
a suitable
solvent,
generally
WFI.
Sterilizing
bulk solution
by passing it
0.22 micron
bacteria-
retentive
filter.
Filling into
individual
sterile
containers
and partially
stoppering
the containers
under aseptic
conditions.
Transporting
containers to
lyophilizer
and loading
into the
chamber
Freezing the
solution by
placing in
shelves in a
freeze-drying
chamber or
pre-freezing
in another
chamber.
Applying
vacuum to
chamber ,
heating
shelves to
evaporate the
water from
the frozen
state.
Stoppering of
the vials
installed in
lyophilizers.
Lyophilization generally includes the following steps:
Drug-X is available as parenteral dosage formulations consisting of
sterile packaged dry powder blend admixtures of the Monohydrate from
of Drug-X, sodium chloride and mannitol.
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Exotherm which represents crystallization temperature at -20°C and e
Endotherm which represents at ice melting at -1.60°C and melting at 4.37°C.
Optimization of freeze drying parameters –
Differential Scanning Calorimeter
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The freeze drying parameters are optimized by using DSC
Freezing temperature = -20°C-25°C
Primary drying = 1-5°C
Secondary drying = 20°C-25°C.
The freezing can be set to more than -25°C ; as lyophilizer runs for long time and also
to avoid any fluctuations.
Different lyophilization batches are operated varying in vacuum, freezing time,
primary drying time, secondary drying time. all the batches yields cakes with good
appearance and greater stability.
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Batch Thermal Treatment Primary Drying Secondary Drying
Batch-1 Freezing to -40°C 150 min High vacuum
(500 m Torr)
1330 min High vacuum
(500 m Torr)
100 min
Batch-2 Freezing to -40°C 240 min Moderate
vacuum
(380 m Torr)
1180 min High vacuum
(500 m Torr)
120 min
Batch-3 Freezing to -40°C 360 min Less vacuum
(200 m Torr)
1100 min Less vacuum
(200 m Torr)
1200 min
Batch-4 Freezing to -40°C 1270 min Less vacuum
(200 m Torr)
2810 min High vacuum
(500 m Torr)
500 min
Batch-5 Freezing to -40°C 260 min Less vacuum
(200 m Torr)
2540 min High vacuum
(500 m Torr)
240 min
Batch-6 Freezing to -
40°C
360 min Less vacuum
(200 m Torr)
1100 min High vacuum
(500 m Torr)
40 min
Freeze dried formulations are analyzed by using XRD & KF
Freeze Drying cycle- Lyophilizer
Freeze dried formulation of 6 different Batches
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Water content - Karl Fisher Titration
Water content of Freeze dried formulations
S.NO Sample/Batch Percentage of Water Content
1 Drug-X (API) 6.18%
2 Batch-1 0.002%
3 Batch-2 0.002%
4 Batch-3 0.004%
5 Batch-4 0.004%
6 Batch-5 0.002%
7 Batch-6 4.35%
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5 Batches - overlayed and compared with monohydrate form of Drug-X and mannitol
peaks, Batch-3 shows significant decrease in intensities .
Solid pattern studies-XRD
Diffractogram of Freeze dried formulations
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S. No RELATIVE HUMIDITY (%)
RANGE
TIME INFERENCE
1 Zero % (Desorption) 16 hrs Physical form of drug changes to powder to sticky liquid.
2 Zero % (Desorption) 4 hrs 7.1% weight loss
Sticky, semisolid form
3 0-90% 20 hrs
4.5 % weight gain
Sticky, semisolid form
1.2 % loss at 40-50% RH
4
0-20%
Zero % (Desorption) for an hr
20 % for 2 hrs
3 hrs 4.28% weight loss
Sticky, semisolid form
5 5% RH 15 hrs 5.2% weight loss
Sticky, semisolid form
6 20-30% RH 10 hrs 0.8 % weight loss
Powder form
7 80 % RH 6 hrs 0.5% weight gain
Powder form
Effect of Relative humidity- Gravimetric Sorption Analyzer
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Continued…
Monohydrate from of Drug-X is subjected 0% RH to 90% RH with changes in time
intervals
At lower RH: loss in weight ; anhydrous form ; physical nature : semisolid and sticky in
nature; unstable
Back to room RH: weight gain ; physical nature remains same.
At higher RH: weight gain; monohydrate nature; physical nature remains same;
crystalline powder form; stable.
Back to room RH: Weight loss; physical nature remains same.
Therefore optimum RH conditions for the Monohydrate from of Drug-X to be stored are
20-30% RH, where negligible weight loss is seen that withstands monohydrate nature.
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Drug-X is subjected to various relative humidity conditions -reduced in intensities
Variations in relative humidity conditions
Diffractogram of Drug-X at various RH
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Drug-X is subjected to higher relative humidity conditions where crystalline form
is unchanged. It means monohydrate form of Drug-X is stable in its crystal form at
higher relative humidities.
Higher Relative Humidity
Diffractogram of Drug-X at higher RH
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Non-ambient PXRD Study
Diffractogram of Drug-X using Non-ambient PXRD study
Monohydrate form of Drug-X is subjected to Non-ambient powder x-ray
diffraction study and diffractograms are observed at different intervals of time,
characteristic peaks for monohydrate form slowly disappearing after 2 hrs.
Gradually the monohydrate form converted in to anhydrous after 14 hrs under zero
percent relative humidity.
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Summary
Characterization of Drug and excipient are done by DSC, XRD which helps to
determine the nature of drug and excipient
Monohydrate from of Drug-X is thermally and hydrolytically susceptible and
exhibit poor stability in aqueous solution hence the technique lyophilization is
employed.
Presence of water content in the Drug-X formulation after lyophilization process is
an characteristic feature, as the stable form of Drug-X is monohydrate, therefore
determination of water content by Karl fisher
Studied the changes in the solid state patterns of freeze dried lyophilized cakes and
determines the changes in the nature of solid state patterns with variations in the
freeze drying parameters.
Drug-X is sensitive to humidity variations therefore the solid state characterization
of Monohydrate from of Drug-X by XRD at various humidity conditions and effect
of various relative humidity conditions are done in order to determine the
temperature and relative humidity conditions.
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Conclusion
Powder X-ray diffraction studies able to identify between
monohydrate and anhydrous forms of Drug-X.
By varying the secondary drying conditions in the lyophilizer
an optimum of 4% moisture is achieved in the vial.
Relative humidity effects studies on Monohydrate from of
Drug-X reveals that optimum storage conditions.
Temperature = less than 25°C.
Relative Humidity = 25%-30%.