This document describes a single RP-HPLC method for the quantification of aceclofenac, paracetamol, and chlorozoxazone in formulations. The method utilizes an Inertsil ODS 3V column with a mobile phase of phosphate buffer and acetonitrile in a 67:33 ratio at a flow rate of 1.0 mL/min and detection at 275 nm. The method was validated for specificity, linearity, accuracy, precision, and ruggedness. High resolution was achieved with retention times of 2.1 minutes for paracetamol, 8.8 minutes for chlorozoxazone, and 20.7 minutes for aceclofenac. The method provides a simple, validated approach
in process quality control test for ophthalmic and parenterals Henisha Patel
This document provides information on in-process quality control (IPQC) tests for ophthalmic and parenteral dosage forms. It defines ophthalmic and parenteral preparations and lists their common types. For ophthalmics, tests include sterility, uniformity of volume, particulate matter, particle size, and uniformity of weight. For parenterals, tests check content, pH, clarity, environmental controls and sterility. The document outlines procedures for sterility testing using direct transfer and membrane filtration methods and the rabbit pyrogen test.
ISO series, guide of pharmaceutical manufacturing facilities, productivity b...Kailash Vilegave
The document summarizes key aspects of ISO standards for quality management systems, including ISO 9000 and ISO 14000. It discusses the history and development of ISO standards, an overview of the ISO 9000 series, and highlights of the ISO 9000:2000 standard. The presentation focuses on process-based quality management and continual improvement as core principles of the ISO standards.
Reference standards in Pharmaceutical Industriesbhavanavedantam
This presentation is brief introduction about reference standards that are using in pharmaceutical industries for calibration of different instruments, methods and pharmaceutical chemicals...
This document summarizes formulations for various cosmetic preparations including lipsticks, shampoos, cold cream, vanishing cream, toothpastes, hair dyes, and sunscreens. It provides information on the definition, key ingredients, preparation methods, and evaluation of these products. The main formulations covered are lipsticks, shampoos, cold cream, and toothpastes. It also briefly discusses packaging materials science and factors that influence the choice of packaging for pharmaceutical products.
Premises - Part of Good Manufacturing PracticesTeny Thomas
This document discusses good manufacturing practices for pharmaceutical premises. It covers factors to consider for location, design, construction, sanitation, maintenance, utilities, and environmental control of premises to prevent contamination. The premises must have defined areas for receiving, sampling, storage, production, packaging, and quality control. Cleaning procedures and environmental monitoring programs are important to control contamination. Grade A or B areas for sterile products require additional controls like air quality standards and maintenance of sterile conditions.
The document discusses preformulation and summarizes some of its key aspects. Preformulation involves determining the physicochemical properties of new drug substances to aid in developing effective dosage forms. It covers topics like organoleptic properties, purity, particle size and shape, solubilization using surfactants, and the effect of temperature, pH and co-solvents on solubility. It also mentions the importance of preformulation stability studies and considering drug characteristics for different dosage forms. The goals of preformulation are establishing parameters, kinetic profiles, physical characteristics and compatibility with excipients.
Principle and Applications Of MBTH, NQS, FC and BM ReagentsLakshmi Kalyani
This document discusses MBTH, FC, and BM reagents which are used for qualitative and quantitative analysis of pharmaceuticals. It provides background on each reagent, including their chemical structure and properties. The principles and mechanisms of how each reagent reacts with different functional groups like phenols, amines, and aldehydes are described. Examples of using each reagent to estimate drugs are provided, such as using MBTH to analyze acyclovir and FC to determine protein concentration. The document concludes that these reagents can successfully quantify and qualify drugs in formulations when used at optimized concentrations.
in process quality control test for ophthalmic and parenterals Henisha Patel
This document provides information on in-process quality control (IPQC) tests for ophthalmic and parenteral dosage forms. It defines ophthalmic and parenteral preparations and lists their common types. For ophthalmics, tests include sterility, uniformity of volume, particulate matter, particle size, and uniformity of weight. For parenterals, tests check content, pH, clarity, environmental controls and sterility. The document outlines procedures for sterility testing using direct transfer and membrane filtration methods and the rabbit pyrogen test.
ISO series, guide of pharmaceutical manufacturing facilities, productivity b...Kailash Vilegave
The document summarizes key aspects of ISO standards for quality management systems, including ISO 9000 and ISO 14000. It discusses the history and development of ISO standards, an overview of the ISO 9000 series, and highlights of the ISO 9000:2000 standard. The presentation focuses on process-based quality management and continual improvement as core principles of the ISO standards.
Reference standards in Pharmaceutical Industriesbhavanavedantam
This presentation is brief introduction about reference standards that are using in pharmaceutical industries for calibration of different instruments, methods and pharmaceutical chemicals...
This document summarizes formulations for various cosmetic preparations including lipsticks, shampoos, cold cream, vanishing cream, toothpastes, hair dyes, and sunscreens. It provides information on the definition, key ingredients, preparation methods, and evaluation of these products. The main formulations covered are lipsticks, shampoos, cold cream, and toothpastes. It also briefly discusses packaging materials science and factors that influence the choice of packaging for pharmaceutical products.
Premises - Part of Good Manufacturing PracticesTeny Thomas
This document discusses good manufacturing practices for pharmaceutical premises. It covers factors to consider for location, design, construction, sanitation, maintenance, utilities, and environmental control of premises to prevent contamination. The premises must have defined areas for receiving, sampling, storage, production, packaging, and quality control. Cleaning procedures and environmental monitoring programs are important to control contamination. Grade A or B areas for sterile products require additional controls like air quality standards and maintenance of sterile conditions.
The document discusses preformulation and summarizes some of its key aspects. Preformulation involves determining the physicochemical properties of new drug substances to aid in developing effective dosage forms. It covers topics like organoleptic properties, purity, particle size and shape, solubilization using surfactants, and the effect of temperature, pH and co-solvents on solubility. It also mentions the importance of preformulation stability studies and considering drug characteristics for different dosage forms. The goals of preformulation are establishing parameters, kinetic profiles, physical characteristics and compatibility with excipients.
Principle and Applications Of MBTH, NQS, FC and BM ReagentsLakshmi Kalyani
This document discusses MBTH, FC, and BM reagents which are used for qualitative and quantitative analysis of pharmaceuticals. It provides background on each reagent, including their chemical structure and properties. The principles and mechanisms of how each reagent reacts with different functional groups like phenols, amines, and aldehydes are described. Examples of using each reagent to estimate drugs are provided, such as using MBTH to analyze acyclovir and FC to determine protein concentration. The document concludes that these reagents can successfully quantify and qualify drugs in formulations when used at optimized concentrations.
Quality control for rubber closures & secondary materialkavita bahmani
This document outlines various tests that are conducted on rubber closures and secondary packaging materials like paper and board. It describes the preparation of a solution for rubber closures and then lists different tests like sterility testing, fragmentation testing, self-seal ability, pH testing, light absorption testing, and residue on evaporation. It also provides an overview of 20 different tests that are performed on secondary packaging materials to analyze properties like moisture content, density, tensile strength, tear strength, puncture resistance, stiffness, water absorbency, rub resistance, pH, roughness, brightness, wet burst strength, and more.
This document discusses quality control tests for suppositories. It describes the different types of suppositories and various tests conducted during quality control, including visual examination, uniformity of weight and texture, melting point determination, breaking strength, dissolution testing, content uniformity, and disintegration testing. The goals of these tests are to ensure suppositories meet specifications for attributes like appearance, consistency, and ability to dissolve or disintegrate properly when administered.
This document provides instructions for synthesizing sulphanilamide from acetanilide in 3 steps:
1. Acetanilide is treated with chlorosulphonic acid to form the intermediate p-acetamidobenzenesulphonyl chloride.
2. p-acetamidobenzenesulphonyl chloride is reacted with ammonia to form p-acetamidobenzenesulphonamide.
3. p-acetamidobenzenesulphonamide undergoes acid hydrolysis with hydrochloric acid to remove the acetamide group and yield the final product sulphanilamide hydrochloride.
The percentage yield of sulphan
The document provides instructions for 12 experiments involving the synthesis and analysis of various pharmaceutical compounds. The experiments cover topics such as synthesizing sulphanilamide, 7-hydroxy-4-methyl coumarin, chlorbutanol, tolbutamide, hexamine, and assaying drugs like isonicotinic acid hydrazide and metronidazole. For each experiment, the document provides the aim, principle, required chemicals, procedure, and a report section to record theoretical yield, practical yield, and percentage yield. The document serves as a practical manual for 6th semester B.Pharm students, outlining key medicinal chemistry experiments.
Pharmaceutical aerosols can be filled using either a cold-fill or pressure-fill process depending on the nature of the product concentrate and propellant. The cold-fill process involves cooling the concentrate and propellant below their boiling points to liquefy them before filling the chilled container. The pressure-fill process places the concentrate in the container before forcing the hydrocarbon propellant in under pressure. Both processes involve sealing the valve and checking for leaks by heating the filled container in a water bath.
Oxytocin is a hormone produced in the hypothalamus that stimulates contractions of the uterus during childbirth and the mammary glands to produce milk during breastfeeding. It plays an important role in bonding between mothers and their children. There are four main methods used to test the potency of oxytocin in biological assays: by measuring its ability to decrease blood pressure in chickens, induce contractions in isolated rat uteri, increase milk ejection pressure in lactating rats, and elevate blood pressure through vasopressor activity in rats. Each method involves carefully preparing test animals, administering doses of both a standard and test oxytocin preparation, and recording and statistically analyzing the biological responses.
This document discusses various reagents used in pharmaceutical analysis including PDAB, Folin Ciocalteau, and MBTH reagents. It provides details on the principles, mechanisms, procedures, examples, and applications of each reagent. PDAB is used to detect primary amine groups via a colorimetric reaction. Folin Ciocalteau is used to detect phenols and reduces tungstate-molybdate to form a blue complex. MBTH forms colored complexes with aldehydes, phenols, and amines through oxidative coupling and can be used to analyze samples containing these functional groups. The document concludes that optimizing reagent volume and concentration allows these reagents to be successfully used to quantify drugs in pharmaceutical formulations.
Pharmaceutical aerosols are therapeutic active ingredients packaged in a pressurized system. They have advantages like direct delivery to affected areas without contamination. Aerosols consist of a propellant, container, valve, and product concentrate. Common propellants include hydrocarbons and gases. Containers must withstand high pressure and are often metal or glass. Valves meter doses and come in types like spray or foam. Formulations contain an active ingredient and propellant to achieve desired properties. Quality is ensured through testing of components, dosage, leakage and other parameters.
Degradation and Degradant CharacterizationGagan Deep
This document discusses degradation, degradants, and degradant characterization. It defines degradation as changes in a substance's properties due to environmental factors or formulation interactions. Degradants are products formed from degradation that can reduce potency or induce toxicity. Degradant characterization involves profiling degradants using analytical techniques like LC-MS, GC-MS, and LC-NMR to separate and identify degradants. Factors like temperature, moisture, light exposure, pH changes, and microbes can induce degradation.
Eye, ear and nasal drops are sterile aqueous or oily solutions meant for instillation into respective areas. Eye drops contain drugs that are antiseptic, anesthetic, anti-inflammatory or cause pupil dilation/constriction. Ear drops and nasal drops contain medications to relieve conditions like congestion. All three include active ingredients, vehicles, preservatives and adjuvants in suitable containers. They must be free of particles, sterile, have proper pH, tonicity, viscosity, surface activity and not cause irritation. Thickening agents, isotonic solutions, and surfactants are added to meet these requirements.
Inprocess as per usp ip bp liquid dosage formsDeepak Jain
This document discusses liquid dosage forms. It defines various types of liquid dosage forms including solutions, suspensions, emulsions, and colloids. It describes advantages like ease of swallowing and more rapid drug absorption. It also discusses problems like bulkiness, stability issues, and accurate dosing. It provides definitions and examples of different oral liquid formulations like elixirs, mixtures, and syrups. Finally, it outlines some common tests for oral liquids including uniformity of content and microbial quality.
This document discusses quality control tests for pharmaceutical containers, including glass and plastic containers. It provides details on various tests conducted for glass containers, such as hydrolytic resistance testing via surface testing, powdered glass testing, and etched surface testing. It also describes tests for arsenic levels, light transmission of colored glass, and tests for containers holding blood and blood components. For plastic containers, it outlines tests for leakage, collapsibility, clarity of aqueous extract, and non-volatile residue for non-injectable preparations. For injectable preparations, it lists tests conducted on both the containers and container materials.
This document discusses various dissolution apparatus used to test the dissolution of pharmaceutical dosage forms. It describes the 7 main types of apparatus specified in pharmacopeias like USP including basket, paddle, flow-through cell and reciprocating cylinder apparatuses. Each type of apparatus has a specific design and is used to test different dosage forms like tablets, capsules, transdermal patches based on simulating their dissolution environment in the body. Dissolution testing provides critical information for quality control and drug development.
Non chromatographic separation_techniques_ppt-convertedPoonamtaru
Fractional distillation and sublimation are two non-chromatographic separation techniques. Fractional distillation uses a fractional column to separate liquids with similar boiling points, such as ethanol and water. Sublimation transitions substances directly from solid to gas without an intermediate liquid phase, as seen with dry ice. Derivatization is a chemical reaction that converts polar functional groups to nonpolar groups to make molecules volatile for analysis by gas chromatography. Froth flotation selectively separates hydrophobic and hydrophilic materials using bubbles to carry hydrophobic particles to the surface in a stable froth.
This document discusses guidelines from the International Council for Harmonisation (ICH) for stability testing of drug substances and products. It provides guidance on topics such as the need for harmonized stability testing, types of stability testing, selection of batches and storage conditions for testing, and evaluation of stability data. The guidelines aim to establish a systematic approach to stability testing to ensure quality, safety and efficacy over a product's shelf life and recommend conditions for testing drug substances intended for various storage conditions.
This document discusses excipients, which are inactive substances formulated alongside active pharmaceutical ingredients in medications. Excipients help ensure efficacious drug products by affecting properties like drug release consistency, stability, and ease of administration. They are classified into categories like binders, disintegrants, fillers, and lubricants. The document focuses on disintegrants, which help tablets break down in the gastrointestinal tract, and describes common types like starches and their derivatives, clays, and cross-linked polymers. It also discusses binders, emulsifiers, viscosity modifiers, and other excipient types and their ideal properties and functions in drug formulations.
plastic and glass containers and its evaluation test, drug plastic considera...SUJIT DAS
This document discusses quality control tests that must be conducted on plastic containers used for pharmaceutical products. It outlines specific tests for non-parenteral and parenteral preparations, including leakage tests, clarity of extracts, and limits for substances like barium, heavy metals, and tin. It also discusses considerations for using plastic versus glass containers, noting potential issues like permeation of gases/liquids, leaching of substances from the plastic, and chemical reactions between drugs and container materials.
Opthalmics Preparation and its Evaluation parametersKavya S
This document summarizes the packaging and evaluation of ophthalmic products. It discusses various containers like plastics and glass used for ophthalmic packaging. It also describes different types of ophthalmic products like eye drops, ointments, lotions and inserts. Key evaluation parameters discussed include sterility testing, clarity testing, leakage testing and testing for metal particles. Assay, pH, viscosity testing are also summarized as important evaluation methods. The document concludes with a brief overview of the definition, ideal properties and formulation of different ophthalmic preparations.
Photo catalytic degradation of m dinitrobenzene using semiconductor zn o and ...ijsidonlineinfo
The document summarizes a study on the photocatalytic degradation of m-dinitrobenzene using zinc oxide (ZnO) and hydrogen peroxide (H2O2). Various parameters that affect the degradation rate were investigated, including pH, irradiation time, light intensity, substrate concentration, catalyst concentration, and H2O2 concentration. The maximum degradation rate occurred at pH 8.5, with 0.14 grams of ZnO catalyst and 0.30 mL/h of H2O2. The degradation rate increased with light intensity, substrate concentration (up to an optimum level), catalyst amount (up to a saturation point), and H2O2 concentration (until it became excessive). The mechanism of
Quality control for rubber closures & secondary materialkavita bahmani
This document outlines various tests that are conducted on rubber closures and secondary packaging materials like paper and board. It describes the preparation of a solution for rubber closures and then lists different tests like sterility testing, fragmentation testing, self-seal ability, pH testing, light absorption testing, and residue on evaporation. It also provides an overview of 20 different tests that are performed on secondary packaging materials to analyze properties like moisture content, density, tensile strength, tear strength, puncture resistance, stiffness, water absorbency, rub resistance, pH, roughness, brightness, wet burst strength, and more.
This document discusses quality control tests for suppositories. It describes the different types of suppositories and various tests conducted during quality control, including visual examination, uniformity of weight and texture, melting point determination, breaking strength, dissolution testing, content uniformity, and disintegration testing. The goals of these tests are to ensure suppositories meet specifications for attributes like appearance, consistency, and ability to dissolve or disintegrate properly when administered.
This document provides instructions for synthesizing sulphanilamide from acetanilide in 3 steps:
1. Acetanilide is treated with chlorosulphonic acid to form the intermediate p-acetamidobenzenesulphonyl chloride.
2. p-acetamidobenzenesulphonyl chloride is reacted with ammonia to form p-acetamidobenzenesulphonamide.
3. p-acetamidobenzenesulphonamide undergoes acid hydrolysis with hydrochloric acid to remove the acetamide group and yield the final product sulphanilamide hydrochloride.
The percentage yield of sulphan
The document provides instructions for 12 experiments involving the synthesis and analysis of various pharmaceutical compounds. The experiments cover topics such as synthesizing sulphanilamide, 7-hydroxy-4-methyl coumarin, chlorbutanol, tolbutamide, hexamine, and assaying drugs like isonicotinic acid hydrazide and metronidazole. For each experiment, the document provides the aim, principle, required chemicals, procedure, and a report section to record theoretical yield, practical yield, and percentage yield. The document serves as a practical manual for 6th semester B.Pharm students, outlining key medicinal chemistry experiments.
Pharmaceutical aerosols can be filled using either a cold-fill or pressure-fill process depending on the nature of the product concentrate and propellant. The cold-fill process involves cooling the concentrate and propellant below their boiling points to liquefy them before filling the chilled container. The pressure-fill process places the concentrate in the container before forcing the hydrocarbon propellant in under pressure. Both processes involve sealing the valve and checking for leaks by heating the filled container in a water bath.
Oxytocin is a hormone produced in the hypothalamus that stimulates contractions of the uterus during childbirth and the mammary glands to produce milk during breastfeeding. It plays an important role in bonding between mothers and their children. There are four main methods used to test the potency of oxytocin in biological assays: by measuring its ability to decrease blood pressure in chickens, induce contractions in isolated rat uteri, increase milk ejection pressure in lactating rats, and elevate blood pressure through vasopressor activity in rats. Each method involves carefully preparing test animals, administering doses of both a standard and test oxytocin preparation, and recording and statistically analyzing the biological responses.
This document discusses various reagents used in pharmaceutical analysis including PDAB, Folin Ciocalteau, and MBTH reagents. It provides details on the principles, mechanisms, procedures, examples, and applications of each reagent. PDAB is used to detect primary amine groups via a colorimetric reaction. Folin Ciocalteau is used to detect phenols and reduces tungstate-molybdate to form a blue complex. MBTH forms colored complexes with aldehydes, phenols, and amines through oxidative coupling and can be used to analyze samples containing these functional groups. The document concludes that optimizing reagent volume and concentration allows these reagents to be successfully used to quantify drugs in pharmaceutical formulations.
Pharmaceutical aerosols are therapeutic active ingredients packaged in a pressurized system. They have advantages like direct delivery to affected areas without contamination. Aerosols consist of a propellant, container, valve, and product concentrate. Common propellants include hydrocarbons and gases. Containers must withstand high pressure and are often metal or glass. Valves meter doses and come in types like spray or foam. Formulations contain an active ingredient and propellant to achieve desired properties. Quality is ensured through testing of components, dosage, leakage and other parameters.
Degradation and Degradant CharacterizationGagan Deep
This document discusses degradation, degradants, and degradant characterization. It defines degradation as changes in a substance's properties due to environmental factors or formulation interactions. Degradants are products formed from degradation that can reduce potency or induce toxicity. Degradant characterization involves profiling degradants using analytical techniques like LC-MS, GC-MS, and LC-NMR to separate and identify degradants. Factors like temperature, moisture, light exposure, pH changes, and microbes can induce degradation.
Eye, ear and nasal drops are sterile aqueous or oily solutions meant for instillation into respective areas. Eye drops contain drugs that are antiseptic, anesthetic, anti-inflammatory or cause pupil dilation/constriction. Ear drops and nasal drops contain medications to relieve conditions like congestion. All three include active ingredients, vehicles, preservatives and adjuvants in suitable containers. They must be free of particles, sterile, have proper pH, tonicity, viscosity, surface activity and not cause irritation. Thickening agents, isotonic solutions, and surfactants are added to meet these requirements.
Inprocess as per usp ip bp liquid dosage formsDeepak Jain
This document discusses liquid dosage forms. It defines various types of liquid dosage forms including solutions, suspensions, emulsions, and colloids. It describes advantages like ease of swallowing and more rapid drug absorption. It also discusses problems like bulkiness, stability issues, and accurate dosing. It provides definitions and examples of different oral liquid formulations like elixirs, mixtures, and syrups. Finally, it outlines some common tests for oral liquids including uniformity of content and microbial quality.
This document discusses quality control tests for pharmaceutical containers, including glass and plastic containers. It provides details on various tests conducted for glass containers, such as hydrolytic resistance testing via surface testing, powdered glass testing, and etched surface testing. It also describes tests for arsenic levels, light transmission of colored glass, and tests for containers holding blood and blood components. For plastic containers, it outlines tests for leakage, collapsibility, clarity of aqueous extract, and non-volatile residue for non-injectable preparations. For injectable preparations, it lists tests conducted on both the containers and container materials.
This document discusses various dissolution apparatus used to test the dissolution of pharmaceutical dosage forms. It describes the 7 main types of apparatus specified in pharmacopeias like USP including basket, paddle, flow-through cell and reciprocating cylinder apparatuses. Each type of apparatus has a specific design and is used to test different dosage forms like tablets, capsules, transdermal patches based on simulating their dissolution environment in the body. Dissolution testing provides critical information for quality control and drug development.
Non chromatographic separation_techniques_ppt-convertedPoonamtaru
Fractional distillation and sublimation are two non-chromatographic separation techniques. Fractional distillation uses a fractional column to separate liquids with similar boiling points, such as ethanol and water. Sublimation transitions substances directly from solid to gas without an intermediate liquid phase, as seen with dry ice. Derivatization is a chemical reaction that converts polar functional groups to nonpolar groups to make molecules volatile for analysis by gas chromatography. Froth flotation selectively separates hydrophobic and hydrophilic materials using bubbles to carry hydrophobic particles to the surface in a stable froth.
This document discusses guidelines from the International Council for Harmonisation (ICH) for stability testing of drug substances and products. It provides guidance on topics such as the need for harmonized stability testing, types of stability testing, selection of batches and storage conditions for testing, and evaluation of stability data. The guidelines aim to establish a systematic approach to stability testing to ensure quality, safety and efficacy over a product's shelf life and recommend conditions for testing drug substances intended for various storage conditions.
This document discusses excipients, which are inactive substances formulated alongside active pharmaceutical ingredients in medications. Excipients help ensure efficacious drug products by affecting properties like drug release consistency, stability, and ease of administration. They are classified into categories like binders, disintegrants, fillers, and lubricants. The document focuses on disintegrants, which help tablets break down in the gastrointestinal tract, and describes common types like starches and their derivatives, clays, and cross-linked polymers. It also discusses binders, emulsifiers, viscosity modifiers, and other excipient types and their ideal properties and functions in drug formulations.
plastic and glass containers and its evaluation test, drug plastic considera...SUJIT DAS
This document discusses quality control tests that must be conducted on plastic containers used for pharmaceutical products. It outlines specific tests for non-parenteral and parenteral preparations, including leakage tests, clarity of extracts, and limits for substances like barium, heavy metals, and tin. It also discusses considerations for using plastic versus glass containers, noting potential issues like permeation of gases/liquids, leaching of substances from the plastic, and chemical reactions between drugs and container materials.
Opthalmics Preparation and its Evaluation parametersKavya S
This document summarizes the packaging and evaluation of ophthalmic products. It discusses various containers like plastics and glass used for ophthalmic packaging. It also describes different types of ophthalmic products like eye drops, ointments, lotions and inserts. Key evaluation parameters discussed include sterility testing, clarity testing, leakage testing and testing for metal particles. Assay, pH, viscosity testing are also summarized as important evaluation methods. The document concludes with a brief overview of the definition, ideal properties and formulation of different ophthalmic preparations.
Photo catalytic degradation of m dinitrobenzene using semiconductor zn o and ...ijsidonlineinfo
The document summarizes a study on the photocatalytic degradation of m-dinitrobenzene using zinc oxide (ZnO) and hydrogen peroxide (H2O2). Various parameters that affect the degradation rate were investigated, including pH, irradiation time, light intensity, substrate concentration, catalyst concentration, and H2O2 concentration. The maximum degradation rate occurred at pH 8.5, with 0.14 grams of ZnO catalyst and 0.30 mL/h of H2O2. The degradation rate increased with light intensity, substrate concentration (up to an optimum level), catalyst amount (up to a saturation point), and H2O2 concentration (until it became excessive). The mechanism of
Anthropometric, dietary intakes and exercise habits of niddm in guntur cityijsidonlineinfo
The study examined the dietary habits and exercise patterns of 50 type 2 diabetics in Guntur City, India. It found that over 50% of subjects were obese, with a BMI over 25. The typical meal pattern was 3 meals and 1 snack per day. Common foods restricted were those high in sugar and carbohydrates. However, over 70% included foods like millets, bitter gourd and green leafy vegetables. Nearly half the subjects used indigenous foods like fenugreek seeds to manage their diabetes. Walking was the main form of exercise.
Este documento analisa como a avaliação pode contribuir para a aprendizagem em softwares educativos de línguas estrangeiras. Ele discute diferentes concepções de avaliação e como elas estão presentes nos softwares, além de analisar funções da avaliação como diagnóstico e feedback. Também examina tipos de softwares e características relacionadas à organização dos conteúdos e interação.
Erro e fracasso_novo. lidia e ana liviaAndreza Lira
Este documento discute o erro e o fracasso no contexto da aprendizagem. Ele afirma que o erro não é necessariamente indício de fracasso, mas parte integrante do processo de aprendizagem. O documento também explora diferentes tipos de erros e suas possíveis interpretações, além de discutir que o fracasso escolar envolve múltiplas variáveis e não é apenas responsabilidade do aluno.
O documento discute as práticas avaliativas nas escolas brasileiras e propõe uma redefinição destas práticas. Atualmente, a avaliação se baseia quase que exclusivamente nos resultados de provas, que usam uma linguagem diferente do dia a dia da sala de aula. Além disso, a avaliação é usada para punir os alunos em vez de ser um processo formativo. O documento defende que a avaliação deve mudar para melhorar as relações e ações na escola.
Este documento discute a avaliação escolar e a democratização da educação no Brasil. A avaliação nas escolas geralmente se concentra em notas e julgamentos ao invés de diagnóstico e melhoria, e precisa mudar para apoiar todos os estudantes. Os professores devem envolver estudantes e pais no processo de avaliação para torná-la mais justa e útil para a aprendizagem.
O documento discute as causas do fracasso escolar, incluindo falta de pré-requisitos, rótulos negativos e problemas sociais. Anteriormente, culpava-se os alunos e suas famílias, mas hoje reconhece-se que fatores externos como a performance do professor também influenciam. Não devemos apontar culpados, mas sim buscar novas abordagens, como liderança, clima escolar positivo e capacitação docente.
The document is a report by Hamoud Al-Breiki on renewable and non-renewable energy. It defines energy and discusses various types of renewable energy like solar, hydropower and wind. It also discusses non-renewable energy sources like oil, gas and coal. The report covers advantages and disadvantages of both renewable and non-renewable energy. It concludes by mentioning Masdar company and providing references.
Usfda generic drug user fee act a complete reviewijsidonlineinfo
This document provides a review of the Generic Drug User Fee Act (GDUFA) implemented by the US Food and Drug Administration (USFDA). It discusses:
1) The increasing backlog of generic drug applications and inspections that GDUFA aims to address by providing additional funds to the USFDA.
2) The key goals of GDUFA are to ensure safety, efficacy, and access by prioritizing application review, increasing facility inspections, and expediting approval processes.
3) GDUFA fees are paid by generic drug manufacturers and facility owners and are split between application fees and facility fees, with the total revenue expected to be $299 million annually from 2013-
Avaliação da aprendizagem escolar: um ato amorosoAndreza Lira
O documento discute a avaliação da aprendizagem escolar como um ato amoroso, enfatizando que ela deve identificar os atos e situações dos alunos e acolhê-los, ao invés de excluí-los ou classificá-los. A avaliação deve fazer um diagnóstico e incluir o aluno no processo, ao contrário de testes que selecionam e julgam.
This document provides an overview of Tokyo, Japan including its geography and climate, culture, famous traditional foods, transportation options, and top tourist attractions. Tokyo has hot, humid summers and mild winters with an average annual temperature of 16°C. The culture has been influenced by Jomon, Chinese, Korean, Greek, Indian, European and American traditions. Popular tourist destinations include Mount Fuji, Tokyo DisneySea, and the electric district of Akihabara.
The document provides information about the upcoming Common Written Examination (CWE) to be conducted by the Institute of Banking Personnel Selection (IBPS) in September 2014 for recruitment of officers and office assistants in regional rural banks across India. It lists the 56 participating regional rural banks and their head office locations. The eligibility criteria include nationality, age, educational qualifications, physical disability definitions. Candidates qualifying the CWE will be considered for subsequent rounds of selection including interviews to be conducted by individual regional rural banks.
Alternate teaching learning methods a welcome idea among students!ijsidonlineinfo
1) The study compared the effectiveness of two teaching methods - a PowerPoint presentation versus a blackboard/chalk presentation aided by 3D models.
2) An assessment given after each session found no significant difference in student performance between the two methods. However, feedback indicated that students preferred the use of 3D models as it helped visualize concepts.
3) When the lesson was recapped using a combination of methods, 58% of students rated this approach best over using a single method alone. The study concluded that using multiple teaching methods can make lectures more interesting for students.
A simple rp hplc method for simultaneous analysis of pseudoephedrine, bambute...ijsidonlineinfo
This document describes the development and validation of a reverse phase HPLC method for the simultaneous analysis of Pseudoephedrine, Bambuterol, Levocetirizine, and Montelukast in pharmaceutical dosage forms. The method uses a C18 column with a gradient mobile phase of buffer and acetonitrile at a flow rate of 1 mL/min. The compounds were well separated with retention times between 4.1-21.1 minutes. The method was validated for linearity, precision, accuracy and robustness according to ICH guidelines and is suitable for quality control of these drugs in tablets and other dosage forms.
Histopathology of intestinal tissue of mastacembelus armatus parasitized by p...ijsidonlineinfo
This document summarizes a research article that studied the histopathological changes in the intestinal tissue of Mastacembelus armatus fish parasitized by the Ptychobothridae cestode parasite Senga Sp. The normal intestinal tissue structure is described. Sections of infected intestine tissue showed the parasite penetrating the mucosal layer and damaging the villi and epithelium. Higher magnifications showed the parasite crossing multiple intestinal layers and reaching near the serosa. The parasite was concluded to have a pathogenic effect and cause damage to the host intestinal tissue to obtain nutrients, making it an important consideration for aquaculture and fish disease management.
Choosingtherightpoliticalmodelforpakistan 130118125219-phpapp02Naqash Aman
Pakistan was created as an Islamic state through the sacrifices of millions who wanted to establish a nation governed by Islamic principles, with authority derived from Allah alone. A dialogue between Muhammad Ali Jinnah and Allama Shabbir Ahmad Usmani discussed that Pakistan's constitution and sovereignty would be limited to the principles prescribed by Islam. The objective of Pakistan's birth was to have a country where Islamic laws and values formed the basis of governance.
The document discusses the benefits of exercise for mental health. Regular physical activity can help reduce anxiety and depression and improve mood and cognitive function. Exercise causes chemical changes in the brain that may help protect against developing mental illness and improve symptoms for those who already suffer from conditions like anxiety and depression.
The document describes the development and validation of an HPLC method for the estimation of Irbesartan in pharmaceutical dosage forms. A simple reverse phase HPLC method was developed using an inertsil ODS C-18 column, methanol, acetonitrile and 2% OPA mobile phase. The method was validated for accuracy, precision, linearity and specificity. Limit of detection was 10 ng and recovery from tablet formulation was 100.61%, indicating the method is accurate for quantifying Irbesartan in tablets.
Simultaneous estimation of amitryptyline and chlordiazepoxide by RP-HPLC methodpharmaindexing
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of amitriptyline and chlordiazepoxide. The method utilizes a C18 column, mobile phase of phosphate buffer and acetonitrile (55:45), flow rate of 1 ml/min, and detection wavelength of 252 nm. Linearity was achieved between 25-150 μg/ml for amitriptyline and 10-60 μg/ml for chlordiazepoxide. The method was validated for accuracy, precision, specificity, linearity, robustness and sensitivity. The developed RP-HPLC method allows for the simultaneous quantitative analysis of amitriptyline
Simultaneous estimation of meclizine and nicotinic acid by using RP-HPLCpharmaindexing
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous estimation of Meclizine and Nicotinic acid. The method utilizes a mobile phase of acetonitrile and potassium dihydrogen phosphate buffer with a flow rate of 1.0 mL/min. The retention times were 3.01 minutes for Meclizine and 6.07 minutes for Nicotinic acid. The method was validated and found to be accurate, precise, specific, linear, robust, sensitive and able to quantify the drugs in tablet dosage forms without interference from other components.
Formulation and evaluation of microspheres with aceclofenacSagar Savale
Aceclofenac is an analgesic and anti-inflammatory drug that reduces fever, pain, and inflammation in rheumatoid
arthritis, osteoarthritis and ankylosing spondylitis. Aceclofenac has higher anti-inflammatory action than
conventional NSAIDs. Development of microspheres is a promising technology for controlled release and drug
targeting. Various types of microspheres such as bio-adhesive, magnetic, floating, radioactive and polymeric
microspheres are developed for various purposes. Microspheres occupied a central place in novel drug delivery, it
can targeted and localized drug delivery system. This Aceclofenac Microsphere is Prepared by using Spray drying
Technique in which release rate of drug is mainly depends on formulation composition (Eudragit RS 30 D and
Ethyl Cellulose (1:2 ratio)). Formulated microspheres were characterized for particle size, encapsulation efficiency
and In vitro studies. The optimum drug-to-polymer ratio and feed flow rate is responsible for higher percent yield,
smaller particle size and maximum encapsulation efficiency.
Analytical method development and validation for the estimation of aspirin an...SriramNagarajan19
A simple and selective LC method is described for the determination of Aspirin and Omeprazole in tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of 30 volumes of ammonium acetate buffer, 40 volumes of acetonitrile and 30 volumes of Methanol with detection of 233 nm. Linearity was observed in the range 18-42 µg/ml for Aspirin (r2 =0.983) and 6-14 µg /ml for Omeprazole (r2 =0.970) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
This document describes the development and validation of an RP-HPLC method for the simultaneous estimation of atenolol and amlodipine in tablet dosage forms. The method utilizes a C18 column with a mobile phase of triethylamine buffer, acetonitrile and methanol pumped isocratically at a flow rate of 1.0 mL/min. Atenolol and amlodipine were detected at 232.2 nm. The method was validated per ICH guidelines and showed good precision, accuracy, linearity, specificity and robustness, making it suitable for the simultaneous analysis of these drugs in pharmaceutical formulations.
IOSR Journal of Pharmacy and Biological Sciences(IOSR-JPBS) is a double blind peer reviewed International Journal that provides rapid publication (within a month) of articles in all areas of Pharmacy and Biological Science. The journal welcomes publications of high quality papers on theoretical developments and practical applications in Pharmacy and Biological Science. Original research papers, state-of-the-art reviews, and high quality technical notes are invited for publications.
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the simultaneous quantification of hydrochlorothiazide and eprosartan in bulk drug and pharmaceutical formulations. The method utilizes a C18 column with a mobile phase of 50mM KH2PO4 (pH 4.0) and acetonitrile in a 30:70 ratio at a flow rate of 1 mL/min. Hydrochlorothiazide and eprosartan were detected at 270nm and the method was linear over a range of 5-25 μg/mL and 8-40 μg/mL, respectively. The developed method was successfully applied for the analysis of a marketed tablet
UV spectrophotometric method development and validation for quantitative esti...Sagar Savale
UV Spectrophotometric Method Development and Validation for quantitative estimation of Ondansetron
Hydrochloride (HCL). U.V Spectrophotometric method have been widely employed in determination of
individual components in a mixture or fixed dose combination. Our aim is to develop spectroscopic method for
estimation of the Ondansetron HCL in ternary mixture by using U.V spectrophotometry. The method was
validated as per ICH guidelines. The recovery studies confirmed the accuracy and precision of the method. It was
successfully applied for the analysis of the drug in bulk and could be effectively used for the routine analysis.
Bioanalytical RP-HPLC Method Development and Validation for Estimation of Cur...Sagar Savale
The present study was aimed at developing a reversed phase high performance liquid chromatography (RPHPLC) method for determination of curcumin (CRM) in plasma and hydrochlorothiazide was used as an internal
standard. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.)
coupled with a guard column of silica, mobile phase was consisting of acetonitrile: water with 0.1% formic acid
(40:60 v/v). The flow rate was 0.3 ml/min and the drug was detected using PDA detector at the wavelength of 423
nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation
and flow rate, were optimised to provide high-resolution and reproducible peaks. The developed method was
validated in terms of linearity, recovery, precision, ruggedness, sensitivity (LOD and LOQ) and stability study
(short and long-term stabilities, Freeze/thaw stability and post-preparative).
New RP HPLC method for the simultaneous estimation of rosuvastatin and aspiri...SriramNagarajan19
A simple and selective LC method is described for the determination of Rosuvastatin and Aspirin tablet dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of A mixture of 60 volumes of 20mM Phosphate buffer pH 3.5: 20 volumes of Acetonitrile and 20 voulmes of Methanol. With detection of 232 nm. Linearity was observed in the range 12-28 µg /ml for Rosuvastatin (r2 =0.9977) and 90-210 µg /ml for Aspirin (r2 =0.9953) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing % RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
Method Development and Validation for Estimation of Oral Hypoglycaemic Drug D...ijtsrd
HPLC is a chromatographic technique employed in active compound chemistry and biochemistry to separate a mixture and substances with the goal of identifying, measuring, and purifying the different components of the mixture. Its a much better variety of column and traditional chromatography. The objective of the research work is to develop and validate a simple and accurate reverse phase chromatographic method to estimate amount of drug in dosage form. The developed method successfully can be applied to estimate the amount of Dapagliflozin in tablet dosage form. After oral administration of dapagliflozin, the maximum plasma concentration Concentration max under two hours. High performance liquid chromatographic system was alleviated according to the chromatographic settings. After attaining the steady base line, to verify the system suitability, a single 40 µg ml of standard solution proportional to 100 test concentration of dapagliflozin was injected into the HPLC system. The gradient mobile phase flow rate programming assisted in optimising the lengthy run duration and resolution of sample analysis, making the approach more cost effective and quick. Validation of the developed and optimized HPLC method was carried out according to ICH guidelines with respect to parameters such as linearity, specificity, precision and accuracy. Junaid Ahmed | Himanchal Sharma | Shiva Teotia "Method Development and Validation for Estimation of Oral Hypoglycaemic Drug Dapagliflozinina Tablet Dosage form by the Employment of Rp-HPLC" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-5 | Issue-6 , October 2021, URL: https://www.ijtsrd.com/papers/ijtsrd46395.pdf Paper URL : https://www.ijtsrd.com/pharmacy/analytical-chemistry/46395/method-development-and-validation-for-estimation-of-oral-hypoglycaemic-drug-dapagliflozinina-tablet-dosage-form-by-the-employment-of-rphplc/junaid-ahmed
This document describes the development and validation of a new reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of paracetamol in pharmaceutical dosage forms. Some key points:
- An isocratic RP-HPLC method was developed using a mobile phase of acetonitrile and potassium dihydrogen orthophosphate buffer at a ratio of 15:85, pH 2.5.
- The method was validated for parameters such as linearity, accuracy, precision, limit of detection, limit of quantification, and robustness as per ICH guidelines.
- The method showed good linearity in the range of 25-60 μg/ml with a correlation coefficient of 0.999
A new precise accurate and reliable validated method for the determination of Capecitabine was developed by using
reverse phase high performance liquid chromatography in pharmaceutical dosage forms. Spectrophotometer
determination was carried out at an absorption maximum of 240nm by using methanol. The linearity was over the
concentration range of 20-120 μg/ml with correlation coefficient 0.999. Chromatographic separation was carried
out by using a mobile phase of methanol: Acetonitrile: water (80:20:80 V/V) on Waters 2487 dual absorbance
column in an isocratic mode at a flow rate of 1.1 ml/min with UV detection at 240 nm. The developed methods were
found to be precise and accurate for the estimation of Capecitabine in pharmaceutical dosage forms and could be
used for routine analysis.
Keywords: Capecitabine, RP-HPLC, Spectrophotometry, Waters 2487 dual absorbance detector, Nova pack 300 ×
3.9mm 5μ as column, 240nm
Stabilized compositions of prasugre hydrochloride tabletsijsidonlineinfo
This document summarizes a research article that studied stabilized tablet compositions of prasugrel hydrochloride. Prasugrel is a thienopyridine derivative and ADP receptor antagonist used to reduce cardiovascular events in patients with acute coronary syndrome undergoing percutaneous coronary intervention. The researchers developed tablet formulations using Opadry AMB, a moisture barrier film coating, which showed better stability compared to normal hypromellose coatings. They used a dry direct compression method and evaluated compositions containing prasugrel hydrochloride, mannitol, crospovidone, hypromellose, and magnesium stearate coated with Opadry AMB or Opadry II. The Opadry AMB coated tablets provided
Green synthesis of gold nanoparticles using various extract of plants and spicesijsidonlineinfo
1. The document describes the green synthesis of gold nanoparticles using various plant and spice extracts, which reduce aqueous HAuCl4.3H2O to Au° and stabilize the nanoparticles.
2. Twenty-five plants and four spice extracts were used to synthesize gold nanoparticles, as confirmed by the color change from yellow to various colors and monitoring of surface plasmon resonance using UV-Vis spectroscopy.
3. The phytochemicals in the plant and spice extracts, such as polyphenols, terpenes, and carbohydrates, contain active groups that play an important role in reducing HAuCl4 to Au nanoparticles.
Barriers to internationalization–a study of the pharmacy sector in trinidad a...ijsidonlineinfo
This document summarizes a study that examined barriers to internationalization faced by retail pharmacies in Trinidad and Tobago. The study used surveys to measure pharmacies' willingness to internationalize and identify perceived barriers. Three hypotheses were tested: 1) access to finance is a major constraint, 2) strong international networks increase willingness, and 3) younger firms are more willing to internationalize. The results found support for the first two hypotheses but not the third - age was not a significant factor. The study provides insight into challenges small businesses in the pharmacy sector face when considering expanding internationally.
Sesame oil cake an inexpensive substrate for neutral protease production by p...ijsidonlineinfo
This document describes research on using sesame oil cake as a substrate for neutral protease production by Penicillium chrysogenum NCIM 737 under solid-state fermentation. Sesame oil cake supported the maximum protease production of the substrates tested. Process parameters like fermentation time, temperature, pH, inoculum age, and initial moisture content were optimized. Maximum protease activity of 172.5 U/gds was obtained at 7 days of fermentation, 25°C, pH 7, with a 7-day old culture at 45% initial moisture content. Supplementing the substrate with sucrose, peptone, and ammonium chloride further increased activity to 197.5 U/gds.
Evaluation of effects of botanical extracts against the pink mealy bug (macon...ijsidonlineinfo
The document evaluates the effects of botanical extracts on the activity of aminotransferases in silkworms fed mulberry leaves infested by the pink mealy bug. Specifically, it studied the impacts of spraying extracts from Azadirachta indica, Ocimum Sanctum, and parthenium hysterophorus on the protease and transaminase activity in silkworm tissues. The results showed that protease and ALAT activity gradually increased in silkworms fed the treated leaves, while AAT activity decreased from day 4 to day 6, though these changes were not statistically significant. The study suggests that foliar spraying of these plant extracts can control pink mealy bugs on mulberry leaves without negatively affecting
Effects of endosulfan and fenvalerate on pyruvate of the freshwater fish, lab...ijsidonlineinfo
The document reports on a study that examined the effects of the pesticides endosulfan and fenvalerate on pyruvate levels in the freshwater fish Labeo rohita. The fish were exposed to sublethal concentrations of the pesticides for 24 hours and 15 days. Pyruvate levels decreased in the brain, gill, kidney, liver, and muscle tissues of the fish after exposure. Fenvalerate exposure resulted in greater decreases in pyruvate levels than endosulfan exposure. The decreases in pyruvate suggest a shift towards anaerobic metabolism in the fish due to pesticide stress.
Voltametric determination of acephate pesticide by liquid state lipase enzyma...ijsidonlineinfo
This document summarizes a study that developed an electroanalytical method for determining the organophosphorus pesticide Acephate using liquid state lipase enzyme inhibition. The method is based on measuring the inhibition of lipase enzyme's ability to hydrolyze p-Nitro phenyl acetate to p-Nitro phenol, which is then detected by cyclic voltammetry. The study optimized various parameters such as enzyme concentration, substrate concentration, pH, incubation time and obtained a linear calibration for detecting Acephate concentrations between 100-900 μM. The detection limit was found to be 159.77 μM and the quantification limit was 532.57 μM for Acephate using this lipase enzyme inhibition method.
Study of cladocera species diversity with reference to chydoridae and bosma...ijsidonlineinfo
This document summarizes a study of Cladocera species diversity in the Nira left bank canal and Tarangawadi lake in India. 14 species across 2 families (Bosminidae and Chydoridae) were identified based on appendages like the labrum, antennules, dorsal, ventral, and post abdomen features. In the Bosminidae family, 2 species of Bosmina and Bosminopsis were found. The Chydoridae family contained 6 genera including the genus Alona which had 4 species identified by the presence of ocelli and varied post abdomen shapes.
Strategies for Effective Upskilling is a presentation by Chinwendu Peace in a Your Skill Boost Masterclass organisation by the Excellence Foundation for South Sudan on 08th and 09th June 2024 from 1 PM to 3 PM on each day.
LAND USE LAND COVER AND NDVI OF MIRZAPUR DISTRICT, UPRAHUL
This Dissertation explores the particular circumstances of Mirzapur, a region located in the
core of India. Mirzapur, with its varied terrains and abundant biodiversity, offers an optimal
environment for investigating the changes in vegetation cover dynamics. Our study utilizes
advanced technologies such as GIS (Geographic Information Systems) and Remote sensing to
analyze the transformations that have taken place over the course of a decade.
The complex relationship between human activities and the environment has been the focus
of extensive research and worry. As the global community grapples with swift urbanization,
population expansion, and economic progress, the effects on natural ecosystems are becoming
more evident. A crucial element of this impact is the alteration of vegetation cover, which plays a
significant role in maintaining the ecological equilibrium of our planet.Land serves as the foundation for all human activities and provides the necessary materials for
these activities. As the most crucial natural resource, its utilization by humans results in different
'Land uses,' which are determined by both human activities and the physical characteristics of the
land.
The utilization of land is impacted by human needs and environmental factors. In countries
like India, rapid population growth and the emphasis on extensive resource exploitation can lead
to significant land degradation, adversely affecting the region's land cover.
Therefore, human intervention has significantly influenced land use patterns over many
centuries, evolving its structure over time and space. In the present era, these changes have
accelerated due to factors such as agriculture and urbanization. Information regarding land use and
cover is essential for various planning and management tasks related to the Earth's surface,
providing crucial environmental data for scientific, resource management, policy purposes, and
diverse human activities.
Accurate understanding of land use and cover is imperative for the development planning
of any area. Consequently, a wide range of professionals, including earth system scientists, land
and water managers, and urban planners, are interested in obtaining data on land use and cover
changes, conversion trends, and other related patterns. The spatial dimensions of land use and
cover support policymakers and scientists in making well-informed decisions, as alterations in
these patterns indicate shifts in economic and social conditions. Monitoring such changes with the
help of Advanced technologies like Remote Sensing and Geographic Information Systems is
crucial for coordinated efforts across different administrative levels. Advanced technologies like
Remote Sensing and Geographic Information Systems
9
Changes in vegetation cover refer to variations in the distribution, composition, and overall
structure of plant communities across different temporal and spatial scales. These changes can
occur natural.
How to Build a Module in Odoo 17 Using the Scaffold MethodCeline George
Odoo provides an option for creating a module by using a single line command. By using this command the user can make a whole structure of a module. It is very easy for a beginner to make a module. There is no need to make each file manually. This slide will show how to create a module using the scaffold method.
বাংলাদেশের অর্থনৈতিক সমীক্ষা ২০২৪ [Bangladesh Economic Review 2024 Bangla.pdf] কম্পিউটার , ট্যাব ও স্মার্ট ফোন ভার্সন সহ সম্পূর্ণ বাংলা ই-বুক বা pdf বই " সুচিপত্র ...বুকমার্ক মেনু 🔖 ও হাইপার লিংক মেনু 📝👆 যুক্ত ..
আমাদের সবার জন্য খুব খুব গুরুত্বপূর্ণ একটি বই ..বিসিএস, ব্যাংক, ইউনিভার্সিটি ভর্তি ও যে কোন প্রতিযোগিতা মূলক পরীক্ষার জন্য এর খুব ইম্পরট্যান্ট একটি বিষয় ...তাছাড়া বাংলাদেশের সাম্প্রতিক যে কোন ডাটা বা তথ্য এই বইতে পাবেন ...
তাই একজন নাগরিক হিসাবে এই তথ্য গুলো আপনার জানা প্রয়োজন ...।
বিসিএস ও ব্যাংক এর লিখিত পরীক্ষা ...+এছাড়া মাধ্যমিক ও উচ্চমাধ্যমিকের স্টুডেন্টদের জন্য অনেক কাজে আসবে ...
How to Setup Warehouse & Location in Odoo 17 InventoryCeline George
In this slide, we'll explore how to set up warehouses and locations in Odoo 17 Inventory. This will help us manage our stock effectively, track inventory levels, and streamline warehouse operations.
it describes the bony anatomy including the femoral head , acetabulum, labrum . also discusses the capsule , ligaments . muscle that act on the hip joint and the range of motion are outlined. factors affecting hip joint stability and weight transmission through the joint are summarized.
Exploiting Artificial Intelligence for Empowering Researchers and Faculty, In...Dr. Vinod Kumar Kanvaria
Exploiting Artificial Intelligence for Empowering Researchers and Faculty,
International FDP on Fundamentals of Research in Social Sciences
at Integral University, Lucknow, 06.06.2024
By Dr. Vinod Kumar Kanvaria
A workshop hosted by the South African Journal of Science aimed at postgraduate students and early career researchers with little or no experience in writing and publishing journal articles.
How to Fix the Import Error in the Odoo 17Celine George
An import error occurs when a program fails to import a module or library, disrupting its execution. In languages like Python, this issue arises when the specified module cannot be found or accessed, hindering the program's functionality. Resolving import errors is crucial for maintaining smooth software operation and uninterrupted development processes.
RPMS TEMPLATE FOR SCHOOL YEAR 2023-2024 FOR TEACHER 1 TO TEACHER 3
Single rp hplc method for the quantification of aceclofenac, paracetamol and chlorozoxazone in formulations
1. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
ISSN:2249-5347
IJSID
International Journal of Science Innovations and Discoveries An International peer
Review Journal for Science
Research Article Available online through www.ijsidonline.info
SINGLE RP-HPLC METHOD FOR THE QUANTIFICATION OF ACECLOFENAC, PARACETAMOL AND
CHLOROZOXAZONE IN FORMULATIONS
1Dept. of Chemistry, Sri Krishnadevaraya University, Anantapur, AP, India; 2Department of Chemistry,
Hari kishan Reddy Ganthi1*, Hanimi Reddy Bapatu2, Maram Ravi Kumar3, Useni Reddy Mallu1,
JNT University, Kukatpally, Hyderabad, AP, India-500072.; 3 AR&D, Custom Pharmaceutical Services,
Dr. Reddy’s Laboratories Ltd, Bachupally, Hyd-72, India.
Received: 14-08-2012
Accepted: 17-10-2012 ABSTRACT
Objectives: To develop a single RP-HPLC method for determination of Aceclofenac,
Paracetamol and Chlorozoxazone contents in formulation.
*Corresponding Author
Methods: Chromatographic separation was achieved on Inertsil ODS 3V, 150 x4.6mm, 5µ
column. Mobile phase composed of phosphate b u f f e r of pH 6.0 and
a c e t o n i t r i l e i n t h e r a t i o n 6 7 : 3 3 v / v . 1.0ml per min flow rate and detection
was at 275 nm.
Results: High resolution was achieved with the simple mobile phase composition and
retention time of Paracetamol, Chlorozoxazone, and Aceclofenac are about 2.1min, 8.8min
and 20.7min, respectively. The area of all ingredient peaks were a linear function of
concentration in the range 150.4 to 752.3 ppm for Paracetamol, 120.2 to 761.4 ppm for
Chlorozoxazone and 29.9 to 159.9 ppm for Aceclofenac and the correlation co-efficient
Address:
value of all activeINTRODUCTION limit (0.999).
ingredients within the
Name:
Conclusion: Proposed HPLC method was validated with specificity, linearity, accuracy,
Hari Kishan Reddy Ganthi
Place:
reproducibility and ruggedness and it is applicable for regular analysis.
Sri Krishnadevaraya University
Keywords: Aceclofenac, Paracetamol, Chlorozoxazone and RP-HPLC method.
Anantapur, AP, India
E-mail:
kishangan05ster@gmail.com
INTRODUCTION
471
International Journal of Science Innovations and Discoveries, Volume 2, Issue 4, July-August 2012
2. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
Paracetamol (acetaminophen) is one of the most popular over-the-counter (OTC) analgesic and antipyretic drugs.
INTRODUCTION
Paracetamol (1-8) is available in different dosage forms: tablet, capsules, drops, elixirs, suspensions and suppositories.
Aceclofenac is a non-steroidal anti-inflammatory drug (NSAID). It is used for the relief of pain and inflammation in
rheumatoid arthritis, osteoarthritis and ankylosing spondylitis. The dose is 100 mg twice daily. It should not be given to
people with porphyria or breast-feeding mothers, and is not recommended for children.
Chlorzoxazone is used to relieve pain and stiffness caused by muscle strains and sprains. It is used in combination with
physical therapy, analgesics (such as aspirin or acetaminophen), and rest. The side effects are upset stomach, drowsiness,
dizziness, lightheadedness, weakness, skin rash or itching, yellowing of the skin or eyes and stomach pain.
Chemical structures of all ingredients were represented in figure-1.All three ingredients are available in liquid pharmaceutical
dosage forms.
Paracetamol Chlorozoxazone Aceclofenac
Figure-1: Chemical structure of all ingredients
All ingredients have reported methods for individual and other combination products, but the objective of the present
study is to develop a single RP-HPLC method for the estimation of Paracetamol, Aceclofenac and Chlorozoxazone in
formulations and the developed and validated method is simple, novel, rugged and linear.
MATERIALS AND METHODS
Various buffer salts, pH values were tried with different organic solvents (acetonitrile or methanol) for the optimization of
Selection of mobile phase:
mobile phase. Finally well shaped and high resolution was achieved with pH 6.0 phosphate buffer and acetonitrile at 67:33 v/v
ratio.
Ortho phosphoric acid, triethyl amine (AR Grade) was procured from S.D fine chemicals. High pure (NLT 98.5%) standards
Chemicals and reagents:
(Aceclofenac, Paracetamol and Chlorozoxazone) were used for this study. HPLC grade acetonitrile were procured from
Spectrochem Pvt. Ltd. Water is prepared by mili Q system (Milli-pore).
Buffer preparation: Diluted 2.0mL of ortho phosphoric acid to 1000 mL of water. Adjusted to pH 6.0 with triethyl amine
Filtered through 0.45µm membrane filter and degassed.
Mobile Phase: Mixed the buffer and acetonitrile in the ration 67:33 v/v.
Diluent: Mobile phase.
Column : Inertsil ODS 3V (150X4.6mm, 5μm)
HPLC conditions:
Wavelength : 275nm
Injection volume: 20 μL
472
International Journal of Science Innovations and Discoveries, Volume 2, Issue 4, July-August 2012
3. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
Flow rate : 1.0 mL/min
Temperature : 30°C
Run time : 30min
Mobile phase : Buffer and Acetonitrile 67:33 v/v
Accurately weigh and transfer about 100 mg of Aceclofenac working standard into 50 mL volumetric flask, add to it about
Preparation of standard solution: For 100/ 500 / 500 mg Tablets:
30 mL of acetonitrile and sonicate to dissolve, dilute up to the mark with acetonitrile and mix well. (Concentration of
Aceclofenac is about 2000µg/mL)
Accurately weigh and transfer 100 mg of Paracetamol working standard, and 100 mg of Chlorzoxazone working standard
in to 200 mL volumetric flask, add to it about 10 mL of above Aceclofenac stock solution and sonicate to dissolve, dilute up
to the mark with mobile phase and mix well. (Concentration of Aceclofenac is about 100 µg/mL, concentration of
Paracetamol is about 500µg/mL and concentration of Chlorzoxazone is about 500µg/mL ).
Accurately weigh and transfer about 100 mg of Aceclofenac working standard into 50 mL volumetric flask, add to it about
Preparation of standard solution: For 100/ 325/ 250 mg Tablets:
30 mL of acetonitrile and sonicate to dissolve, dilute up to the mark with acetonitrile and mix well. (Concentration of
Aceclofenac is about 2000µg/mL)
Accurately weigh and transfer 65 mg of Paracetamol working standard, and 50 mg of Chlorzoxazone working standard in
to 200 mL volumetric flask, add to it about 10 mL of above Aceclofenac stock solution and sonicate to dissolve, dilute up to
the mark with mobile phase and mix well. (Concentration of Aceclofenac is about 100 µg/mL, concentration of
Paracetamol is about 325µg/mL and concentration of Chlorzoxazone is about 250µg/mL).
Accurately weigh and transfer about 100 mg of Aceclofenac working standard into 50 mL volumetric flask, add to it about
Preparation of standard solution: For 100/ 500 mg Tablets:
30 mL of acetonitrile and sonicate to dissolve, dilute up to the mark with acetonitrile and mix well. (Concentration of
Aceclofenac is about 2000µg/mL)
Accurately weigh and transfer 100 mg of Paracetamol working standard, in to 200 mL volumetric flask, add to it about 10
mL of above Aceclofenac stock solution and sonicate to dissolve, dilute up to the mark with mobile phase and mix well.
(Concentration of Aceclofenac is about 100 µg/mL, concentration of Paracetamol is about 500µg/mL).
Accurately weigh and transfer about 100 mg of Aceclofenac working standard into 50 mL volumetric flask, add to it about
Preparation of standard solution: For 100/ 500/15 mg Tablets:
30 mL of acetonitrile and sonicate to dissolve, dilute up to the mark with acetonitrile and mix well. (Concentration of
Aceclofenac is about 2000µg/mL)
Accurately weigh and transfer 100 mg of Paracetamol working standard, in to 200 mL volumetric flask, add to it about 10
mL of above Aceclofenac stock solution and sonicate to dissolve, dilute up to the mark with mobile phase and mix well.
(Concentration of Aceclofenac is about 100 µg/mL, concentration of Paracetamol is about 500µg/mL).
Accurately weigh and transfer about 100 mg of Aceclofenac working standard into 50.0 mL volumetric flask, add to it
Preparation of standard solution: For 100mg Tablets:
about 30 mL of acetonitrile and sonicate to dissolve, dilute up to the mark with acetonitrile and mix well. (Concentration
of Aceclofenac is about 2000µg/mL)
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Dilute the 10 mL of above Aceclofenac stock solution to 200 mL with mobile phase and mix well. (Concentration of
Aceclofenac is about 100 µg/mL).
Accurately weigh not less than 20 tablets and determine the average weight. Crush the tablets to fine powder. Weigh
Preparation of test solution: For 100/ 500 / 500 mg Tablets:
accurately the powder equivalent to 500 mg of Paracetamol into a 200 mL volumetric flask, add to it 20 ml of
acetonitrile and sonicate to disperse the content. Add to it 130 ml of mobile phase and sonicate to dissolve for 15 minutes
with intermittent shaking. Allow the solution cool to room temperature. Dilute to the volume with mobile phase and mix.
Filter the solution through 0.45µ nylon membrane filter. Further dilute 5 mL of the supernatant solution to 25 mL with
diluent.
Accurately weigh not less than 20 tablets and determine the average weight. Crush the tablets to fine powder. Weigh
Preparation of test solution: For 100/ 325 / 250 mg Tablets:
accurately the powder equivalent to 325 mg of Paracetamol into a 200 mL volumetric flask, add to it 20 ml of
acetonitrile and sonicate to disperse the content. Add to it 130 ml of mobile phase and sonicate to dissolve for 15 minutes
with intermittent shaking. Allow the solution cool to room temperature. Dilute to the volume with mobile phase and mix.
Filter the solution through 0.45µ nylon membrane filter. Further dilute 5 mL of the supernatant solution to 25 mL with
diluent.
Accurately weigh not less than 20 tablets and determine the average weight. Crush the tablets to fine powder. Weigh
Preparation of test solution: For 100/ 500 / 15 mg Tablets:
accurately the powder equivalent to 500 mg of Paracetamol into a 200 mL volumetric flask, add to it 20 ml of
acetonitrile and sonicate to disperse the content. Add to it 130 ml of mobile phase and sonicate to dissolve for 15 minutes
with intermittent shaking. Allow the solution cool to room temperature. Dilute to the volume with mobile phase and mix.
Filter the solution through 0.45µ nylon membrane filter. Further dilute 5 mL of the supernatant solution to 25 mL with
diluent.
Prepare the test solutions in duplicate.
Equilibrate the column with mobile phase for sufficient time until stable baseline is obtained. Inject blank, standard and
Procedure:
sample preparation filter through 0.45µ nylon filter. Inject blank (diluent) in single, standard preparation in five
replicates, and each test preparation into the chromatographic system and record the chromatograms. Inject standard
preparation as a bracketing after every six injections of test preparations. Evaluate the system suitability parameters from
the standard chromatograms. The order of elution is Paracetamol, Chlorzoxazone and Aceclofenac.
% content= Test solution area x Std. Dilution factor x Std. Potency
Standard solution area x Test dilution factor
Calculation:
RESULTS AND DISCUSSION
Standard solution was prepared as per the proposed test method and injected into the HPLC system. The results of the
System suitability:
system suitability assessment for initial validation study parameters were tabulated in Table 1.
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Table 1: System suitability
Sr. Observations
System Suitability parameter Limits
The % RSD of peak area response for
No. Aceclofenac Paracetamol Chlorzoxazone
0.3 0.1 0.2 NMT 2.0
five replicate injections of standard
1
Theoretical plates 2963 1506 3986 NLT 1000
Tailing factor 2.0 1.8 1.9 NMT 2.0
2
3
Precision Studies:
Standard solution of working standard was prepared as per the proposed test procedure for repeatability studies. Five
System Precision:
replicate injections were injected into the HPLC system. % RSD for the peak responses as the peak area was calculated,
Results are tabulated in Table 2.
Table 2: System Precision
Area Response
3481243 9580728 14147918
Injection No.
Aceclofenac Paracetamol Chlorzoxazone
3480070 9596079 14192275
1
3474685 9605600 14200613
2
3456683 9587599 14148073
3
3462315 9597724 14154756
4
3470999 9593546 14168727
5
10967.78 9602.586 25622.336
Average
0.3 0.1 0.2
SD
% RSD
Six test preparations were prepared as per the proposed test method for individual test preparation. All individual test
Method Precision:
preparations were injected into the HPLC system as per the test method. The %assay results were calculated for each
individual test sample, along with average assay and % RSD for the six preparations. The results are tabulated in Table 3.
Table 3: Method Precision Studies
% Assay
98.4 95.8 103.4
Sr. No
Aceclofenac Paracetamol Chlorzoxazone
98.1 95.9 103.4
1
98.7 95.8 103.5
2
98.6 96.1 103.9
3
98.2 95.9 103.5
4
98.8 95.6 103.2
5
98.5 95.9 103.5
6
0.2805 0.1643 0.2317
Average
0.3 0.2 0.2
SD
% RSD
Six test preparations were prepared as per the proposed test method for individual test preparation and injected into the
Ruggedness (Intermediate precision):
different HPLC system by the different analyst using different make of HPLC Column at different day.
The %assay results were calculated for each of the sample for each of the variability. Average assay values and % RSD for
the six preparations were calculated. The results are tabulated in Table 4.
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Table 4: Ruggedness
% Assay
98.8 95.8 103.8
Sr. No
Aceclofenac Paracetamol Chlorzoxazone
98.4 95.7 103.7
1
98.6 95.8 103.8
2
98.8 96.1 104.0
3
98.9 96.0 103.9
4
98.9 96.0 103.9
5
98.7 95.9 103.9
6
0.1966 0.1549 0.1049
Average
0.2 0.2 0.1
SD
% RSD
Table 5: Ruggedness data evaluation
% Assay
98.4 98.8 95.8 95.8 103.4 103.8
Sr. No
Aceclofenac Paracetamol Chlorzoxazone
98.1 98.4 95.9 95.7 103.4 103.7
1
98.7 98.6 95.8 95.8 103.5 103.8
2
98.6 98.8 96.1 96.1 103.9 104.0
3
98.2 98.9 95.9 96.0 103.5 103.9
4
98.8 98.9 95.6 96.0 103.2 103.9
5
6
Overall
98.6 95.9 103.7
Average
Overall SD 0.2697 0.1545 0.2570
Overall
0.3 0.2 0.2
% RSD
Linearity and Range:
The linearity studies of detector response for analytes were evaluated in the concentration range from about 50% of lower
Linearity of Detector Response:
strength to 150% of the higher strength of the targeted concentration. The diluted standard solutions were prepared from
stock solution in the above range and analysed using proposed analytical method by injecting each level in to the system.
The Linearity graph of average area response verses concentration was plotted and the correlation coefficient was
calculated. The results are tabulated in Table 6.
Table6: Linearity of Detector Response:
Aceclofenac Paracetamol Chlorzoxazone
Sr. No Concentration Area Concentration Area Concentration Area
29.9976 1051778 150.4635 2644943 120.2281 3603632
(g/mL) response (g/mL) response (g/mL) response
59.9951 2105682 200.6180 3519271 200.3802 6047772
1
75.9938 2451169 401.2361 7010633 320.6083 9611741
2
99.9919 3503313 501.5451 8745948 500.9505 14946798
3
109.9911 3849570 551.6996 9595498 601.1406 17884943
4
119.9903 4187013 626.9314 10901381 721.3687 21323730
5
159.9870 5600698 752.3177 13044334 761.4448 22494050
6
0.999 1.000 1.000
7
Correlation
35288.4907 17291.5590 29427.4152
Coefficient
56878.5049 55950.5535 139465.4305
Slope
Intercept
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The results obtained in accuracy study were further interpreted for the evaluation of linearity of the test method. The
Linearity of Test Method (Inferred from Accuracy):
results of average of mg added at each spiked level was plotted against average mg recovered at each accuracy level and the
correlation coefficient for set of data was evaluated. The results are tabulated in Table 7.
Table 7: Linearity of Test method (Inferred from accuracy)
For 100/500/500 mg Tablets:
Aceclofenac Paracetomol Chlorzoxazone
Recovery level Amount Amount Amount Amount Amount
Amount
Recovered Added Recovered Added Recovered
79.4 81.0 397.2 401.0 397.1 403.0
Added (mg)
(mg) (mg) (mg) (mg) (mg)
99.6 101.0 495.8 498.0 495.6 502.0
80%
119.6 121.0 594.8 590.0 595.0 594.0
100%
1.000 0.9999 0.9997
120%
Correlation
0.995 0.9565 0.9651
Coefficient
1.9627 21.9933 21.0867
Slope
Intercept
Precision at lower and higher extreme range concentration for Aceclofenac (29.9976 µg/ml and 159.9870 µg/ml),
Precision at Lower and Higher extreme concentrations:
Paracetamol (150.4635 µg/ml and 752.3177 µg/ml), and Chlorzoxazone (120.2281 µg/ml and 761.4448 µg/ml) of
Linearity levels were determined as per proposed method by injecting six replicate injections of standards for both the
levels. % RSD for peak responses for both the level was evaluated. The results are tabulated in Table 8.
Table 8: Precision at Lower and Higher extreme Levels of linearity
Area Responses
Area Responses Aceclofenac Area Responses Paracetamol
Chlorzoxazone
Injection Number
Lower level Higher level Lower level Higher level Lower level Higher level
1051198 5593151 2654481 13053921 3607531 22487458
(25%) (150%) (25%) (150%) (25%) (150%)
1053062 5599304 2655088 13029744 3605991 22475748
1
1052477 5593984 2646499 13073632 3602871 22554993
2
1051003 5598529 2637079 13028568 3600717 22472092
3
1052376 5602959 2635339 13056944 3598395 22506195
4
1050552 5616261 2641174 13023193 3606288 22467814
5
1051778 5600698 2644943 13044334 3603632 22494050
6
993.4749 8438.0317 8539.324 20088.1667 3586.7515 32895.1346
Average
0.1 0.2 0.3 0.2 0.1 0.1
SD
% RSD
An accuracy study was conducted by spiking the known amount of analytes in the equivalent weight of placebo. Accuracy
Accuracy:
study was conducted in triplicate at three different levels, (80%, 100% and 120% of target concentration). The samples
were analyzed as per the proposed test procedure and the % recovery for each spike level was calculated. The precision at
each spike level was also established.
The results are tabulated in Table 9, 10 and 11.
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Table 9: Accuracy of Aceclofenac
Aceclofenac
Recovery
Level Amount Amount Average
79.4 80.5 101.4
% Recovery % RSD
Added (mg) Recovered (mg) Recovery (%)
79.4 80.9 101.9 101.5 0.4
79.5 80.4 101.1
80%
99.6 101.7 102.1
99.6 101.1 101.5 101.7 0.3
99.6 101.2 101.6
100%
119.6 119.8 100.2
119.6 121.3 101.4 101.3 1.0
119.6 122.4 102.3
120%
Table 10: Accuracy Paracetamol
Overall 101.5 0.6
Paracetamol
Recovery
Amount Amount Average
397.1 399.9 100.7
Level % Recovery % RSD
Added (mg) Recovered (mg) Recovery (%)
397.1 402.6 101.4 101.0 0.4
397.3 400.3 100.8
80%
495.8 500.1 100.9
495.8 495.9 100.0 100.3 0.5
495.9 496.5 100.1
100%
594.8 582.6 97.9
594.8 590.9 99.3 99.2 1.3
594.8 597.3 100.4
120%
Table 11: Accuracy of Chlorzoxazone
Overall 100.2 1.0
Chlorzoxazone
Recovery
Amount Amount Average
397.1 403.6 101.6
Level % Recovery % RSD
Added (mg) Recovered (mg) Recovery (%)
397.1 405.6 102.1 101.6 0.5
397.2 401.1 101.0
80%
495.6 502.6 101.4
495.7 502.0 101.3 101.4 0.1
495.6 502.4 101.4
100%
595.0 588.2 98.9
595.0 591.4 99.4 99.8 1.2
595.0 601.3 101.1
120%
Overall 100.9 1.0
Robustness:
Mobile phase Flow rate as per proposed analytical method is 1.0 ml/min. Change in flow rate by –10% = 0.9 ml/min. Change in
Effect of variation in Flow rate of mobile phase (±10%):
flow rate by +10% = 1.1 ml/min. The effect due to change in flow rate on the system suitability parameters are compared.
Results are tabulated in Table 12.
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Table 12: System suitability of change in Flow Rate
Sr. Observations
The % RSD of Aceclofenac 0.1 0.1 0.2
System Suitability parameter Limits
No. As Such - 10% + 10%
peak area Paracetamol 0.1 0.1 0.2
response for five NMT 2.0
replicate Chlorzoxazone 0.1 0.2 0.3
1
injections
Aceclofenac 6209 6301 6158
Theoretical plates Paracetamol 2559 2697 2413 NLT 1000
Chlorzoxazone 10476 10660 9988
2
Aceclofenac 2.0 2.0 2.0
Tailing factor Paracetamol 1.4 1.4 1.3 NMT 2.0
Chlorzoxazone 1.1 1.1 1.1
3
The Column Oven temperature as per proposed analytical method is 30°C. Change in Column oven Temperature by –5°C =
Effect of variation in Column oven temperature (±5°C):
25°C. Change in Column oven Temperature by +5°C = 35°C. The effect due to change in Column oven temperature on the
system suitability parameters are compared. Results are tabulated in Table 13.
Table 13: System suitability of change in Column Oven temperature
Sr. Observations
System Suitability parameter Limits
Aceclofenac 0.1 0.1 0.5
No.
The % RSD of peak
As Such -5°C + 5°C
area response for five Paracetamol 0.1 0.0 0.1 NMT 2.0
replicate injections Chlorzoxazone 0.1 0.0 0.1
1
Aceclofenac 6209 5881 6531
Theoretical plates Paracetamol 2559 2434 2497 NLT 1000
Chlorzoxazone 10476 9784 9947
2
Aceclofenac 2.0 2.0 2.0
Tailing factor Paracetamol 1.4 1.4 1.4 NMT 2.0
Chlorzoxazone 1.1 1.1 1.1
3
The Organic phase ratio of mobile phase as per proposed analytical method is 0.2% v/v Orthophosphoric acid: Acetonitrile is
Effect of variation in organic phase composition (± 10%):
67:33 v/v. Change in Organic phase ratio of mobile phase by +10% and -10% of 0.2% v/v Orthophosphoric acid:
Acetonitrile was performed. The effect due to change in organic phase composition on the system suitability parameters are
compared. Results are tabulated in Table 14.
Table 14: System suitability of change in organic phase composition
Sr. Observations
The % RSD of peak Aceclofenac 0.1 0.2 0.1
System Suitability parameter Limits
No. As Such -5% + 5%
area response for five Paracetamol 0.2 0.1 0.2 NMT 2.0
replicate injections Chlorzoxazone 0.4 0.1 0.1
1
Aceclofenac 5973 6363 5176
Theoretical plates Paracetamol 2526 2216 2581 NLT 1000
Chlorzoxazone 8420 8537 7227
2
Aceclofenac 1.6 1.3 1.4
Tailing factor Paracetamol 1.4 1.3 1.4 NMT 2.0
Chlorzoxazone 1.1 1.1 1.1
3
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The pH of mobile phase A as per proposed analytical method is 6.0. Change in pH of mobile phase A by – 0.2 units is 5.8
Effect of variation in Mobile phase pH (± 0.2 Units):
Change in pH of mobile phase A by + 0.2 units is 6.2 The effect due to change in pH of mobile phase A on the system
suitability parameters are compared. Results are tabulated in Table 15.
Table 15: System suitability of change in mobile phase pH
Sr. Observations
System Suitability parameter Limits
The % RSD of Aceclofenac 0.2 0.1 0.0
No. As Such - 0.2 units + 0.2units
peak area Paracetamol 0.1 0.1 0.0
response for five NMT 2.0
replicate Chlorzoxazone 0.2 0.1 0.1
1
injections
Aceclofenac 6470 6225 6333
Theoretical plates Paracetamol 2055 2100 2107 NLT 1000
Chlorzoxazone 9806 9473 9646
2
Aceclofenac 1.9 1.9 1.9
Tailing factor Paracetamol 1.3 1.4 1.4 NMT 2.0
Chlorzoxazone 1.1 1.1 1.1
3
Standard solutions and sample solution were prepared. Some portion of above solutions was filtered through 0.45
Filter Interference studies:
membrane filter. Both the samples further diluted as per proposed method and injected in to the HPLC system. For
comparison the % area difference was calculated between unfiltered and filtered solutions. The data tabulated in Table 16,
Table 16: Filter paper details
17, 18 and 19.
Nylon MDI Syringe 0.45µ 25 mm SN0850
Type Make Micron size Diameter Lot No
Table 17: Filter paper interference study Aceclofenac
Aceclofenac
Average Standard Area Average Test Area
Prep. No. % %
STD-1 % Diff STD-2 Test-1 % Diff Test-2
3551905 NA 3524335 NA 3595532 NA 3591554 NA
Diff Diff
3548229 0.1 3563626 1.1 3588334 0.2 3581025 0.3
Unfiltered
0.45µFilter
Table 18: Filter paper interference study Paracetamol
Paracetamol
Average Standard Area Average Test Area
Prep. No. % %
9556575 NA 9525387 NA 9730520 NA 9753048 NA
STD-1 STD-2 % Diff Test-1 % Diff Test-2
Diff Diff
9512533 0.5 9564122 0.4 9720541 0.1 9713146 0.4
Unfiltered
0.45µFilter
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Table 19: Filter paper interference study Chlorzoxazone
Chlorzoxazone
Average Standard Area Average Test Area
Prep. No. % %
STD-1 % Diff STD-2 Test-1 % Diff Test-2
14171478 NA 14113560 NA 15017843 NA 15040877 NA
Diff Diff
14143527 0.2 14114024 0.0 14979503 0.3 14994880 0.3
Unfiltered
0.45µFilter
Test preparation was prepared as per the test method and injected into HPLC system. The peak purity result was
Peak Purity results of Sample As such:
evaluated by Photo Diode Array Detector.
The results are tabulated in Table 20 and 21.
Table 20: Sample As such Higher Strength 100/500/500 mg tablets
Peak purity results
Parameter Aceclofenac Chlorzoxazone Paracetamol
Purity-1 angle 0.071 0.271 2.092
Purity-1 threshold 0.251 0.282 6.619
Purity Flag No No No
Table 21: Sample As such Lower Strength 100/500/15 mg tablets
Peak purity results
Parameter Aceclofenac Paracetamol
Purity-1 angle 0.057 2.171
Purity-1 threshold 0.232 6.775
Purity Flag No No
The stress degradation study was carried out on the sample preparations (100/500/500 mg and 100/500/15 mg strength)
Forced Degradation studies:
of Tablet, and the degradation was evaluated by calculating the % degradation of in comparison with unstressed sample
preparation. The degradation of 10-30% was tried by following stress conditions to prove the stability indicating
characteristics of the method. The stress conditions and results were compiled in Table 22 and 23.
Table 22: % degradation data for 100/500/500 mg tablets
Aceclofenac Paracetamol Chlorzoxazone
Stress Condition % % %
Acid degradation
degradation degradation degradation
16.2 0.1 3.2
0.1N HCl, 1hr at 60°C
Alkali degradation
95.1 9.9 7.0
1N NaOH, 1hr at 80°C
Peroxide degradation
17.5 0.5 1.9
6% H2O2, 2hrs at 80°C
Thermal degradation
11.3 1.4 1.4
2 hrs at 80°C
Photolytic degradation
12.0 1.4 1.6
1.2 m.lux hrs
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Table 23: % degradation data for 100/500/15 mg tablets
Aceclofenac Paracetamol
Stress Condition % %
Acid degradation 0.1N HCl, 1hr at 60°C 10.7 3.6
degradation degradation
Alkali degradation 1N NaOH, 1hr at 80°C 98.6 19.2
Peroxide degradation 6% H2O2, 2hrs at 80°C 17.4 2.5
Thermal degradation 2 hrs at 80°C 8.2 3.0
Photolytic degradation 1.2 m.lux hrs 8.2 3.0
Solution Stability Studies:
The mobile phase was prepared as per the proposed test method and kept at room temperature for a period of two days in
Mobile phase stability at room temperature:
well closed condition. The system suitability solutions were prepared and injected into the HPLC system at initially and
periodically after 1day. The system suitability parameters were evaluated. The mobile phase was also observed for Physical
changes like haziness or precipitation. System suitability results are tabulated in Table 24.
Table 24: Mobile phase stability at room temperature
Observations
The % RSD of peak area Aceclofenac 0.2 0.1
Sr. No. System Suitability parameter Limits
Initial Day-1
response for five replicate Paracetamol 0.2 0.2 NMT 2.0
injections Chlorzoxazone 0.1 0.1
1
Aceclofenac 6737 6704
Theoretical plates Paracetamol 3013 3227 NLT 1000
Chlorzoxazone 10870 10725
2
Aceclofenac 1.9 1.8
Tailing factor Paracetamol 1.3 1.2 NMT 2.0
Chlorzoxazone 1.0 1.0
3
Standard and test preparations were prepared as per the proposed test method and the stock solutions were kept at room
Analytical Solution Stability (Standard and Test preparation) at room temperature:
temperature. The solutions were diluted freshly at each time and injected into the HPLC system at initially and at different
time intervals. The % difference in area was calculated against the fresh standard solution injected at each time interval.
The % difference in area response was evaluated against the initial assay value. The results are tabulated in Table 25, 26
Table 25: Stability of Aceclofenac Standard and test solution at room temperature
and 27.
Aceclofenac Standard Aceclofenac Test
3549534 NA 3598615 NA
Time (Hours) Area Response % Difference Area Response % Difference
3539237 0.3 3578216 0.6
Initial
3540881 0.2 3609559 0.3
4 Hrs 35 min
3559542 0.3 3597509 0.0
8 Hrs
3546836 0.1 3575222 0.7
12 Hrs 15 min
3540089 0.3 3575272 0.6
16 Hrs 20 min
3557104 0.2 3571046 0.8
20 Hrs 25 min
3528644 0.6 3562606 1.0
23 Hrs
3532159 0.5 3581784 0.5
24 Hrs 30 min
3581358 0.9 3581157 0.5
29 Hrs
3630421 2.3 3581119 0.5
33 Hrs
40 Hrs 50 min
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Table 26: Stability of Paracetamol Standard and test solution at room temperature
Paracetamol Standard Paracetamol Test
9533772 NA 9674499 NA
Time (Hours) Area Response % Difference Area Response % Difference
9485553 0.5 9681641 0.1
Initial
9529119 0.0 9720005 0.5
4 Hrs 35 min
9562369 0.3 9713140 0.4
8 Hrs
9558274 0.3 9703185 0.3
12 Hrs 15 min
9551274 0.2 9705705 0.3
16 Hrs 20 min
9554327 0.2 9673281 0.0
20 Hrs 25 min
9551111 0.2 9659821 0.2
23 Hrs
9541020 0.1 9661378 0.1
24 Hrs 30 min
9619965 0.9 9674547 0.0
29 Hrs
9760962 2.4 9661793 0.1
33 Hrs
Table 27: Stability of Chlorzoxazone Standard and test solution at room temperature
40 Hrs 50 min
Chlorzoxazone Standard Chlorzoxazone Test
14101688 NA 14905697 NA
Time (Hours) Area Response % Difference Area Response % Difference
14074515 0.2 14896823 0.1
Initial
14105493 0.0 15018775 0.8
4 Hrs 35 min
14182706 0.6 14980781 0.5
8 Hrs
14175597 0.5 14922091 0.1
12 Hrs 15 min
14185354 0.6 14925356 0.1
16 Hrs 20 min
14165758 0.5 14885819 0.1
20 Hrs 25 min
14150058 0.3 14871542 0.2
23 Hrs
14064098 0.3 14908388 0.0
24 Hrs 30 min
14290784 1.3 14911371 0.0
29 Hrs
14499323 2.8 14930540 0.2
33 Hrs
40 Hrs 50 min
BLANK CHROMATOGRAM
483
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14. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
STANDARD CHROMATOGRAM
TEST CHROMATOGRAM
LINEARITY OF DETECTOR RESPONSE OF ACECLOFENAC
484
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15. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
LINEARITY OF DETECTOR RESPONSE OF PARACETAMOL
LINEARITY OF DETECTOR RESPONSE OF CHLORZOXAZONE
LINEARITY GRAPH (INFERRED FROM ACCURACY STUDIES) OF ACECLOFENAC
485
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16. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
LINEARITY GRAPH (INFERRED FROM ACCURACY STUDIES) OF PARACETAMOL
LINEARITY GRAPH (INFERRED FROM ACCURACY STUDIES) OF CHLORZOXAZONE
AS SUCH SAMPLE CHROMATOGRAM HIGHER STRENGTH
486
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17. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
AS SUCH SAMPLE PURITY PLOT HIGHER STRENGTH
AS SUCH SAMPLE CHROMATOGRAM LOWER STRENGTH
487
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18. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
AS SUCH SAMPLE PURITY PLOT LOWER STRENGTH
ACID DEGRADATION SAMPLE CHROMATOGRAM HIGHER STRENGTH
488
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19. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
ALKALI DEGRADATION SAMPLE CHROMATOGRAM HIGHER STRENGTH
PEROXIDE DEGRADATION SAMPLE CHROMATOGRAM HIGHER STRENGTH
THERMAL DEGRADATION SAMPLE CHROMATOGRAM HIGHER STRENGTH
489
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20. Hari Kishan Reddy Ganthi et al., IJSID, 2012, 2 (4), 471-490
PHOTOLYTIC DEGRADATION SAMPLE CHROMATOGRAM HIGHER STRENGTH
The complete study results reveals that the developed and validated RP-HPLC method is accurate, precise, robust and
CONCLUSION
stability indicating. This method has wide applicability and useful for regular quality control analysis of formulation samples.
1. Granberg RA, Rasmuson AC, Solubility of paracetamol in pure solvents, Journal of Chemical & Engineering Data, 1999, 44
REFERENCES
(6), 1391–1395.
2. Acetaminophen Drugs.com
3. Bertolini A, Ferrari A, Ottani A, Guerzoni S, Tacchi R, Leone S, Paracetamol: new vistas of an old drug, CNS drug reviews,
2006, 12 (3–4), 250–275.
4. Altinoz MA, Korkmaz R, NF-kappaB, macrophage migration inhibitory factor and cyclooxygenase-inhibitions as likely
mechanisms behind the acetaminophen- and NSAID-prevention of the ovarian cancer, Neoplasma, 2004, 51 (4), 239–247.
5. Moller, P, Sindet-Pedersen S, Petersen C, Juhl G, Dillenschneider A, Skoglund L, Onset of acetaminophen analgesia:
comparison of oral and intravenous routes after third molar surgery, British journal of anaesthesia, 2005, 94 (5): 642–
648.
6. Viswanathan, Feskanich, Schernhammer ES, Aspirin, NSAID and Acetaminophen use and the Risk of Endometrial Cancer,
Cancer Research, 2008, 68 (7), 2507.
7. Acetaminophen, chemicalland21.com, 2011.
8. Byrant, Bronwen, Knights, Katleen, Salerno, Evelyn, Pharmacology for health professionals, Elsevier, 2007, 270.
9. International Conference on Harmonization, Q2A: Text on Validation of Analytical Procedures, Federal Register, 1995, 60
(40), 11260–11262.
10. FDA, Analytical Procedures and Methods Validation: Chemistry, Manufacturing and Controls Documentation, Availability,
Federal Register (Notices), 2000, 65(169), 52776–52777.
11. International Conference on Harmonization, Q2B: Validation of Analytical Procedures: Methodology and
Availability, Federal Register, 1997, 62 (96), 27463–27467.
12. USP 25–NF 20, Validation of Compendial Methods Section (1225) (United States Pharmacopeal Convention, Rockville,
Maryland, USA, 2002), 2256.
490
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