Related Substances-Method Validation-PPT_slideBhanu Prakash N
This document provides an overview of analytical method validation. It defines validation as demonstrating a method is suitable for its intended purpose. Key validation characteristics discussed include precision, accuracy, specificity, linearity, range, detection limit, quantitation limit, ruggedness and robustness. The document describes the methodology for evaluating each characteristic, such as spiking known concentrations of analytes and establishing acceptance criteria. It emphasizes that validation confirms a method consistently produces results meeting pre-defined standards of quality.
In 3 sentences:
This document discusses different methods for determining drug absorption - in vitro, in vivo, and in situ. In vitro methods determine permeability outside the body using tissues. In vivo methods are conducted inside the body by measuring drug levels in blood/urine. In situ methods simulate in vivo conditions by perfusing intestinal segments to determine drug diffusion rates.
Analytical method validation as per ich and usp shreyas B R
Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
Dissolution : Official and Non official methods, Alternative methods of dissolution testing and transport models, Drug release testing, Invitro drug release testing
This document discusses the key aspects of analytical method validation including specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability testing. It provides detailed descriptions and recommendations for establishing each validation characteristic to demonstrate that an analytical procedure is suitable for its intended use.
This document discusses in-vivo methods for determining drug permeability and absorption. It describes two main types of in-vivo methods: direct and indirect. The direct method involves measuring drug levels in blood or urine over time after administration to determine the rate and extent of absorption. The indirect method measures pharmacological response instead of drug concentration when direct measurement is difficult. In-vivo methods provide a more precise understanding of factors like gastric emptying and drug effects on the gastrointestinal tract compared to in-vitro or in situ methods.
Validation of cone blender, mixer granulator and tablet compression machine.MayuriGhavate
The document summarizes the validation process for common pharmaceutical equipment used in powder blending, granulation, and tablet compression. It discusses the validation of cone blenders, mixers, granulators, and tablet compression machines. The validation process involves design qualification, installation qualification, operational qualification, and performance qualification to ensure equipment is properly designed, installed, operated, and performs as intended. Key aspects that are validated include design criteria, utilities, cleaning procedures, operating parameters, and finished product quality attributes. Validation helps improve safety, reproducibility, and compliance for pharmaceutical manufacturing.
Related Substances-Method Validation-PPT_slideBhanu Prakash N
This document provides an overview of analytical method validation. It defines validation as demonstrating a method is suitable for its intended purpose. Key validation characteristics discussed include precision, accuracy, specificity, linearity, range, detection limit, quantitation limit, ruggedness and robustness. The document describes the methodology for evaluating each characteristic, such as spiking known concentrations of analytes and establishing acceptance criteria. It emphasizes that validation confirms a method consistently produces results meeting pre-defined standards of quality.
In 3 sentences:
This document discusses different methods for determining drug absorption - in vitro, in vivo, and in situ. In vitro methods determine permeability outside the body using tissues. In vivo methods are conducted inside the body by measuring drug levels in blood/urine. In situ methods simulate in vivo conditions by perfusing intestinal segments to determine drug diffusion rates.
Analytical method validation as per ich and usp shreyas B R
Analytical method validation is a process of documenting/ proving that an analytical method provides analytical data acceptable for the intended use.After the development of an analytical procedure, it is must important to assure that the procedure will consistently produce the intended a precise result with high degree of accuracy. The method should give a specific result that may not be affected by external matters. This creates a requirement to validate the analytical procedures. The validation procedures consists of some characteristics parameters that makes the method acceptable with addition of statistical tools.
Dissolution : Official and Non official methods, Alternative methods of dissolution testing and transport models, Drug release testing, Invitro drug release testing
This document discusses the key aspects of analytical method validation including specificity, linearity, range, accuracy, precision, detection limit, quantitation limit, robustness, and system suitability testing. It provides detailed descriptions and recommendations for establishing each validation characteristic to demonstrate that an analytical procedure is suitable for its intended use.
This document discusses in-vivo methods for determining drug permeability and absorption. It describes two main types of in-vivo methods: direct and indirect. The direct method involves measuring drug levels in blood or urine over time after administration to determine the rate and extent of absorption. The indirect method measures pharmacological response instead of drug concentration when direct measurement is difficult. In-vivo methods provide a more precise understanding of factors like gastric emptying and drug effects on the gastrointestinal tract compared to in-vitro or in situ methods.
Validation of cone blender, mixer granulator and tablet compression machine.MayuriGhavate
The document summarizes the validation process for common pharmaceutical equipment used in powder blending, granulation, and tablet compression. It discusses the validation of cone blenders, mixers, granulators, and tablet compression machines. The validation process involves design qualification, installation qualification, operational qualification, and performance qualification to ensure equipment is properly designed, installed, operated, and performs as intended. Key aspects that are validated include design criteria, utilities, cleaning procedures, operating parameters, and finished product quality attributes. Validation helps improve safety, reproducibility, and compliance for pharmaceutical manufacturing.
This document discusses drug product performance and bioequivalence studies. It defines drug product performance as the release of the drug substance from the product leading to bioavailability, which relates to clinical safety and efficacy. Bioequivalence studies compare formulations and are used to assess the impact of changes to the drug substance, formulation, or manufacturing process. They can be conducted in vivo using pharmacokinetic or pharmacodynamic endpoints or in vitro using dissolution studies.
This document discusses various compendial methods for drug dissolution testing. It begins by defining dissolution as the process where a solid substance solubilizes in a solvent, transferring mass from the solid surface to the liquid phase. It then describes the seven USP dissolution apparatus types and their applications for testing different drug products like tablets, capsules, modified release formulations and transdermal systems. The document provides details on factors that influence dissolution test design and the principles of operation for each apparatus type.
The release of the drug substance from the drug product leading to the bioavailability of the drug substance. The assessment of drug product performance is imp. Since bioavailability is related both to the pharmacodynamic responses and the adverse events. The performance tests relate the quality of a drug product to clinical safety and efficacy.
Bioavailability studies are drug product performance studies used to define
the effect of changes in the physicochemical properties of the drug substance, the formulation of the drug, and the manufacturing process of the drug product.
SELF MICRO EMULSIFYING DRUG DELIVERY SYSTEM [SMEDDS]Sagar Savale
Oral route is the main route of drug administration in many diseases. Major problem in oral route of drug administration is bioavailability which mainly results from poor aqueous solubility. This leads to lack of dose uniformity and high intrasubject/intersubject variability. It is found that 40% of active substances are poorly water-soluble. Various technologies are developed to overcome this problem, like solid dispersion or complex formation. Much attention has been given to lipid-based formulation with particular emphasis on self-micro emulsifying drug delivery system to improve the oral bioavailability of lipophilic drugs. It requires small amount of dose and also drugs can be protected from hostile environment in gut. Self-micro emulsifying drug delivery systems are specialized form of delivery system in which drug is encapsulated in a lipid base with or without pharmaceutical acceptable surfactant.
Problems of variable control in dissolution testing discusses issues that can affect the results of dissolution testing. Dissolution testing is important for characterizing drug release from oral solid dosages and ensuring bioavailability. However, variables like equipment alignment and agitation levels can increase variability in dissolution rates measured. Both the paddle and basket methods are sensitive to different issues like tilting, clogging, or air bubbles. No single method works best for all products, so selection depends on the specific drug formulation and optimizing test conditions.
This document discusses alternative non-official methods for measuring drug dissolution that do not require a sink condition. It describes natural convection non-sink methods including the Klein solvmeter, Nelson hanging pellet, and Levy static disk methods. Forced convection non-sink methods are also covered, such as the tumbling, beaker, and rotating disk methods. Each method is explained in one to two sentences, outlining how the drug dosage form is placed in the dissolution medium and how samples are collected and analyzed over time to determine the dissolution rate.
This document compares different methods for comparing dissolution profiles of drug products. It defines dissolution profile comparison and its objectives such as developing bioequivalent products and in vitro-in vivo correlations. Graphical, statistical, model-dependent and model-independent methods are described. The most common model-independent method is the f2 similarity factor test recommended by the FDA, which provides a single value to determine if two dissolution profiles are similar based on the percent dissolved over time. Proper selection of time points and criteria for coefficient of variation are important for f2 testing.
This document discusses biopharmaceutical factors that can affect the bioavailability of drugs. It focuses on pharmaceutical factors including physicochemical properties of drug molecules and dosage form characteristics. Physicochemical properties like solubility, dissolution rate, particle size, polymorphism, salt form, and ionization state can impact drug absorption. The pH-partition hypothesis explains how a drug's pKa and lipid solubility relate to absorption based on gastrointestinal pH. Dosage form properties such as disintegration time, manufacturing methods, and ingredients are also discussed as formulation factors influencing bioavailability.
The document describes the development and validation of UV spectrophotometric methods for analyzing risperidone and lacosamide. It discusses selecting analytical wavelengths, developing standard curves, and validating the methods by determining accuracy, precision, specificity, linearity, range and other parameters as required by ICH guidelines. Validation results for the risperidone and lacosamide methods such as recovery percentages between 98.4-99.8%, precision of 0.67-0.50%, linear ranges of 2-6 μg/ml and 12-40 μg/ml respectively are also presented. The developed and validated methods provide accurate and precise quantification of active pharmaceutical ingredients and finished dosage forms using UV spectrophotometry.
USFDA guidelines for bioanalytical method validationbhatiaji123
The document discusses guidelines for bioanalytical method validation from the USFDA. It describes key parameters that must be validated for a bioanalytical method, including selectivity, accuracy, precision, recovery, calibration curves, sensitivity, reproducibility and stability. Accuracy and precision are determined by analyzing quality control samples in replicates across multiple runs. Recovery experiments compare extracted samples to unextracted standards. A calibration curve consisting of multiple concentrations over the expected range must be precise and reproducible.
The document provides an overview of optimization techniques used in pharmaceutical formulation and processing. It begins by defining optimization and its importance in developing drug products that meet bioavailability and mass production requirements. The key parameters of optimization discussed are problem type (constrained vs unconstrained), variables (independent vs dependent), and application areas (formulation vs processing). Several optimization techniques are then outlined, including evolutionary operations, simplex method, Lagrangian method, search method, and canonical analysis. Examples of each technique are provided, such as using simplex to optimize an analytical method or the Lagrangian method to optimize tablet formulation based on two variables.
Human liver microsomes & rat liver microsomesgaurav sharma
Human and rat liver microsomes are subcellular fractions containing cytochrome P450 enzymes and other drug-metabolizing enzymes. They are commonly used in vitro to study drug metabolism and interactions. Human liver microsomes are obtained from human liver tissue through differential centrifugation and contain enzymes for phase I and phase II drug metabolism. They are useful for identifying drug metabolites, evaluating interspecies differences, predicting in vivo clearance, and studying interindividual variability in drug metabolism. Rat liver microsomes were also discussed as an experimental model. Incubation methods and analytical techniques like HPLC were described for evaluating metabolism using liver microsomes.
Analytical method transfer involves qualifying a receiving laboratory to perform an analytical test procedure originally developed in a transferring laboratory. It ensures the receiving laboratory has the knowledge and ability to carry out the procedure as intended. There are different types of method transfers, including comparative testing, co-validation between laboratories, revalidation/partial validation, and waivers. Both the transferring and receiving laboratories have responsibilities in the method transfer process, which typically involves testing replicate samples, evaluating acceptance criteria, and documenting the transfer in a protocol.
This document discusses how drug transporters affect the absorption, distribution, and excretion of drugs. It describes uptake and efflux transporters expressed in the intestine, liver, kidney, and blood-brain barrier that determine drug concentrations in tissues. Inhibition or induction of these transporters by other drugs can impact the pharmacokinetics and pharmacodynamics of victim drugs. The document then classifies and provides examples of important uptake transporters like OATPs and OCTs and efflux transporters like P-gp, BCRP, MRP2, and BSEP, noting their tissue expression and roles in drug absorption, distribution, and excretion.
This document discusses bioavailability and bioequivalence studies, which are essential to ensure uniform quality, efficacy, and safety of pharmaceutical products. Bioavailability refers to the amount and rate of drug absorption from its dosage form into systemic circulation. Bioequivalence compares the rate and extent of absorption of a test product to a reference product. The document outlines various study designs used in bioequivalence studies, including crossover, parallel, and replicated designs. It also discusses the statistical evaluation of these studies and requirements for establishing bioequivalence.
This document discusses methods for comparing drug dissolution profiles, which provide information about how completely and quickly an active pharmaceutical ingredient is released from its dosage form. Graphical and statistical methods are described for directly comparing dissolution curves. Model-dependent approaches apply kinetic models like zero-order, first-order, and Higuchi models to the data. Model-independent methods calculate similarity factors f1 and f2 that provide single values for comparing profiles. Comparing dissolution profiles is important for evaluating drug release and bioequivalence of pharmaceutical formulations.
postmarketing surviellance,,outsourcing of BA ,BE , CRO. supriyawable1
This document provides an overview of post-marketing surveillance, outsourcing of bioavailability and bioequivalence studies to contract research organizations. It discusses the need for post-marketing surveillance to identify rare or long-term adverse drug reactions not seen in clinical trials. Methods for post-marketing surveillance include controlled trials, spontaneous reporting, cohort and case-control studies. Outsourcing bioavailability and bioequivalence studies to CROs can help reduce costs and improve resource efficiency for pharmaceutical companies.
This document discusses various study designs used in bioequivalence studies. It describes the objectives of such studies as determining if a test product is bioequivalent to a reference product when administered at the same molar dose under similar conditions. Some key study designs discussed include non-replicated parallel studies for long-acting drugs, multiple dose steady state studies, and clinical endpoint studies comparing therapeutic effects. Special considerations are also noted for highly variable drugs.
Simultaneous estimation and validation of atenolol hydrochloro thiazide and l...srirampharma
This document describes the development and validation of a reverse phase HPLC method for the simultaneous estimation of atenolol, hydrochlorothiazide, and losartan K from pharmaceutical tablet dosage forms. The method utilizes a C18 column with a mobile phase of acetonitrile and phosphate buffer at a ratio of 70:30 delivered at 1.2 mL/min. The drugs were detected at 229 nm and provided good resolution and peak symmetry. The developed method was validated in terms of accuracy, precision, linearity, limits of detection and quantification, robustness, and solution stability. The method was applied to a commercial tablet dosage form and found to provide accurate results within 100% of the labeled claim for each drug.
Global Medical Cures™ | Crestor- Post Marketing Adverse Event ReviewGlobal Medical Cures™
The AERS search identified 2 fatal pediatric cases and 10 non-fatal serious pediatric cases associated with rosuvastatin use from 2003-2010. Both fatal cases involved in utero exposure to rosuvastatin. Of the 10 non-fatal cases, 7 involved accidental exposure in children under 3 years old. The other cases included a suicide attempt, in utero exposure, and diarrhea with increased liver enzymes in a 16-year-old transplant patient taking rosuvastatin. The cases did not identify adverse events unique to pediatrics. More information would be needed to determine if rosuvastatin caused the reported events.
This document discusses drug product performance and bioequivalence studies. It defines drug product performance as the release of the drug substance from the product leading to bioavailability, which relates to clinical safety and efficacy. Bioequivalence studies compare formulations and are used to assess the impact of changes to the drug substance, formulation, or manufacturing process. They can be conducted in vivo using pharmacokinetic or pharmacodynamic endpoints or in vitro using dissolution studies.
This document discusses various compendial methods for drug dissolution testing. It begins by defining dissolution as the process where a solid substance solubilizes in a solvent, transferring mass from the solid surface to the liquid phase. It then describes the seven USP dissolution apparatus types and their applications for testing different drug products like tablets, capsules, modified release formulations and transdermal systems. The document provides details on factors that influence dissolution test design and the principles of operation for each apparatus type.
The release of the drug substance from the drug product leading to the bioavailability of the drug substance. The assessment of drug product performance is imp. Since bioavailability is related both to the pharmacodynamic responses and the adverse events. The performance tests relate the quality of a drug product to clinical safety and efficacy.
Bioavailability studies are drug product performance studies used to define
the effect of changes in the physicochemical properties of the drug substance, the formulation of the drug, and the manufacturing process of the drug product.
SELF MICRO EMULSIFYING DRUG DELIVERY SYSTEM [SMEDDS]Sagar Savale
Oral route is the main route of drug administration in many diseases. Major problem in oral route of drug administration is bioavailability which mainly results from poor aqueous solubility. This leads to lack of dose uniformity and high intrasubject/intersubject variability. It is found that 40% of active substances are poorly water-soluble. Various technologies are developed to overcome this problem, like solid dispersion or complex formation. Much attention has been given to lipid-based formulation with particular emphasis on self-micro emulsifying drug delivery system to improve the oral bioavailability of lipophilic drugs. It requires small amount of dose and also drugs can be protected from hostile environment in gut. Self-micro emulsifying drug delivery systems are specialized form of delivery system in which drug is encapsulated in a lipid base with or without pharmaceutical acceptable surfactant.
Problems of variable control in dissolution testing discusses issues that can affect the results of dissolution testing. Dissolution testing is important for characterizing drug release from oral solid dosages and ensuring bioavailability. However, variables like equipment alignment and agitation levels can increase variability in dissolution rates measured. Both the paddle and basket methods are sensitive to different issues like tilting, clogging, or air bubbles. No single method works best for all products, so selection depends on the specific drug formulation and optimizing test conditions.
This document discusses alternative non-official methods for measuring drug dissolution that do not require a sink condition. It describes natural convection non-sink methods including the Klein solvmeter, Nelson hanging pellet, and Levy static disk methods. Forced convection non-sink methods are also covered, such as the tumbling, beaker, and rotating disk methods. Each method is explained in one to two sentences, outlining how the drug dosage form is placed in the dissolution medium and how samples are collected and analyzed over time to determine the dissolution rate.
This document compares different methods for comparing dissolution profiles of drug products. It defines dissolution profile comparison and its objectives such as developing bioequivalent products and in vitro-in vivo correlations. Graphical, statistical, model-dependent and model-independent methods are described. The most common model-independent method is the f2 similarity factor test recommended by the FDA, which provides a single value to determine if two dissolution profiles are similar based on the percent dissolved over time. Proper selection of time points and criteria for coefficient of variation are important for f2 testing.
This document discusses biopharmaceutical factors that can affect the bioavailability of drugs. It focuses on pharmaceutical factors including physicochemical properties of drug molecules and dosage form characteristics. Physicochemical properties like solubility, dissolution rate, particle size, polymorphism, salt form, and ionization state can impact drug absorption. The pH-partition hypothesis explains how a drug's pKa and lipid solubility relate to absorption based on gastrointestinal pH. Dosage form properties such as disintegration time, manufacturing methods, and ingredients are also discussed as formulation factors influencing bioavailability.
The document describes the development and validation of UV spectrophotometric methods for analyzing risperidone and lacosamide. It discusses selecting analytical wavelengths, developing standard curves, and validating the methods by determining accuracy, precision, specificity, linearity, range and other parameters as required by ICH guidelines. Validation results for the risperidone and lacosamide methods such as recovery percentages between 98.4-99.8%, precision of 0.67-0.50%, linear ranges of 2-6 μg/ml and 12-40 μg/ml respectively are also presented. The developed and validated methods provide accurate and precise quantification of active pharmaceutical ingredients and finished dosage forms using UV spectrophotometry.
USFDA guidelines for bioanalytical method validationbhatiaji123
The document discusses guidelines for bioanalytical method validation from the USFDA. It describes key parameters that must be validated for a bioanalytical method, including selectivity, accuracy, precision, recovery, calibration curves, sensitivity, reproducibility and stability. Accuracy and precision are determined by analyzing quality control samples in replicates across multiple runs. Recovery experiments compare extracted samples to unextracted standards. A calibration curve consisting of multiple concentrations over the expected range must be precise and reproducible.
The document provides an overview of optimization techniques used in pharmaceutical formulation and processing. It begins by defining optimization and its importance in developing drug products that meet bioavailability and mass production requirements. The key parameters of optimization discussed are problem type (constrained vs unconstrained), variables (independent vs dependent), and application areas (formulation vs processing). Several optimization techniques are then outlined, including evolutionary operations, simplex method, Lagrangian method, search method, and canonical analysis. Examples of each technique are provided, such as using simplex to optimize an analytical method or the Lagrangian method to optimize tablet formulation based on two variables.
Human liver microsomes & rat liver microsomesgaurav sharma
Human and rat liver microsomes are subcellular fractions containing cytochrome P450 enzymes and other drug-metabolizing enzymes. They are commonly used in vitro to study drug metabolism and interactions. Human liver microsomes are obtained from human liver tissue through differential centrifugation and contain enzymes for phase I and phase II drug metabolism. They are useful for identifying drug metabolites, evaluating interspecies differences, predicting in vivo clearance, and studying interindividual variability in drug metabolism. Rat liver microsomes were also discussed as an experimental model. Incubation methods and analytical techniques like HPLC were described for evaluating metabolism using liver microsomes.
Analytical method transfer involves qualifying a receiving laboratory to perform an analytical test procedure originally developed in a transferring laboratory. It ensures the receiving laboratory has the knowledge and ability to carry out the procedure as intended. There are different types of method transfers, including comparative testing, co-validation between laboratories, revalidation/partial validation, and waivers. Both the transferring and receiving laboratories have responsibilities in the method transfer process, which typically involves testing replicate samples, evaluating acceptance criteria, and documenting the transfer in a protocol.
This document discusses how drug transporters affect the absorption, distribution, and excretion of drugs. It describes uptake and efflux transporters expressed in the intestine, liver, kidney, and blood-brain barrier that determine drug concentrations in tissues. Inhibition or induction of these transporters by other drugs can impact the pharmacokinetics and pharmacodynamics of victim drugs. The document then classifies and provides examples of important uptake transporters like OATPs and OCTs and efflux transporters like P-gp, BCRP, MRP2, and BSEP, noting their tissue expression and roles in drug absorption, distribution, and excretion.
This document discusses bioavailability and bioequivalence studies, which are essential to ensure uniform quality, efficacy, and safety of pharmaceutical products. Bioavailability refers to the amount and rate of drug absorption from its dosage form into systemic circulation. Bioequivalence compares the rate and extent of absorption of a test product to a reference product. The document outlines various study designs used in bioequivalence studies, including crossover, parallel, and replicated designs. It also discusses the statistical evaluation of these studies and requirements for establishing bioequivalence.
This document discusses methods for comparing drug dissolution profiles, which provide information about how completely and quickly an active pharmaceutical ingredient is released from its dosage form. Graphical and statistical methods are described for directly comparing dissolution curves. Model-dependent approaches apply kinetic models like zero-order, first-order, and Higuchi models to the data. Model-independent methods calculate similarity factors f1 and f2 that provide single values for comparing profiles. Comparing dissolution profiles is important for evaluating drug release and bioequivalence of pharmaceutical formulations.
postmarketing surviellance,,outsourcing of BA ,BE , CRO. supriyawable1
This document provides an overview of post-marketing surveillance, outsourcing of bioavailability and bioequivalence studies to contract research organizations. It discusses the need for post-marketing surveillance to identify rare or long-term adverse drug reactions not seen in clinical trials. Methods for post-marketing surveillance include controlled trials, spontaneous reporting, cohort and case-control studies. Outsourcing bioavailability and bioequivalence studies to CROs can help reduce costs and improve resource efficiency for pharmaceutical companies.
This document discusses various study designs used in bioequivalence studies. It describes the objectives of such studies as determining if a test product is bioequivalent to a reference product when administered at the same molar dose under similar conditions. Some key study designs discussed include non-replicated parallel studies for long-acting drugs, multiple dose steady state studies, and clinical endpoint studies comparing therapeutic effects. Special considerations are also noted for highly variable drugs.
Simultaneous estimation and validation of atenolol hydrochloro thiazide and l...srirampharma
This document describes the development and validation of a reverse phase HPLC method for the simultaneous estimation of atenolol, hydrochlorothiazide, and losartan K from pharmaceutical tablet dosage forms. The method utilizes a C18 column with a mobile phase of acetonitrile and phosphate buffer at a ratio of 70:30 delivered at 1.2 mL/min. The drugs were detected at 229 nm and provided good resolution and peak symmetry. The developed method was validated in terms of accuracy, precision, linearity, limits of detection and quantification, robustness, and solution stability. The method was applied to a commercial tablet dosage form and found to provide accurate results within 100% of the labeled claim for each drug.
Global Medical Cures™ | Crestor- Post Marketing Adverse Event ReviewGlobal Medical Cures™
The AERS search identified 2 fatal pediatric cases and 10 non-fatal serious pediatric cases associated with rosuvastatin use from 2003-2010. Both fatal cases involved in utero exposure to rosuvastatin. Of the 10 non-fatal cases, 7 involved accidental exposure in children under 3 years old. The other cases included a suicide attempt, in utero exposure, and diarrhea with increased liver enzymes in a 16-year-old transplant patient taking rosuvastatin. The cases did not identify adverse events unique to pediatrics. More information would be needed to determine if rosuvastatin caused the reported events.
The main objective of the present research work is to formulate the Clopidogrel Fast Dissolving tablets. Clopidogrel, an antiplatelet drug, belongs to BCS Class-II and used to control Heart attack, Hypertension by inhibiting Platelet activation and aggregation .The Fast Dissolving tablets of Clopidogrel were prepared employing different concentrations of Crospovidone and Croscarmellose sodium in different combinations as a Superdisintegrant by Direct Compression technique using 32 factorial design. The concentration of Crospovidone and Croscarmellose sodium was selected as independent variables, X1 and X2 respectively whereas, wetting time, Disintegration time, t50%, t90% were selected as dependent variables. Totally nine formulations were designed and evaluated for hardness, friability, thickness, Assay, Wetting time, Disintegration time, and in-vitro drug release. From the Results it was concluded that all the formulation were found to be with in the Pharmacopoeial limits and the in-vitro dissolution profiles of all formulations were fitted into different Kinetic models, the statistical parameters like intercept (a), slope (b) and regression coefficient (r) were calculated. Polynomial equations were developed for Wetting time, Disintegration time, t50%, t90%. Validity of developed polynomial equations was verified by designing 2 check point formulations (C1, C2). According to SUPAC guidelines, the formulation (F5) containing combination of 15% Crospovidone and 15% Croscarmellose, is the most similar formulation (similarity factor f2=91.3936, dissimilarity factor f1= 1.203& No significant difference, t= -0.00062) to marketed product (PLAVIX-75). The selected formulation (F1) follows First order, Higuchi’s kinetics, mechanism of drug release found to be Fickian Diffusion (n= 0.226).
This document provides a product list from Zim Labs categorized by medical condition or disease. It includes over 50 products across categories like anti-rheumatoid, anti-hypertensive, anti-diabetic, anti-microbial, vitamins and minerals. The products are available in various forms like tablets, capsules, granules for oral suspension. The list covers a wide range of therapeutic areas and provides dosage strengths for each product.
A Simple Rp- HPLC Method for Simultaneous Estimation of Six Cardiovascular Dr...iosrjce
A simple, convenient Rp-HPLC method has been developed and validated for the simultaneous
estimation of Metolazone, Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone. The column
used was an Inertsil ODS 3 V column of 250 mm length × 4.6 mm ID, with 3 micron particle size of adsorbent.
Separation was achieved using isocratic elution in a buffer-acetonitrile-methanol mobile phase at a flow rate of
1.2 ml/min. The detection was performed at wavelength of 225 nm using a UV detector. The column temperature
was 450C and injection volume was 20µl. The method was validated for precision, linearity and accuracy. The
% RSD for all the drugs was found to be less than 2 %. The correlation coefficient (r2
) was not less than 0.999
for all drugs. The mean percent recovery of the drugs from tablet placebo at 50%, 100% and 150% were within
limits. The marketed formulations of the drugs were analyzed and the mean assay results were found to be
within limits. The developed method can thus be employed for routine simultaneous analysis of Metolazone,
Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone in bulk and in their marketed
formulations
ABSTRACT
The main objective of present research work is to formulate the of Domperidone Maleate floating tablets.
Domperidone Maleate, an antiemetic and a prokinetic agent belongs to BCS Class-II and Indicated for treatment of
upper gastrointestinal motility disorders by blocking the action of Dopamine. The Floating tablets of Domperidone
Maleate were prepared employing different concentrations of HPMCK4M and Guar Gum in different combinations
as a release rate modifiers by Direct Compression technique using 32 factorial design. The concentration of
HPMCK4M and Guar Gum was selected as independent variables, X1 and X2 respectively whereas, time required
for drug dissolution t10%, t50%,t75%,t90%were selected as dependent variables. Totally nine formulations were designed
and are evaluated for hardness, friability, thickness, Assay, Floating Lag time, In-vitro drug release. From the
Results concluded that all the formulation were found to be with in the Pharmacopoeial limits and the In-vitro
dissolution profiles of all formulations were fitted in to different Kinetic models, the statistical parameters like
intercept (a), slope (b) & regression coefficient (r) were calculated. Polynomial equations were developed for t10%,
t50%, t75%, t90%. Validity of developed polynomial equations were verified by designing 2 check point formulations(C1,
C2). According to SUPAC guidelines the formulation (F5) containing combination of 18.75% HPMCK4M and
18.75% Guar Gum, is the most similar formulation (similarity factor f2=89.03, dissimilarity factor f1= 11.539& No
significant difference, t= 0.169) to marketed product (DOMSTAL OD). The selected formulation (F5) follows
Higuchi’s kinetics, and the mechanism of drug release was found to be Non-Fickian Diffusion (n= 0.925).
Keywords: Domperidone Maleate, 32Factorial Design, Gastro retentive Floating Tablet, HPMCK100M, Sodium
bicarbonate, Floating Lag Time, SUPAC, Non-Fickian Diffusion Mechanism.
Traditional Kashmiri Recipe “Shangri-Kahwa” as a Stimulant Drink and Effectiv...SriramNagarajan15
The popular recipe “Shangri-kahwa” is an age old home remedy for respiratory and various other problems in almost whole of Kashmir. It is prepared from important spices like liquorice, clove, cinnamon, and cardamom, which have documented health benefits. Information about its use and method of preparation was obtained from group discussions held in some villages of Baramullah district of Jammu and Kashmir. People in these villages believe that Shangri-kahwa is cost effective, delicious, made from easily available ingredients and can be prepared easily at home. Being residents of this area, the authors are aware of the popularity of this magical drink used as a first line of treatment for various ailments at home, particularly during cold days. This recipe is extremely famous in these villages both as a refreshing and stimulant drink, as well as believed to be highly efficacious in respiratory illnesses. It is cost effective and highly palatable. The ingredients of Shangri-kahwa are being used extensively in Unani system of medicine and Ayurveda for almost same indications as the recipe is used. This study was carried out to highlight the effectiveness and focus the attention of the researchers towards this attractive and effective dosage form used as home remedy in Kashmir.
Spectrophotometric Estimation of Rosuvastatin Calcium in Bulk and Pharmaceuti...pharmaindexing
This document describes the development and validation of an RP-HPLC method for the simultaneous estimation of Lamivudine and Zidovudine in tablet dosage forms. The method utilizes a C18 column with a mobile phase of ammonium acetate buffer pH 4.0, acetonitrile and THF in a 60:30:10 ratio at a flow rate of 1 mL/min. Lamivudine and Zidovudine were well separated with retention times of 3.793 minutes and 2.547 minutes, respectively. The method was validated per ICH guidelines and demonstrated to be linear, precise, accurate, specific and robust for the simultaneous analysis of these two drugs in tablets.
Stability indicating RP-HPLC method for estimation of dapagliflozin in bulk a...SriramNagarajan19
A simple, specific, accurate, precise and stability-indicating reverse phase high performance liquid chromatography (RP-HPLC) method is developed for estimation of Dapagliflozin (DGF) in bulk and Pharmaceutical dosage form. The method employed, Hypersil BDS C18 250 mm x 4.6 mm, 5 mm column in isocratic mode with mobile phase of 0.1% Ortho phosphoric acid buffer and acetonitrile 50:50% v/v. The flow rate was 1.0 mL min-1 and effluent was monitored at 245 nm using PDA detector. The injection volume was 10 µl and the total runtime was set as 5min. The retention time for DGF was found to be 2.226min.The method was validated in terms of Linearity, accuracy, precision, limit of detection (LOD), limit of quantification (LOQ) etc. in accordance with ICH guidelines. Linear regression analysis data for the calibration plot showed that there was a good linear relationship between response and concentration in the range of 25 - 150 µg/ml respectively. The LOD and LOQ values for HPLC method were found to be 0.04 and 0.121 µg/ml respectively. No chromatographic interference from the tablet excipients was found. The proposed method was successfully used for estimation of Dapagliflozin (DGF) in Bulk and Pharmaceutical dosage form.
A novel validated RP-HPLC method was developed for the estimation of Liraglutide in bulk and parenteral dosage forms. The method utilized a C18 column, mobile phase of methanol and phosphate buffer with UV detection at 246 nm. The method was validated per ICH guidelines and found to be accurate, precise, specific and linear over a concentration range of 20-80 μg/ml. The method was successfully applied to a liraglutide injection sample with 99.84% assay results. In summary, a novel HPLC method was developed and validated for the analysis of liraglutide in bulk and parenteral dosage forms.
Application of Validated High-performance Liquid Chromatography Method for De...BRNSS Publication Hub
A novel and simple reversed-phase liquid chromatographic method has been established for the determination of saxagliptin and metformin HCl Saxagliptin and metformin HCl is used to control Type 2 diabetes. The proposed work was performed on Young Lin (S.K) isocratic System UV Detector. Saxagliptin and metformin HCl is used to control Type 2 diabetes. The proposed work was performed on Young Lin (S.K) isocratic System UV Detector C18 column (150 mm × 4.6 mm). A mixture of potassium phosphate, mobile phase in this method with flow rate of 0.7 mL/min (UV detection at 203 nm) and the method was validated as per the ICH guidelines. Forced degradation studies were performed by exposing the drug saxagliptin and metformin HCl to acidic, alkaline, oxidation, and thermal stress degradations. The proposed reversed-phase-high-performance liquid chromatography method was found to be robust and specific, and this method is suitable for the assay of pharmaceutical dosage forms as well as kinetic studies.
RP-HPLC Assay Method Validation for the estimation of new Anti-retroviral dru...SriramNagarajan15
A reverse phase HPLC method was developed and validated for the quantification of lamivudine in bulk and tablet formulations. The method used an ODS column with a mobile phase of acetate buffer and acetonitrile (50:50) at a flow rate of 1.5 mL/min. Lamivudine had a retention time of 1.85 minutes when detected at 272 nm. The method was linear over a concentration range of 10-50 μg/mL with a correlation coefficient of 0.999. Accuracy and precision studies demonstrated recoveries between 98-102% and %RSD below 2%, respectively. The method was found to be robust, specific, and suitable for the routine analysis of lamivudine in
The document describes the development and validation of a reverse phase HPLC method for the estimation of the anti-retroviral drug lamivudine in bulk and tablet formulations. An ODS column with a mobile phase of acetate buffer and acetonitrile was used to achieve separation of lamivudine. The method was validated as per ICH guidelines and was found to be linear, precise, accurate and robust. The developed method can be used for the routine analysis of lamivudine in pharmaceutical dosage forms.
RP-HPLC Assay Method Validation for the estimation of new Anti-retroviral dru...SriramNagarajan15
A Reverse phase HPLC method was developed for estimation of the Lamivudine in bulk and tablet formulation by using ODS column (250mm×4.6mm, 5µm) and Acetate buffer: acetonitrile (50:50) as mobile phase, at a flow rate of 1.5ml/min. The detection was carried at the 272nm the retention time of the Lamivudine is 1.850. The developed method was validated for the various parameters as per the ICH guidelines like accuracy precision, linearity and range, Robustnes. Linearity was obtained in the concentration range of 10µg/ml to 50µg/ml with correlation coefficient of 0.999. The accuracy of the method was assessed by recovery studies at three different concentration levels. The percentage recovery of Lamivudine was found to be in the range of 98% -102%. The method was found to be precise as indicated by the repeatability, inter-day, intra-day analysis, showing %RSD less than 2. Key words: RP-HPLC, Lamivudine, Pharmaceutical dosage form.
The document describes the development and validation of a reverse phase HPLC method for the estimation of the anti-retroviral drug lamivudine in bulk and tablet formulations. An ODS column with a mobile phase of acetate buffer and acetonitrile was used to achieve separation of lamivudine. The method was validated as per ICH guidelines and was found to be linear, precise, accurate and robust. The developed method can be used for the routine analysis of lamivudine in pharmaceutical dosage forms.
Analytical Method Development and Validation of Metformin Hydrochloride by us...ijtsrd
A simple and reproducible method was developed for Metformin MET by Reverse Phase High Performance Liquid Chromatography RP HPLC . Metformin was separated on C18 column 4.6x250mm, particle size 5µm , using combination of phosphate buffer with pH of 3.0 and Methanol at the UV detection of 238nm. Isocratic elution of phosphate buffer with pH of 3.0 and Methanol was used as a mobile phase with various ratios and flow rates, eventually 30 70 v v phosphate buffer with pH of 3.0 and Methanol was being set with the flow rate of 1mL min. The statistical validation parameters such as linearity, accuracy, precision, inter day and intra day variation were checked, assay studies of Metformin were within 98 to 102 indicating that the proposed method can be adoptable for quality control analysis of Metformin. Mr. Nilesh Nikam | Dr. Avish Maru | Dr. Anil Jadhav | Dr. Prashant Malpure ""Analytical Method Development and Validation of Metformin Hydrochloride by using RP-HPLC with ICH Guidelines"" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-3 , April 2019, URL: https://www.ijtsrd.com/papers/ijtsrd22812.pdf
Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/22812/analytical-method-development-and-validation-of-metformin-hydrochloride-by-using-rp-hplc-with-ich-guidelines/mr-nilesh-nikam
Stability studies of simvastatin and fenofibrate and degradants identificatio...Mehar Raghavendra YEGGINA
1. A stability indicating RP-HPLC method was developed for the simultaneous quantification of simvastatin and fenofibrate.
2. The method used a C18 column with a mobile phase of acetonitrile and ammonium acetate buffer at pH 4.3 to achieve separation of the drugs from their degradation products.
3. The drugs were subjected to stress conditions and the degraded products were identified using LC-MS to prove the stability indicating capability of the developed method.
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).
Similar to Development and validation of RP-HPLC method for simultaneous estimation of gliclazide and metformin in pure and tablet dosage form (20)
Patient compliance: Challenges in management of cardiac diseases in Kuala Lum...pharmaindexing
Background
The objective of this study was to investigate the degree of compliance among cardiac patients who attend the health facilities in Kuala Lumpur and Perak, Malaysia. The reasons for non-compliance and recommendations from healthcare professionals were also evaluated.
Method
A cross-sectional study of 400 patients and 100 healthcare professionals was carried out. This study utilizes variables on external factors and internal factors as the measurement tools. The questionnaire which consists of Morisky self-reported medication adherence questions was administered to patients and causes for non-compliance sought. Questionnaire for healthcare professionals was used to determine strategies that can improve compliance rate.
Results
The study revealed a 15.8% of high adherence rate, 54.3% of moderate adherence rate and 30% of poor adherence to cardiovascular disease medications. The chi-square tests showed the strong association between dependent and independent variables. The model chosen for testing the patient compliance through external and internal factors gives an R2 value of 85.0% with an adjusted R2 of 84.7%. The F value (317.187) was also significant (p=0.000) which means that the variables have better fit in the multivariate model. The major reasons determined for non-adherence were attitudes and beliefs, lifestyle, side effects and cost of medications. The study recommends that pharmacists and dispensing technicians should be adequately qualified to provide proper counselling to cardiac patients on their medicines and disease conditions.
Conclusion
The result of this study is of value to health care providers. Compliance to cardiovascular medications will avoid treatment failures encountered in therapy.
Overview on Recurrence Pregnancy Loss etiology and risk factorspharmaindexing
Recurrent pregnancy loss (RPL) can be defined as more than two to three consecutive miscarriages before 20 weeks’ gestation; it affects approximately 1% to 2% of women. RPL is a multifactorial disease. It is very important to study the etiology and risk factors of RPL to find the best diagnostic tests and suitable therapeutic intervention. This article will discuss the current understanding etiologies and risk factors of RPL.
Novel treatments for asthma: Corticosteroids and other anti-inflammatory agents.pharmaindexing
Asthma management is a challenge due to the prevalence of disease in the world. Based on the immunological and inflammatory mechanisms of asthma, corticosteroids and anti-inflammatory participate greatly in the treatment plan. Due to different reasons, there is still an unmet need to develop new agents in this field. A lot of compounds with anti-inflammatory effect are investigated in both pre-clinical and clinical studies.
A review on liver disorders and screening models of hepatoprotective agentspharmaindexing
The liver is a vital organ present in vertebrates and some other animals. It has a wide range of functions, including detoxification, protein synthesis, and production of bio chemicals necessary for digestion. The liver is necessary for survival; there is currently no way to compensate for the absence of liver function long term, although liver dialysis can be used short term.
Carbamazepine induced Steven Johnson syndrome: A case reportpharmaindexing
Drugs are the most common cause that induces Steven Johnson syndrome (SJS) and includes antiepileptic drugs, antiretroviral drugs, anti-tuberculosis drugs, Sulphonamides, fluoroquinolones, penicillins, non-Steroidal anti-inflammatory drugs, Multivitamins. The genetic markers are also the cause for carbamazepine induced Steven Johnson Syndrome. In our study, the antiepileptic drug (Carbamazepine) is the cause for Steven Johnson Syndrome. A female patient aged 25 years came to the hospital with the complaints of bubbling over the skin and all over the body with papillary vesicles associated with pain and irritation, fever, myalgia, and nausea. The patient is known case of Phenytoin induced Steven Johnson Syndrome. In this case the patient developed the Steven Johnson Syndrome approximately after one month after starting the carbamazepine.By the withdrawal of the drug, the condition of the patient was improved.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Pneumonia and respiratory failure from swine origin influenza H1n1pharmaindexing
Swine influenza (swine flu) became alarming health concern when World Health Organization declared as “public health emergency of international concern” on April 25, 2009. After documentation of human-to-human transmission of the virus in at least three countries of two WHO regions, the WHO raised the pandemic level to 6.1 During the 1918, flu pandemic infected one-third of the world's population (an estimated 500 million people) and caused approximately 50 million deaths.2 In 1976, an outbreak of swine influenza occurred in New Jersey, USA, which involved more than 200 cases, some of them severe, resulting in one death.3 In 1988, another fatality was reported as a complication of swine influenza.
A descriptive study on newborn care among postnatal mothers in selected mater...pharmaindexing
The newborn health challenge faced by India is more formidable than that experienced by any other country in the world. The newborn health is inevitably affected by the traditional care practices of the mothers causing high infant morbidity and mortality.The aim of the study were determine the knowledge, attitude and practice of postnatal mothers regarding new born care and find out the association between knowledge, attitude and practice of postnatal mothers regarding new born care and to determine the association between these as well as with the selected demographic variables. A descriptive study was conducted to assess the knowledge, attitude and practice of postnatal mothers regarding new born care in selected maternity centres in Madurai. Survey approach was employed to select sample and it consisted of 100 postnatal mothers. Data was collected using structured interview schedule. Findings of the study showed that 65% of postnatal mothers had moderate knowledge; 61% had favourable attitude and 57% of them had high practice of new born care. There was a significant association between knowledge and attitude (r=+0.567), knowledge and practice (r=+0.388), attitude and practice (r=+0.321) .There was a significant association between knowledge and education, monthly family income and obstetrical score at p<0.05. Findings of the study indicated the need to conduct frequent assessment of knowledge, attitude and practice of postnatal mothers regarding new born care. Awareness and attitude of the mothers towards new born care still has lots of lacunae especially in those who belong to the lower socio economic statusand poorly educated postnatal mothers. So it is imperative to provide comprehensive training in the field of new born care for mothers during pregnancy
Late 19th century was evident of intelligent biomaterial; which has changed researcher’s perspective towards science and technology. This intelligent biomaterial are envisioned to have huge impact on Healthcare from sequential signalling of biomedical molecule, mimicking natural gene, an effective drug carrier, to high resolution diagnostic tool.From drug discovery aspect many of NCE fail to reach therapeutic potential due to PK/ PD profile. Nanotechnology has changed the face of drug discovery form chemical evaluation to structure of proteins in signalling pathways and development of chemical antibody. Nanotechnology from lab to market approval is long process due to regulatory evaluation. Though it seems to be bright future market it has to go through a long process from being innovation to complete market product. This makes whole process expensive making investor reluctant to invest in big projects.Western world is aware of dramatic potential of nano-projects; which has its limitation in financial investments; with major challenge of transforming nano science to commercial pharmaceutical product.
The Flaws in health practice in post-operative management of a patient in ter...pharmaindexing
This case study summarizes the treatment of a 4-year old child with congenital urinary tract obstruction who presented with constipation, fever, and cough. Laboratory tests found low electrolyte levels, high blood acids, and kidney damage. The child's treatment included surgery, dialysis to correct electrolyte imbalances, and antibiotics for chest infection. However, the case study notes discrepancies in the post-operative treatment, including questionable antibiotic selection and prescribing of calcium channel blockers not recommended for children. The study concludes there is a need for clinical pharmacists on the healthcare team to improve rational medication use.
Corticosteroid induced disorders – An overviewpharmaindexing
Glucocorticoids are important in the treatment of many inflammatory, allergic, immunologic, and malignant disorders, and the toxicity of glucocorticoids is one of the commonest causes of iatrogenic illness associated with chronic inflammatory disease.Glucocorticoid-induced muscle atrophy is characterized by fast-twitch or type II muscle fiber atrophy. Corticosteroid (CS) therapy is widely used in the treatment of rheumatic diseases.Osteoporosis remains one of its major complications.Steroid induced glaucoma is a form of open angle glaucoma occurring as an adverse effect of corticosteroid therapy. Glucocorticoids induce hepatic and extrahepatic insulin resistance.Glucocorticoid treatment impairs both glucose transport in fat and muscle cells. Corticosteroid-induced psychosis represents a spectrum of psychological changes that can occur at any time during treatment. Cushing’s syndrome describes the signs and symptoms associated with prolonged exposure to inappropriately high levels of the hormone cortisol. Physicians must be aware of these adverse effects and be equipped to manage them.
Anti-inflammatory activity of pupalia lappacea L. Jusspharmaindexing
Pupalia lappacea (L) Juss is an erect shrub used in folklore medicine to treat bone fractures and in inflammatory conditions. Methanolic extract of aerial parts shown is claimed in traditional medicine that the leaves of the plant are used in the treatment of inflammation. In the present study, the methanolic extract of Pupalia lappacea was screened for its anti-inflammatory activity using carageenan induced rat paw edema egg white induced paw oedema models. The methanolic extract at the dose of 200 mg/kg p.o exhibited significant anti-inflammatory activity in carrageenan induced paw edema model (p<0.01). In egg white induced model, methanolic extract at the dose of 200 mg/kg inhibited paw oedema significantly (p<0.01) indicating that both test samples inhibit the increase in number of fibroblasts and synthesis of collagen and mucopolysaccharides during prostaglandin formation during the inflammation. These experimental results have established a pharmacological evidence for the folklore claim of the drug to be used as an anti inflammatory agent. HPTLC analysis of the extract shows the presence of gallic acid 1.24mg/ml, ferulic acid 2.00mg/ml, chlorogenic acid 46.25mg/ml and rutin 7.02mg/ml of the extract which were responsible for the claimed anti-inflammatory action in the animal models studied.
Lucinactant: A new solution in treating neonatal respiratory distress syndrom...pharmaindexing
This document summarizes research on Lucinactant, a novel synthetic surfactant approved by the FDA in 2012 for treatment of neonatal respiratory distress syndrome (RDS). It contains a peptide called sinapultide that mimics the function of human surfactant protein B. Studies found Lucinactant was as effective as or more effective than previous animal-derived surfactants in reducing mortality from RDS, but its pharmacokinetics are not fully understood. The document reviews clinical trials and mechanisms of Lucinactant and discusses its efficacy, safety profile, and potential cost benefits compared to other surfactants.
Bioactivity screening of Soil bacteria against human pathogenspharmaindexing
This study aimed to isolate soil bacteria with potential bioactive properties against human pathogens. 36 bacterial strains were isolated from 3 soil samples and screened against common pathogens. 14 isolates showed antibacterial activity, including against Staphylococcus aureus, Streptococcus faecalis, E. coli, Klebsiella aerogenes, Proteus vulgaris, Pseudomonas aureginosa and Salmonella typhi. The 3 most active bacterial isolates were selected for further production and isolation of their bioactive metabolites. Testing found the metabolites had prominent antibacterial effects against the clinical pathogens studied, indicating their potential as a source of new antimicrobials given the rise in drug resistance.
A study on sigmoid Volvulus presentation and managementpharmaindexing
A study on sigmoid volvulus presentation and management was a 2yr retrospective study done at RMMCH.The diagnosis of sigmoid volvulus was made from a history of large bowel obstruction (constipation, abdominal distension, and abdominal pain), which were often recurrent and plain abdominal radiographs.The morbidity associated isSuperficial wound infection occurred in four patients. All the infected wounds eventually healed with conservative measures. Clinical anastomotic dehiscence was noted in 1 patient for which during relaparotomy proximal colostomy and mucous fistula was done. The mortality associated is shown is there were 9 deaths of which 7 were due to sepsis and 2 were due to comorbid illness. Two out of eight patients for whom a colopexy was done had a recurrent attack of sigmoid volvulus. The duration of hospital stay ranged between 10 and 21 days. Use of sigmoidoscopic detorsion for viable colon should be encouraged. Sigmoidopexy, which is associated with a recurrence rate of 20% in our series of patients, should be used selectively.Hartmann’s procedure is a safe option in sigmoid volvulus with gangrenous bowel. Primary anastomosis in emergency situation can be carried out with morbidity and mortality in patients with viable colon
Evaluation of Preliminary phytochemical on various some medicinal plantspharmaindexing
The present study was carried out to evaluate the physical status and percentage yield of methanolic extract and its fractions of whole plant of Leucas cephalotes, leaves of Hiptage benghalensis and leaves of Kydia calycina were recorded for future references and Preliminary phytochemical screening of MLC, MHB and MKC revealed the presence of carbohydrates, glycosides, saponins, flavonoids, steroidal and phenolic compounds. MLC revealed the presence of all the above mentioned phytoconstituents except saponins and also MKC steroidal compounds. The fractions of MLC, MHB and MKC revealed the presence of glycosides, phenolic compounds, steroids and flavonoids.
Comparision of in vitro antibacterial activity of cefoperazone and levofloxac...pharmaindexing
This study compared the in vitro antibacterial activity of cefoperazone and levofloxacin against various clinical isolates. 120 bacterial isolates from patient samples were tested for susceptibility to cefoperazone and levofloxacin using disc diffusion. Results showed levofloxacin had lower resistance than cefoperazone for E. coli and P. aeruginosa, while cefoperazone was more effective against S. aureus. However, resistance to both antibiotics was gradually increasing, highlighting the need for regular surveillance of antibiotic susceptibility.
Concept of srotas from ayurvedic perspective with special reference to neurologypharmaindexing
Ayurveda is a life science. The researchers of ayurveda could rule out the presence of srotas (channels) spreading throughout the human body. These srotas (channels) are governed by vayu which is using all the srotas (channels) of the body to carry out the functional and physiological activities of the human body without which the human society will not exist. Several synonymous words have been described by the ayurvedicacharyas for srotas. Some are micro and some are macro in structures and they adopt the same colour of the particular dhatus of the body to which it belongs. The aim of the study is to justify that srotas are nothing but innurmerable channels or pathways of the nervous system governed by electric current without which no functional and physiological activities of the human body will develope.
Health promotion survey in overweight and obese students of universities in n...pharmaindexing
Introduction
Overweight and obesity is one of the major health problems in the UK and worldwide. Approximately two-thirds of the population in the UK is either overweight or obese. Overweight and obesity is an important issue that causes distress to most women. Health promotion is the best method to educate overweight and obese women. It is defined as the process enabling people to increase control over and to improve their health by Ottawa Charter for Health Promotion. It is aimed to enhance the well-being of the individuals and their positive attitudes towards prevention of various diseases. In order to make any improvement to the health promotion for overweight and obesity, the risk factors and the opinions from the public should first be identified and addressed.
Methods
Cross-sectional survey design was selected with a questionnaire that consisted of 20 open and close ended questions. A sample size of 196 was determined. The data thus gathered was analyzed using SPSS V20 (Statistical Package for Social Science version 20). Descriptive statistics (fx) and (SD) were used and Chi-square X2 test for association was employed.
Results
Out of the total 196 responses, only (40%) of the students had normal weight (SD 1.1), (25%) students had a good understanding of health promotion (SD 1.6), half (50%) appeared concerned about their weight (SD 0.5), (60%) had an obese family member (0.5). The BMI of students was associated with the presence of an obese member in their family and their weight as a concern for them. (P-value <0.05).
Conclusion
The health promotion service is beneficial as it was found to have raised concerns in the mind of the students regarding over weight and obesity. However it was observed that the understanding of health promotion service was different among students and this is the root of the problem.
Histololgy of Female Reproductive System.pptxAyeshaZaid1
Dive into an in-depth exploration of the histological structure of female reproductive system with this comprehensive lecture. Presented by Dr. Ayesha Irfan, Assistant Professor of Anatomy, this presentation covers the Gross anatomy and functional histology of the female reproductive organs. Ideal for students, educators, and anyone interested in medical science, this lecture provides clear explanations, detailed diagrams, and valuable insights into female reproductive system. Enhance your knowledge and understanding of this essential aspect of human biology.
NVBDCP.pptx Nation vector borne disease control programSapna Thakur
NVBDCP was launched in 2003-2004 . Vector-Borne Disease: Disease that results from an infection transmitted to humans and other animals by blood-feeding arthropods, such as mosquitoes, ticks, and fleas. Examples of vector-borne diseases include Dengue fever, West Nile Virus, Lyme disease, and malaria.
Local Advanced Lung Cancer: Artificial Intelligence, Synergetics, Complex Sys...Oleg Kshivets
Overall life span (LS) was 1671.7±1721.6 days and cumulative 5YS reached 62.4%, 10 years – 50.4%, 20 years – 44.6%. 94 LCP lived more than 5 years without cancer (LS=2958.6±1723.6 days), 22 – more than 10 years (LS=5571±1841.8 days). 67 LCP died because of LC (LS=471.9±344 days). AT significantly improved 5YS (68% vs. 53.7%) (P=0.028 by log-rank test). Cox modeling displayed that 5YS of LCP significantly depended on: N0-N12, T3-4, blood cell circuit, cell ratio factors (ratio between cancer cells-CC and blood cells subpopulations), LC cell dynamics, recalcification time, heparin tolerance, prothrombin index, protein, AT, procedure type (P=0.000-0.031). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and N0-12 (rank=1), thrombocytes/CC (rank=2), segmented neutrophils/CC (3), eosinophils/CC (4), erythrocytes/CC (5), healthy cells/CC (6), lymphocytes/CC (7), stick neutrophils/CC (8), leucocytes/CC (9), monocytes/CC (10). Correct prediction of 5YS was 100% by neural networks computing (error=0.000; area under ROC curve=1.0).
Adhd Medication Shortage Uk - trinexpharmacy.comreignlana06
The UK is currently facing a Adhd Medication Shortage Uk, which has left many patients and their families grappling with uncertainty and frustration. ADHD, or Attention Deficit Hyperactivity Disorder, is a chronic condition that requires consistent medication to manage effectively. This shortage has highlighted the critical role these medications play in the daily lives of those affected by ADHD. Contact : +1 (747) 209 – 3649 E-mail : sales@trinexpharmacy.com
Recomendações da OMS sobre cuidados maternos e neonatais para uma experiência pós-natal positiva.
Em consonância com os ODS – Objetivos do Desenvolvimento Sustentável e a Estratégia Global para a Saúde das Mulheres, Crianças e Adolescentes, e aplicando uma abordagem baseada nos direitos humanos, os esforços de cuidados pós-natais devem expandir-se para além da cobertura e da simples sobrevivência, de modo a incluir cuidados de qualidade.
Estas diretrizes visam melhorar a qualidade dos cuidados pós-natais essenciais e de rotina prestados às mulheres e aos recém-nascidos, com o objetivo final de melhorar a saúde e o bem-estar materno e neonatal.
Uma “experiência pós-natal positiva” é um resultado importante para todas as mulheres que dão à luz e para os seus recém-nascidos, estabelecendo as bases para a melhoria da saúde e do bem-estar a curto e longo prazo. Uma experiência pós-natal positiva é definida como aquela em que as mulheres, pessoas que gestam, os recém-nascidos, os casais, os pais, os cuidadores e as famílias recebem informação consistente, garantia e apoio de profissionais de saúde motivados; e onde um sistema de saúde flexível e com recursos reconheça as necessidades das mulheres e dos bebês e respeite o seu contexto cultural.
Estas diretrizes consolidadas apresentam algumas recomendações novas e já bem fundamentadas sobre cuidados pós-natais de rotina para mulheres e neonatos que recebem cuidados no pós-parto em unidades de saúde ou na comunidade, independentemente dos recursos disponíveis.
É fornecido um conjunto abrangente de recomendações para cuidados durante o período puerperal, com ênfase nos cuidados essenciais que todas as mulheres e recém-nascidos devem receber, e com a devida atenção à qualidade dos cuidados; isto é, a entrega e a experiência do cuidado recebido. Estas diretrizes atualizam e ampliam as recomendações da OMS de 2014 sobre cuidados pós-natais da mãe e do recém-nascido e complementam as atuais diretrizes da OMS sobre a gestão de complicações pós-natais.
O estabelecimento da amamentação e o manejo das principais intercorrências é contemplada.
Recomendamos muito.
Vamos discutir essas recomendações no nosso curso de pós-graduação em Aleitamento no Instituto Ciclos.
Esta publicação só está disponível em inglês até o momento.
Prof. Marcus Renato de Carvalho
www.agostodourado.com
ABDOMINAL TRAUMA in pediatrics part one.drhasanrajab
Abdominal trauma in pediatrics refers to injuries or damage to the abdominal organs in children. It can occur due to various causes such as falls, motor vehicle accidents, sports-related injuries, and physical abuse. Children are more vulnerable to abdominal trauma due to their unique anatomical and physiological characteristics. Signs and symptoms include abdominal pain, tenderness, distension, vomiting, and signs of shock. Diagnosis involves physical examination, imaging studies, and laboratory tests. Management depends on the severity and may involve conservative treatment or surgical intervention. Prevention is crucial in reducing the incidence of abdominal trauma in children.
Rasamanikya is a excellent preparation in the field of Rasashastra, it is used in various Kushtha Roga, Shwasa, Vicharchika, Bhagandara, Vatarakta, and Phiranga Roga. In this article Preparation& Comparative analytical profile for both Formulationon i.e Rasamanikya prepared by Kushmanda swarasa & Churnodhaka Shodita Haratala. The study aims to provide insights into the comparative efficacy and analytical aspects of these formulations for enhanced therapeutic outcomes.
Promoting Wellbeing - Applied Social Psychology - Psychology SuperNotesPsychoTech Services
A proprietary approach developed by bringing together the best of learning theories from Psychology, design principles from the world of visualization, and pedagogical methods from over a decade of training experience, that enables you to: Learn better, faster!
Development and validation of RP-HPLC method for simultaneous estimation of gliclazide and metformin in pure and tablet dosage form
1. Nirupama.D, et al / Int. J. Pharm. & Analytical Res. Vol-3(4) 2014 [326-333]
www.ijpar.com
~ 326~
IJPAR |Vol.3 | Issue 4 | Oct-Dec-2014
Journal Home page: www.ijpar.com
Research article Open Access
Development and validation of RP-HPLC method for simultaneous
estimation of gliclazide and metformin in pure and tablet dosage form
Nirupama.D*, P.Venkateswara Rao, B.Thangabalan, S.Manohar Babu.
Department of Pharmaceutical Analysis, Sims College of Pharmacy, Vijayawada road, Guntur, India.
* Corresponding author: Nirupama.D
E-mail id: dnreddy.niru@gmail.com
ABSTRACT
A simple, precise, accurate and rapid reverse phase high performance liquid chromatographic method was developed for the
simultaneous estimation of Gliclazide(GLZ) and Metformin(MET) in pure and tablet dosage form. The method was carried
on Phenomex (kromosil-250 mm × 4.6 mm, 5 μm) column with mobile phase comprising of phosphate buffer and methanol
in the ratio 60:40 v/v. Flow rate was adjusted to 1.0ml/min and effluents were monitored at 230 nm. The retention time
obtained for Gliclazide and Metformin was 5.0 and 3.2 mint respectively. The calibration curves were linear in the
concentration range of 10-100μg/ml for Gliclazide and Metformin 62.5-625μg/ml for. The developed method was validated
in accordance to ICH guidelines.
Keywords: Gliclazide, Metformin, RP-HPLC and Simultaneous estimation.
INTRODUCTION
Gliclazideis chemically 3-[(3aR, 6aS)-
octahydrocyclopenta[c]pyrrol-2-yl]-1-(4-methyl-
benzenesulfonyl) urea. It is an oral hypoglycemic agent
used in treatment of diabetes mellitus type II. analytical
methods including radioimmunoassay, gas
chromatography, HPLC, Evaporative Light Scattering
Detection, Charged Aerosol Detection and
simultaneous estimation of gliclazide and metformin
hydrochloride in combined dosage forms have been
reported for determination of gliclazide.
Figure 1: chemical structure of gliclazide.
Metformin2
Hydrochlorideis chemically N, N-d
imethylimido di carbonimidicdiamide hydrochloride.
Metformin activates AMP-activated protein kinase
(AMPK), a liver enzyme that plays an important role in
insulin signaling, whole body energy balance, and the
metabolism of glucose and fats; activation of AMPK is
ISSN: 2320-2831
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required for metformin's inhibitory effect on the
production of glucose by liver cells. AMPK probably
also plays a role, as metformin administration increases
AMPK activity in skeletal muscle.
Figure 2: chemical structure of metformin
The objective of this study was to develop reverse
phase high performance liquid chromatography method
for the simultaneous estimation of gliclazide3
and
metformin in pure and pharmaceutical dosage form
without any derivatization4
and having the short
retention time. The method was found to be linear,
precise, accurate, sensitive, specific, and robust, and
therefore suitable for routine analysis.
MATERIALS AND METHOD
HPLC Instrumentation and chromatographic
conditions
The analytical separations were carried out on a waters
2487 HPLC system with Photo Diode Array detector.
The output of signal was monitored and integrated
using LC-solutions 2000 software. The analytical
column was phenomex (kromosil-250mm×
4.6mm,5μm).Mobile phase consisted phosphate
buffer(pH-6.5) and methanol in the ratio of 60:40.
Mobile phase was mixed, filtered through 0.45μ
membrane filter and degassed under ultrasonication.
The mobile phase was used as diluent. The flow rate
was 1.0ml/min and runtime was 7minute. The column
was maintained at ambient temperature. UV detection
was measured at 230nm and the volume of sample
injected was 10μl.
Preparation of mobile phase
Accurately weighed portion of 2.722g of potassium
dihydrogen orthophosphate was dissolved in 200 ml of
HPLC water. Separately 700mg of di-sodium hydrogen
orthophosphate was weighed and dissolved in 20ml of
HPLC water, the pH adjusted to 6.5 using disodium
hydrogen ortho phosphate, and then the solution was
filtered through a 0.22µm filter membrane and stored
in closed container.
Preparation of standard stock solution
Accurately weighed 62.5mg of Metformin and 10mg of
gliclazide was dissolved in diuent, in 100 ml
volumetric flask, that gave 625 µg/ml of Metformin
and 100 µg/ml of Gliclazide1
. From this into a series of
six 10ml volumetric flasks 1, 2, 4, 6, 8, 10ml were
transferred and diluted to 10ml with diluents, that gave
62.5, 125, 250, 375, 500 and 625 µg/ml of Metformin
and 10, 20, 40, 60, 80, and 100 µg/ml of Gliclazide.
Preparation of sample solution
20 tablets of combined formulation of Metformin and
Gliclazide were weighed, average weight was
calculated and triturated in a mortar with pestle from
that, powder equivalent to 62.5 mg of Metformin and
10 mg of Gliclazide was weighed and dissolved in
diluent and test concentration was prepared by further
dilution with same.
RESULTS AND DISCUSSION
HPLC method development and optimization
To optimize the chromatographic conditions, different
columns, mobile phases, flow rates etc., were tested.
Buffer and methanol in the ratio of 60:40 was preffered
as mobile phase. Because it resulted in a greater
response to gliclazide, metformin after several
preliminary investigatory runs compared with the
different mobile phase combinations. The effect of the
flow rate was studied in the range 0.9 to 1.1ml/min and
1.0ml/min was preffered to be effective. Under these
conditions, the analyte peak obtained was well-defined
and free from tailing. The retention time(RT) was
found to be 5.0 and 3.2min. The optimized
chromatographic parameters5
were listed in table 1.
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Fig 1: optimized chromatogram
Table 1: Optimized chromatographic parameters
VALIDATION OF THE METHOD
When method development and optimizations are
complete, it is necessary to accomplish method
validation6
. the validation studies include linear range
(Correlation coefficient), method precision (RSD,%),
method accuracy (%Recovery and RSD%), sensitivity
studies (LOD & LOQ), and robustness.
System suitability studies
System-suitability tests are an integral part of method
development and are used to ensure adequate
performance of the chromatographic system. Retention
time (RT), tailing factor(T), and peak asymmetry (AS),
resolution (RS) were evaluated. The system suitability
test was performed before analysis of sample. The
system suitability method acceptance criteria set in
each validation run were: capacity factor>2.0; tailing
factor <2.0 and theoretical plates>2000. In all cases,
the relative standard deviation(R.S.D) for the analytic
peak area for two consecutive injections was <2.0%.
system suitability parameters were shown in table 2.
Table 2: system suitability parameters
parameters gliclazide metformin
Retention time 5.0 3.2
S.NO Optimized Chromatographic parameters
1 Mobile Phase Buffer:Methanol(60:40 v/v)
2 Pump Mode Isocratic
4 Diluents Mobile phase
5 Column Phenomex C18 (150mm×4.6mm×5µ)
6 Column Temperature Ambient
7 Wavelength 230 nm
8 Injection Volume 10 µl
9 Flow Rate 1 ml/min
10 Run Time 7min
11 Retention Time 5.0 min & 3.2 min
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Linearity
The linearity of the method was evaluated by preparing
six series of standard solutions of gliclazide and
metformin in the range of 10-100 µg/ml, 62.5-
625µg/ml in mobile phase and injecting the solution
into the HPLC system. Excellent correlation between
gliclazide, metformin peak area and concentration was
observed with (R2
)=0.999, (Figure.3). the regression
equation was found to be Y=4617.x + 11446 and
Y=793.3x + 13107 respectively. The statistical data are
presented in table 3. And the calibration curve was
shown in figure 3.
Table 3: linearity results for gliclazide and metformin
Gliclazide Metformin
S.No Conc(µg/ml) Peak Area Conc(µg/ml) Peak Area
1 10 154403 62.5 175033
2 20 206452 125 232162
3 40 305646 250 330190
4 60 397427 375 437433
5 80 482011 500 525305
6 100 572203 625 623402
Fig 2. Calibration curve for gliclazide
Fig 3. Calibration curve for metformin
y = 4617.3x + 114465
R² = 0.999
0
100000
200000
300000
400000
500000
600000
700000
0 50 100 150
y = 793.33x + 131076
R² = 0.9991
0
100000
200000
300000
400000
500000
600000
700000
0 200 400 600 800
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Precision
System precision(Repeatability)
To study precision, five replicate standard solutions of
gliclazide (40µg/ml), metformin(250µg/ml) were
prepared and analyzed using the proposed method. The
percent relative standard deviation7
(%RSD) for peak
responses was calculated. Results of system precision
studies were shown in table 4.
Table 4: system precision results for gliclazide and metformin
Method Precision (Reproducibility)
The intraday and inter-day precision of the proposed
method was determined by analyzing the
correspomding responses 6 times of the same day and
on different days for concentration of 10µg/ml of
gliclazide and 100µg/ml of metformin. The results was
reported in terms of relative standard deviation
(%RSD), results of method precision studies were
shown in table 5.
Table 5: Method precision results for gliclazide and metformin
Intermediate precision
The intermediate precision of the proposed method was
determined by performing the method by two analysts.
(Analyst 1 and Analyst 2) for concentration of sample
solutions of gliclazide (40µg/ml), metformin
(250µg/ml). The percent relative standard deviation
(%RSD) for peak responses was calculated. The results
for intermediate were shown in table 6.
S.No Gliclazide Metformin
Rt(min) Peak Area Rt(min) Peak Area
1 4.975 350236 3.234 315642
2 4.962 350654 3.233 315371
3 4.943 350693 3.231 315598
4 4.965 350398 3.239 315877
5 4.978 350451 3.221 315668
Mean 4.9646 350486.4 3.2316 315631.2
St.deviation 0.013795 188.7731 0.006618 180.7587
%RSD 0.277866 0.05386 0.204795 0.057269
S.No Gliclazide Metformin
Rt(min) Peak Area Rt(min) Peak Area
1 5.005 3503557 3.234 3152466
2 5.007 3505877 3.233 3151745
3 5.006 3503969 3.231 3158954
4 5.006 3508933 3.229 3158663
5 5.004 3501546 3.230 3155433
Mean 5.0056 3504776 3.2314 3155452
St.deviation 0.00114 2786.708 0.002074 3362.772
%RSD 0.022778 0.079512 0.064172 0.10657
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Table 6: results of intermediate precision for gliclazide, metformin.
Repeatability
(% RSD) (n=6)
Intermediate precision (% RSD) (n=6)
Day 1 Day 2
Analyst 1 Analyst 2 Analyst 1 Analyst 2
GLZ 0.0815 0.0398 0.0632 0.0808
MET 0.0777 0.0128 0.0521 0.0636
Accuracy
Accuracy of the method was confirmed by the standard
addition method, which was carried out by performing
recovery studies at different concentrations are
accordance with ICH guidelines, by replicate analisis
(n=3). The closeness of obtained value to the true
value indicates that the proposed method is accurate.
Recovery studies were shown in table 7.
Table 7: Results of recovery studies for gliclazide, metformin
Sample Spiked Amount (mg) Recovered
Amount (mg)
% Recovered % Average
Recovery
GLZ
20 19.76 99.54
99.9040 40.03 100.03
60 60.01 100.006
MET
125 125.02 100.7
100.06250 250.01 100.27
375 375.01 101.07
Robustness
The robustness study was performed to evaluate the
influence of small but deliberate variation in the
chromatographic condition, the robustness was checked
by changing parameters like flow rate of mobile phase
and detection wavelength.
Change the dection wavelength ± 2nm(228nm and
232nm)
Change in flow rate by ± 0.2ml/minute (1.1ml/min
and 0.9ml/min)
After each change, sample solution was injected and
%assay with system suitability parameters were
checked. Robustness values were given in table 8.
Table 8: results of robustness for gliclazide and metformin
Drug Parameters count Changes RT(min) USP Tailing USP Plate
GLZ Flow rate (ml/min) 0.9 6.1 1.2 7487
1.2 4.1 1.1 5954
MET Flow rate (ml/min) 0.9 3.9 1.2 5203
1.2 2.6 1.1 7487
Limit of Detection and Quantitation
Detection and quantitation limit were calculated by the
method based on the standard deviation and slope of
the calibration plot, using the formula.
Limit of Detection = 3.3×σ/S, Limit of
Quantitation=10×σ/S. Where, σ = the standard
deviation of the response and S = slope of the
calibration curve.
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Table 9: Results if LOD, LOQ for gliclazide, metformin
Name of drug LOD (µg/ml) LOQ (µg/ml)
GLZ 0.0750μg/ml 0.2273μg/ml
MET 0.6557μg/ml 1.9872μg/ml
Specificity
Specificity of an analytical method is its ability to
measure the analyte accurately and specifically in the
presence of component that may be expected to be
present in the sample matrix. Chromatograms of
standard and sample solutions were compared in order
to provide an indication of specificity of the method.
Assay
The proposed validated method was successfully
applied to determine gliclazide, metformin in their
pharmaceutical dosage form and the % assay results
were shown in table 10.
Table 10: Results of % assay by using RP-HPLC method
Sample Spiked Amount (mg) Recovered
Amount (mg)
% Recovered % Assay
GLZ
20 19.76 99.54
99.9040 40.03 100.03
60 60.01 100.006
MET
125 125.02 100.7
100.06250 250.01 100.27
375 375.01 101.07
CONCLUSION
A simple, rapid, accurate, and precise RP-HPLC
method for the analysis of gliclazide and metformin in
pure and in pharmaceutical dosage forms had been
developed and validated in accordance with ICH
guidelines. The RP-HPLC method developed is cost-
effective due to short retention time which enabled
analysis of gliclazide and metformin samples with a
small amount of mobile phase. From the%RSD values
of precision and recovery studies the method was found
to be precise and accurate. The low detection and
quantification limits achieved indicate the method is
very sensitie. The robustness data gathered during
method validation showed that the method is not
susceptible to small changes in chromatographic
conditions, the proposed RP-HPLC method developed
by the author is suitable for routine analysis ana quality
assessment of gliclazide, metformin in pharmaceutical
products.
Table 11: summary of validated parameters for proposed method
Parameters GLZ MET
Linearity (µg/ml)
10-100 62.5-625
Regression equation
4617.x + 11446 793.3x + 13107
Slope (m)
4617 793.3
Intercept (C)
11446 13107
Correlation coefficient (r2
)
0.999 0.999
Method precision (%RSD, n=5) 0.06 0.10
LOD (µg/ml)
0.0750μg/ml 0.2273μg/ml
LOQ (µg/ml)
0.6557 μg/ml 1.9872μg/ml
% Assay 99.89% 99.98%
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REFERENCES
[1] Bhagyashri V. Vadnere, Aarti M. Jain and Priyanka S. Jadhav, Prof. S. P. Patil, Dr. S. D. Barhate have developed
and validation for the simultaneous estimation of gliclazide metformin and in tablet dosage form by RP-
HPLC.Journal of Pharmacy Research 2012, 5(10), 5036-5038.
[2] http://en.wikipedia.org/wiki/Metformin.
[3] http://en.wikipedia.org/wiki/Gliclazide.
[4] Edigasasikirangoud, V.Krishna Reddy, Chandra K Sekharhave developed andvalidation for the simultaneous
estimation of metformin and gliclazide in tabletdosage form by RP-HPLC. International Journal of Pharmacy and
Biological Sciences,Volume 2, Issue 4, OCT-DEC-2012
[5] A.anusha, N.Prajwala. M.Sandhya, Dr.UmaMaheswara Rao have developed and validation for the simultaneous
estimation of metformin and gliclazide in tablet dosage form by RP-HPLC. International Journal of Pharmacy and
Pharmaceutical Sciences, Volume- 5, Suppl 4, 2013
[6] KanijFatema, Md.zakirRahman, TasnuvaHaque, Mohammad abulkalamazad, and Md.selimreza, Development and
validation of a simple method for simultaneous estimation of Metformin hydrochloride and gliclazide in tablets by
using RP-HPLC, Dhaka UnivJ.PharmSci , 2010, 9(2) : 83-89
[7] B.V.V.Ravikumar, A.K. Patnaik, Saroj Kumar Raul, NagireddyNeelakanta Rao Development and Validation of a
simple method for the Estimation of Gliclazide in bulk and Pharmaceutical Dosage Forms by RP-HPLC. Journal of
Applied Pharmaceutical Science Vol. 3 (04), pp. 059-062, April, 2013.