RP-HPLC Method Development and Validation for the Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Tablet Dosage FormIjpar 14 607 madhavi
This document describes the development and validation of two stability-indicating methods for the quantitative analysis of rosuvastatin (ROSU) in the presence of its degradation products: a high-performance liquid chromatography (HPLC) method and a high-performance thin layer chromatography (HPTLC) method. Both methods were found to be precise, accurate, specific and sensitive for the analysis of ROSU in raw materials and pharmaceutical formulations in the presence of degradation products. The methods were fully validated per ICH guidelines and successfully applied to analyze ROSU levels in commercial tablet formulations.
Development and Validation of a RP-HPLC methodUshaKhanal3
The document describes the process of developing and validating a reverse phase high performance liquid chromatography (RP-HPLC) method. It involves determining method goals and analysis requirements based on the sample properties, conducting research on existing methods, selecting an analysis technique, optimizing the separation conditions through a systematic approach, and validating the method. Key steps include choosing the detector and mobile phase, optimizing variables like column type, temperature, flow rate and solvent composition to improve resolution and separation time, and testing the method's accuracy, precision, specificity and robustness.
Analytical method development and validation of tapentadol hcl by rp hplcShweta Tiwari
This document summarizes the development and validation of an analytical method using reverse phase high performance liquid chromatography (RP-HPLC) to analyze tapentadol hydrochloride in tablet dosage forms. The method utilized a C18 column with a mobile phase of methanol and water, detected the analyte at 272 nm. Validation of the method showed good linearity, precision, accuracy, specificity. The developed and validated method can be used for quality control of tapentadol hydrochloride tablet formulations.
HPLC Method Development & Method Validation (mr.s)22suresh
This document describes the development and validation of an HPLC method for estimating drugs. It discusses the principles of HPLC, steps in method development including selecting the method, column, mobile phase and detector. Method validation parameters like accuracy, precision, specificity, linearity and robustness are also summarized. The document provides details on the optimization process and validation procedures to ensure the method is suitable for its intended use.
This document presents information on HPLC method development and validation. It begins with an introduction to analytical chemistry and chromatography. It then discusses the principles, types, and modes of HPLC, as well as factors to consider in method development such as column selection and mobile phase selection. The document concludes with a discussion of method validation parameters such as system suitability, specificity, linearity, precision, accuracy, limit of detection, limit of quantification, and robustness. References on the topic are also provided.
Analytical method development and validationANANT NAG
This document describes the development and validation of an analytical method for Azelnidipine using UV-Visible spectroscopy. The method development involved preparation of standard stock and working solutions, selection of the analytical wavelength of 257nm from UV scanning, and generation of a calibration curve. The method validation assessed parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, robustness, and assay of Azelnidipine tablets to prove that the method is suitable for use in pharmaceutical analysis. The results of the study confirmed that UV-Visible spectroscopy can accurately and reliably measure Azelnidipine concentrations in formulations.
This document describes the development and validation of two stability-indicating methods for the quantitative analysis of rosuvastatin (ROSU) in the presence of its degradation products: a high-performance liquid chromatography (HPLC) method and a high-performance thin layer chromatography (HPTLC) method. Both methods were found to be precise, accurate, specific and sensitive for the analysis of ROSU in raw materials and pharmaceutical formulations in the presence of degradation products. The methods were fully validated per ICH guidelines and successfully applied to analyze ROSU levels in commercial tablet formulations.
Development and Validation of a RP-HPLC methodUshaKhanal3
The document describes the process of developing and validating a reverse phase high performance liquid chromatography (RP-HPLC) method. It involves determining method goals and analysis requirements based on the sample properties, conducting research on existing methods, selecting an analysis technique, optimizing the separation conditions through a systematic approach, and validating the method. Key steps include choosing the detector and mobile phase, optimizing variables like column type, temperature, flow rate and solvent composition to improve resolution and separation time, and testing the method's accuracy, precision, specificity and robustness.
Analytical method development and validation of tapentadol hcl by rp hplcShweta Tiwari
This document summarizes the development and validation of an analytical method using reverse phase high performance liquid chromatography (RP-HPLC) to analyze tapentadol hydrochloride in tablet dosage forms. The method utilized a C18 column with a mobile phase of methanol and water, detected the analyte at 272 nm. Validation of the method showed good linearity, precision, accuracy, specificity. The developed and validated method can be used for quality control of tapentadol hydrochloride tablet formulations.
HPLC Method Development & Method Validation (mr.s)22suresh
This document describes the development and validation of an HPLC method for estimating drugs. It discusses the principles of HPLC, steps in method development including selecting the method, column, mobile phase and detector. Method validation parameters like accuracy, precision, specificity, linearity and robustness are also summarized. The document provides details on the optimization process and validation procedures to ensure the method is suitable for its intended use.
This document presents information on HPLC method development and validation. It begins with an introduction to analytical chemistry and chromatography. It then discusses the principles, types, and modes of HPLC, as well as factors to consider in method development such as column selection and mobile phase selection. The document concludes with a discussion of method validation parameters such as system suitability, specificity, linearity, precision, accuracy, limit of detection, limit of quantification, and robustness. References on the topic are also provided.
Analytical method development and validationANANT NAG
This document describes the development and validation of an analytical method for Azelnidipine using UV-Visible spectroscopy. The method development involved preparation of standard stock and working solutions, selection of the analytical wavelength of 257nm from UV scanning, and generation of a calibration curve. The method validation assessed parameters such as linearity, precision, accuracy, limit of detection, limit of quantification, robustness, and assay of Azelnidipine tablets to prove that the method is suitable for use in pharmaceutical analysis. The results of the study confirmed that UV-Visible spectroscopy can accurately and reliably measure Azelnidipine concentrations in formulations.
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of the drug Zidovudine. The method was developed using a C18 column with a mobile phase of acetonitrile and water at a pH of 4.8. The method was validated according to ICH guidelines and showed good linearity, precision, accuracy, specificity, robustness and recovery. The proposed RP-HPLC method can be used for the routine analysis of Zidovudine in pharmaceutical formulations.
Formulation and evaluation of FDT and HPLC method development of Amlodipine b...pooja deshmukh
formulation and evaluation of fast disintegrating tablet by using superdisintegrants and RP-HPLC method development of prepered tablet of Amlodipine besilate and Candesartan cilexetil
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.
Nilesh Dashrath Kamble presented a seminar on method development and validation in HPLC. The presentation discussed the steps involved in HPLC method development including column selection, mobile phase composition, pH range selection, and optimization of separation conditions. It also covered validation parameters such as accuracy, precision, specificity, limit of detection, and limit of quantification as per ICH guidelines. The presentation included an example method development for the simultaneous estimation of atorvastatin and telmisartan from a tablet formulation.
This document discusses analytical method development for pharmaceutical drug substances and products. It describes the importance of method development and outlines the key steps involved, including collecting sample information, selecting the chromatographic technique, stationary and mobile phases. It also discusses sources of impurities in drugs, control and qualification of impurities according to ICH guidelines, and pharmacopeial and ICH quality guidelines for impurity testing and thresholds.
This document presents the development and validation of an RP-HPLC method for the simultaneous estimation of a muscle relaxant drug and analgesic drug in pure form and pharmaceutical dosage forms. It discusses conducting a literature review on existing methods, determining the physicochemical properties of the drugs, optimizing the analytical method, and validating the developed method as per ICH guidelines. The expected outcomes are an accurate, precise, simple, cost-effective and fast method for simultaneously analyzing the two drugs.
The document describes a method development and validation project for the analysis of drugs using UV spectrophotometry and HPLC. It provides an introduction, objectives, literature review, and plan of work. The literature review summarizes 15 research papers on method development and validation using these techniques. The instruments available for the project are also listed. The conclusion states that the project aims to develop analytical methods for quality assessment of drug products to ensure therapeutic effectiveness.
This document describes the development and validation of an RP-HPLC method for the quantification of verapamil in drug substances and products. It involves selecting the optimal chromatographic conditions, such as the column, mobile phase, flow rate, and developing the method according to ICH guidelines. The method development steps include selecting the HPLC method and conditions, optimizing the selectivity and system parameters, and validating the method parameters like accuracy, precision, specificity, linearity and range. The goal is to develop a simple, accurate and precise RP-HPLC method for the analysis of verapamil that can be validated as per regulatory requirements.
This document describes the development and validation of a UV spectrophotometric method for the estimation of methocarbamol in bulk and pharmaceutical dosage forms. The method was developed using acetone and 0.1N sodium hydroxide solution as solvents, in which methocarbamol is soluble. The drug has maximum absorbance at 267 nm. The method was validated as per ICH guidelines and was found to be linear, precise, accurate and specific. The developed method can be used for the quantitative analysis of methocarbamol in bulk and pharmaceutical formulations.
This document describes a liquid chromatographic method for the simultaneous quantitative determination of candesartan cilexetil and hydrochlorothiazide in pharmaceutical dosage forms. A simple and sensitive RP-HPLC method was developed and validated. The method allows for the separation, identification and quantification of candesartan cilexetil and hydrochlorothiazide in tablet formulations using a C18 column with UV detection. The method was validated in terms of specificity, linearity, precision, accuracy and robustness.
This document discusses considerations for developing assay methods. It recommends starting with existing reference standard methods and literature. The method should separate the analyte peak from all impurities and degradants. Tools to reduce run time include shorter columns, larger particle sizes, and optimizing mobile phase composition. The same method can sometimes be used for assay and reference standards if linearity criteria are met. Extraction efficiency must be over 150% and placebo interference under 2%. Runtimes for in-process tests should be under 5 minutes. Sample quantity for content uniformity tests is 1-3 unit doses and for assays is 3-10 unit doses.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
RP-HPLC Method Development and Validation of Ketoconazole in Bulk and Pharmac...Sunil Vadithya
The document describes the development and validation of an RP-HPLC method for the estimation of Ketoconazole in pharmaceutical formulations. A Phenomenex Luna C18 column with a mobile phase of acetonitrile and phosphate buffer was used to separate Ketoconazole. The retention time of Ketoconazole was 4.768 minutes. The method was validated for accuracy, precision, linearity, robustness and specific parameters. The developed and validated method can be used for the routine analysis of Ketoconazole in formulations.
Method validation in HPLC of omeprazole enantiomerscoolprashant33
Nilesh Kamble presented a seminar on the development and validation of a method for the enantiomeric estimation of omeprazole enantiomers in enteric-coated formulations using high-performance liquid chromatography. Omeprazole exists as two enantiomers but the S-enantiomer is metabolized more slowly and at lower doses. The method was developed using a chiral column with normal phase chromatography. Validation showed the method was specific, stability-indicating, linear, accurate and suitable for quantifying the undesired enantiomer in formulations. The developed method can help ensure only the desired enantiomer is present in marketed formulations.
This document provides guidance on developing and optimizing a regulated bioanalytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS). It discusses important considerations for method development including choosing a detection technique, optimizing sample extraction and chromatography conditions, and validating the final method. The goal is to develop a selective, sensitive and reproducible method for quantifying biological samples in a regulated setting.
This document describes the development and validation of a reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of the drug Zidovudine. The method was developed using a C18 column with a mobile phase of acetonitrile and water at a pH of 4.8. The method was validated according to ICH guidelines and showed good linearity, precision, accuracy, specificity, robustness and recovery. The proposed RP-HPLC method can be used for the routine analysis of Zidovudine in pharmaceutical formulations.
Formulation and evaluation of FDT and HPLC method development of Amlodipine b...pooja deshmukh
formulation and evaluation of fast disintegrating tablet by using superdisintegrants and RP-HPLC method development of prepered tablet of Amlodipine besilate and Candesartan cilexetil
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.
Nilesh Dashrath Kamble presented a seminar on method development and validation in HPLC. The presentation discussed the steps involved in HPLC method development including column selection, mobile phase composition, pH range selection, and optimization of separation conditions. It also covered validation parameters such as accuracy, precision, specificity, limit of detection, and limit of quantification as per ICH guidelines. The presentation included an example method development for the simultaneous estimation of atorvastatin and telmisartan from a tablet formulation.
This document discusses analytical method development for pharmaceutical drug substances and products. It describes the importance of method development and outlines the key steps involved, including collecting sample information, selecting the chromatographic technique, stationary and mobile phases. It also discusses sources of impurities in drugs, control and qualification of impurities according to ICH guidelines, and pharmacopeial and ICH quality guidelines for impurity testing and thresholds.
This document presents the development and validation of an RP-HPLC method for the simultaneous estimation of a muscle relaxant drug and analgesic drug in pure form and pharmaceutical dosage forms. It discusses conducting a literature review on existing methods, determining the physicochemical properties of the drugs, optimizing the analytical method, and validating the developed method as per ICH guidelines. The expected outcomes are an accurate, precise, simple, cost-effective and fast method for simultaneously analyzing the two drugs.
The document describes a method development and validation project for the analysis of drugs using UV spectrophotometry and HPLC. It provides an introduction, objectives, literature review, and plan of work. The literature review summarizes 15 research papers on method development and validation using these techniques. The instruments available for the project are also listed. The conclusion states that the project aims to develop analytical methods for quality assessment of drug products to ensure therapeutic effectiveness.
This document describes the development and validation of an RP-HPLC method for the quantification of verapamil in drug substances and products. It involves selecting the optimal chromatographic conditions, such as the column, mobile phase, flow rate, and developing the method according to ICH guidelines. The method development steps include selecting the HPLC method and conditions, optimizing the selectivity and system parameters, and validating the method parameters like accuracy, precision, specificity, linearity and range. The goal is to develop a simple, accurate and precise RP-HPLC method for the analysis of verapamil that can be validated as per regulatory requirements.
This document describes the development and validation of a UV spectrophotometric method for the estimation of methocarbamol in bulk and pharmaceutical dosage forms. The method was developed using acetone and 0.1N sodium hydroxide solution as solvents, in which methocarbamol is soluble. The drug has maximum absorbance at 267 nm. The method was validated as per ICH guidelines and was found to be linear, precise, accurate and specific. The developed method can be used for the quantitative analysis of methocarbamol in bulk and pharmaceutical formulations.
This document describes a liquid chromatographic method for the simultaneous quantitative determination of candesartan cilexetil and hydrochlorothiazide in pharmaceutical dosage forms. A simple and sensitive RP-HPLC method was developed and validated. The method allows for the separation, identification and quantification of candesartan cilexetil and hydrochlorothiazide in tablet formulations using a C18 column with UV detection. The method was validated in terms of specificity, linearity, precision, accuracy and robustness.
This document discusses considerations for developing assay methods. It recommends starting with existing reference standard methods and literature. The method should separate the analyte peak from all impurities and degradants. Tools to reduce run time include shorter columns, larger particle sizes, and optimizing mobile phase composition. The same method can sometimes be used for assay and reference standards if linearity criteria are met. Extraction efficiency must be over 150% and placebo interference under 2%. Runtimes for in-process tests should be under 5 minutes. Sample quantity for content uniformity tests is 1-3 unit doses and for assays is 3-10 unit doses.
The drug or drug combination may not be official in any pharmacopoeias.
A proper analytical procedure for the drug may not be available in the literature due to patent regulations.
Analytical methods may not be available for the drug in the form of a formulation due to the interference caused by the formulation excipients.
Analytical methods for the quantitation of the drug in biological fluids may not be available.
Analytical methods for a drug in combination with other drugs may not be available.
The existing analytical procedures may require expensive reagents and solvents. It may also involve cumbersome extraction and separation procedures and these may not be reliable.
RP-HPLC Method Development and Validation of Ketoconazole in Bulk and Pharmac...Sunil Vadithya
The document describes the development and validation of an RP-HPLC method for the estimation of Ketoconazole in pharmaceutical formulations. A Phenomenex Luna C18 column with a mobile phase of acetonitrile and phosphate buffer was used to separate Ketoconazole. The retention time of Ketoconazole was 4.768 minutes. The method was validated for accuracy, precision, linearity, robustness and specific parameters. The developed and validated method can be used for the routine analysis of Ketoconazole in formulations.
Method validation in HPLC of omeprazole enantiomerscoolprashant33
Nilesh Kamble presented a seminar on the development and validation of a method for the enantiomeric estimation of omeprazole enantiomers in enteric-coated formulations using high-performance liquid chromatography. Omeprazole exists as two enantiomers but the S-enantiomer is metabolized more slowly and at lower doses. The method was developed using a chiral column with normal phase chromatography. Validation showed the method was specific, stability-indicating, linear, accurate and suitable for quantifying the undesired enantiomer in formulations. The developed method can help ensure only the desired enantiomer is present in marketed formulations.
This document provides guidance on developing and optimizing a regulated bioanalytical method using liquid chromatography-tandem mass spectrometry (LC-MS/MS). It discusses important considerations for method development including choosing a detection technique, optimizing sample extraction and chromatography conditions, and validating the final method. The goal is to develop a selective, sensitive and reproducible method for quantifying biological samples in a regulated setting.
Similar to RP-HPLC Method Development and Validation for the Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Tablet Dosage FormIjpar 14 607 madhavi
This document describes the development and validation of an RP-HPLC method for the simultaneous estimation of atenolol and amlodipine in tablet dosage forms. The method utilizes a C18 column with a mobile phase of triethylamine buffer, acetonitrile and methanol pumped isocratically at a flow rate of 1.0 mL/min. Atenolol and amlodipine were detected at 232.2 nm. The method was validated per ICH guidelines and showed good precision, accuracy, linearity, specificity and robustness, making it suitable for the simultaneous analysis of these drugs in pharmaceutical formulations.
This document describes the development and validation of a new reverse phase high performance liquid chromatography (RP-HPLC) method for the estimation of paracetamol in pharmaceutical dosage forms. Some key points:
- An isocratic RP-HPLC method was developed using a mobile phase of acetonitrile and potassium dihydrogen orthophosphate buffer at a ratio of 15:85, pH 2.5.
- The method was validated for parameters such as linearity, accuracy, precision, limit of detection, limit of quantification, and robustness as per ICH guidelines.
- The method showed good linearity in the range of 25-60 μg/ml with a correlation coefficient of 0.999
Method Development and Validation on Etomidate injection by RP-HPLCpharmaindexing
This document describes the development and validation of a high performance liquid chromatography (HPLC) method for the analysis of etomidate injection. The method uses a Waters HPLC system with a Develosil-ODS-UG column and a mobile phase of acetonitrile and phosphate buffer at a ratio of 40:60. The method was validated per ICH guidelines and found to be accurate, precise, linear, robust and sensitive for quantifying etomidate in injections. The method was then applied to analyze etomidate levels in marketed injection formulations.
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
New RP HPLC method for the simultaneous estimation of rosuvastatin and aspiri...SriramNagarajan19
A simple and selective LC method is described for the determination of Rosuvastatin and Aspirin tablet dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of A mixture of 60 volumes of 20mM Phosphate buffer pH 3.5: 20 volumes of Acetonitrile and 20 voulmes of Methanol. With detection of 232 nm. Linearity was observed in the range 12-28 µg /ml for Rosuvastatin (r2 =0.9977) and 90-210 µg /ml for Aspirin (r2 =0.9953) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing % RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
VALIDATION AND DETERMINATION OF CAFFEINE CONTENT IN ENERGY DRINKS BY USING HP...Ruqsar Fatima
This document outlines the validation and determination of caffeine content in energy drinks using HPLC methods. It includes an introduction on caffeine, the principle of HPLC separation, materials and methods for sample preparation and instrument operation, results and discussion of the validation including calibration curves, precision, accuracy, specificity, LOD and LOQ. The method was found to be precise, accurate, specific and sensitive for quantifying caffeine levels in various energy drinks in under 3 minutes. In conclusion, the validated HPLC method provides an effective quality control technique for caffeine analysis in energy drinks.
Method development and validation for the estimation of Atorvastatin, Ezitimi...SriramNagarajan18
Method development and validation for the estimation of Atorvastatin, Ezitimibe and Fenofibrate in bulk and pharmaceutical dosage forms by RP-HPLC method
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
All manuscripts are subject to rapid peer review. Those of high quality (not previously published and not under consideration for publication in another journal) will be published without delay.
Analytical method development and validation for the estimation of aspirin an...SriramNagarajan19
A simple and selective LC method is described for the determination of Aspirin and Omeprazole in tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of 30 volumes of ammonium acetate buffer, 40 volumes of acetonitrile and 30 volumes of Methanol with detection of 233 nm. Linearity was observed in the range 18-42 µg/ml for Aspirin (r2 =0.983) and 6-14 µg /ml for Omeprazole (r2 =0.970) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
Development and Validation of Reverse Phase Liquid Chromatography Method for ...IOSR Journals
This document describes the development and validation of a reverse phase liquid chromatography method for the estimation of losartan in bulk drug samples. The method utilizes an Acquity BEH C18 column with a mobile phase of buffer and acetonitrile at a ratio of 50:50 delivered isocratically at 0.3 mL/min. Losartan was detected at 230 nm. The method was validated per ICH guidelines and found to be linear, precise, accurate, specific and stability-indicating for the quantification of losartan in the range of 25-75 μg/mL. The method validation shows the method is suitable for the routine analysis of losartan in bulk drug materials.
Development and validation of HPLC method for the estimation of Escitalopram ...SriramNagarajan15
A simple, specific, robust, accurate and precise isocratic HPLC method has been developed and subsequently validated for simultaneous determination of escitalopram (ESP) in pharmaceutical dosage forms. Kromosil (250x4.6)mm 5µ with flow rate of 1ml/ min by using JASCO PU-1580 and UV/VIS JASCO UV-1570 at 238 nm. The separation was carried out using a mobile phase consisting of acetonitrile, methanol and 5mM ammonium acetate buffer (pH 3.0) in the ratio 30:20:50 respectively. The retention time for escitaloparm was found to be 5.36 minutes respectively. The correlation coefficient was found to be 0.9997 (ESP). The mean percentage recovery was found to be 101.86 respectively. The % estimation of the drugs was found near to 100 % representing the accuracy in the method. The proposed method was also validated and applied for the analysis of drugs in tablet formulation.
Development and validation of HPLC method for the estimation of Escitalopram ...pharmaindexing
This document describes the development and validation of a HPLC method for the estimation of Escitalopram oxalate in tablets. Key points:
- An isocratic HPLC method was developed and validated for the simultaneous determination of Escitalopram in pharmaceutical formulations.
- The method used a C18 column, mobile phase of acetonitrile:methanol:ammonium acetate buffer, and UV detection at 238nm. Escitalopram had a retention time of 5.36 minutes.
- The method was validated per ICH guidelines and found to be linear, precise, accurate, rugged and robust. Analysis of tablet formulations found Escitalopram levels within 100% of claimed content.
Method development and validation for the simultaneous estimation of sitaglip...pharmaindexing
Method development and validation for the simultaneous estimation of sitagliptin and metformin in tablet dosage form by RP-HPLC
Similar to RP-HPLC Method Development and Validation for the Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Tablet Dosage FormIjpar 14 607 madhavi (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
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A descriptive study on newborn care among postnatal mothers in selected mater...pharmaindexing
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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.
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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.
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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.
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Osvaldo Bernardo Muchanga-GASTROINTESTINAL INFECTIONS AND GASTRITIS-2024.pdfOsvaldo Bernardo Muchanga
GASTROINTESTINAL INFECTIONS AND GASTRITIS
Osvaldo Bernardo Muchanga
Gastrointestinal Infections
GASTROINTESTINAL INFECTIONS result from the ingestion of pathogens that cause infections at the level of this tract, generally being transmitted by food, water and hands contaminated by microorganisms such as E. coli, Salmonella, Shigella, Vibrio cholerae, Campylobacter, Staphylococcus, Rotavirus among others that are generally contained in feces, thus configuring a FECAL-ORAL type of transmission.
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Among patients with gastritis and/or ulcers, one of the dilemmas is associated with the foods to consume in order to minimize the sensation of pain and discomfort.
June 2024 Oncology Cartoons By Dr Kanhu Charan Patro
RP-HPLC Method Development and Validation for the Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Tablet Dosage FormIjpar 14 607 madhavi
1. 109
*Corresponding author: K.Madhavi
E-mail address: madhavi.kori@gmail.com
IJPAR |Volume 3 | Issue 1 | Jan-Mar-2014 ISSN: 2320-2831
Available Online at: www.ijpar.com
[Research article]
RP-HPLC Method Development and Validation for the
Simultaneous Estimation of Atenolol and Indapamide in
Pharmaceutical Tablet Dosage Form
* K.Madhavi, 2
K.Deepti, 3
B.Harika
Department of Pharmaceutical Analysis and Quality Assurance, Smt. Sarojini Ramulamma
College of Pharmacy, Sheshadrinagar, Mahabubnagar - 509001, Andhrapradesh, India.
ABSTRACT
A simple reversed-phase high-performance liquid chromatographic (RP-HPLC) method has been developed and
validated for simultaneous determination of ATENOLOL and INDAPAMIDE in pharmaceutical tablet dosage form.
Chromatographic analysis was performed on a Symmetry X-terra C8 (4.6mm x 100mm, 5m) column at ambient
temperature with a mixture of Potassium di hydrogen phosphate buffer and Acetonitrile in the ratio 40:60 v/v as
mobile phase, at a flow rate of 0.7 mL min-1
. UV detection was performed at 240 nm. The retention times of
Atenolol and Indapamide were 2.1 and 3.6 min, respectively. The correlation coefficient of Atenolol and
Indapamide was found to be 0.999. Calibration plots were linear over the concentration ranges 20–100 μg mL- 1
and
1-5 μg mL-
for Atenolol and Indapamide respectively. The Limit of detection was 0.223 and 0.286µg mL-1
and the
quantification limit were 0.677 µg mL-1
and 0.86µg mL-1
for Atenolol and Indapamide, respectively. The accuracy
of the proposed method was determined by recovery studies and found to be 100.74% to 99.93%.The method was
validated for accuracy, linearity, sensitivity, precision, robustness, system suitability Commercial tablet formulation
was successfully analyzed using the developed method and the proposed method is applicable to routine analysis of
determination of Atenolol and Indapamide in pharmaceutical tablet dosage form.
Keywords: Atenolol, Indapamide, RP-HPLC, Validation.
INTRODUCTION
Atenolol is chemically (RS)-2-{4-[2-hydroxy-3-
(propan-2-yl amino) propoxy] phenyl} acetamide
[Figure 1] and its molecular formula is C14H22N2O3
hypertension, and molecular weight is 266.34
gm/mole. Atenolol can be used to treat
cardiovascular diseases and conditions such as,
coronary heart disease, arrhythmias, angina and to
treat and reduce the risk of heart complications
following myocardial infarction. Indapamide is
chemically 4-chloro-N-(2-methyl-2,3-dihydroindol-
1-yl)-3-sulfamoyl-benzamide [Figure-2]. Its
molecular formula is C16H16ClN3O3S having
molecular weight 365.84 gm/mole. Indapamide is a
non-thiazide sulphonamide diuretic drug. generally
used in the treatment of hypertension, as well as
decompensated cardiac failure.
2. K.Madhavi et al / Int. J. of Pharmacy and Analytical Research Vol-3(1) 2014 [109-117]
Fig:1 Atenolol Fig:2 lndapamide
MATERIALS AND METHODS
Chemicals/ Reagents and Solvents
Atenolol-25 mg and Indapamide-2.5mg were
obtained from, ZYDUS MEDICA Health Care. Ltd.
Ahmedabad, Double Distilled Water (HPLC grade),
Methanol (HPLC grade), Acetonitrile (HPLC grade),
orthophosphoric acid and Potassium-dihydrogen
phosphate were of reagent grade. The pharmaceutical
preparations of combination of Atenolol &
Indapamide that is ATEN-D tablet (ZYDUS
MEDICA Health Care. Ltd. Ahmedabad).
Instrumentation and Equipments
The HPLC analysis was accomplished on WATERS
high pressure liquid chromatograph outfitted with
515 reciprocating dual column HPLC pump, a
manually operating Rheodyne injector with 20μL
sample loop, X-terra C8 4.6mm x 150mm analytical
column reversed-phase material of 5μ size and a 2487
model UV-Visible detector. All the parameters of
HPLC were controlled by N 2000 chromatographic
system software. Other instruments used were
TECHCOMP UV-Vis spectrophotometer of model
2310, Shimadzu electronic balance of model XEX-
200, ADWA of model AD102U digital pH meter
and ENERTECH of model SE60US ultrasonic bath
sonicator
ANALYTICAL METHOD DEVELOPMENT
Optimization of UV conditions
A waters symmetry X-terra C8 (4.6mm x 150mm,
5m) was used for chromatographic separation.
Mobile phase and sample solution were filtered
through a 0.45μm membrane filter and degassed. The
mobile phase composed of pH3 Buffer (Potassium di
hydrogen phosphate):Acetonitrile ( 40:60 ) at flow
rate 0.7 mL/min with run time 5mins detection of
both drugs was carried out at 240nm.
Fig.3. Isobestic point of Atenolol and indapamide
Optimized Method Parameters
Mobile Phase : Phosphate buffer (3.0 pH): Acetonitrile(40:60)
Column (Stationary Phase) : X-terra(C8) (4.6mm x 150mm, 5m)
Flow rate (ml/min) :0.7
Column temperature (°C) : Ambient
Volume of injection loop (l) : 20
Detection wavelength (nm) :240
Drug RT (min) : Atenolol – 2.1
Indapamide-3.6
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Figure- 4 Optimized chromatogram
Procedure for preparation of solution
Preparation of buffer
Take 1000ml of HPLC grade water. Dissolve 2.72
grams of Potassium di hydrogen phosphate salt and
Adjusted the pH to 3.0 with orthophosphoric acid.
Preparation of mobile phase
A mixture of above prepared buffer 400 ml (40%),
and 600 ml of HPLC grade Acetonitrile (60%) were
mixed and degassed in ultrasonic water bath for 5
minutes. The mobile phase was filterred through 0.45
µ filter under vacuum.
Diluent Preparation
Use the Mobile phase as Diluent.
ASSAY
Preparation of the Atenolol and Indapamide
standard & sample solution
Preparation of Standard Solution
Accurately weighed and transferred 58.8mg of
atenolol and indapamide working standard into a
50ml clean dry volumetric flask and added about
30ml of diluent. It was sonicated to dissolve
completely and made volume up to the mark with the
same diluent. (Stock solution)
From the above stock solution, 10ml of the solution
was pipetted into a 50 ml volumetric flask and diluted
up to the mark with diluent. . From this, 3 ml of the
solution was pipetted into another 10ml volumetric
flask and diluted up to the mark with diluent..
Sample Solution Preparation
Accurately weighed and transferred 58.8 mg of
Atenolol and Indapamide tablet powder into a 100ml
clean dry volumetric flask and added about 70 ml of
diluent. It was sonicated to dissolve it completely and
made volume up to the mark with the same diluent.
(Stock solution).
From the above stock solution, 3 ml of the solution
was pipetted into a 10 ml volumetric flask and diluted
up to the mark with diluent.
Procedure
20 µL of the standard and sample solutions were
injected into the chromatographic system and areas
for the Atenolol and Indapamide peaks were
measured. %Assay was calculated by using the
formulae.
Calculation
Assay % =
AT WS DT P Avg. Wt
--------- x -------- -x ------- x ------- x ------------- X 100
AS DS WT 100 Label Claim
Where:
AT = Average area counts of sample preparation.
AS = Average area counts of standard preparation.
WS = Weight of working standard taken in mg.
P = Percentage purity of working standard
LC = LABEL CLAIM mg/ml.
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ANALYTICAL METHOD VALIDATION
The HPLC method was validated in accordance with
ICH guidelines.
Accuracy
Accuracy was carried out by % recovery studies at
three different concentration levels. To the pre-
analyzed sample solution of ATEN and INDA a
known amount of standard drug powder of ATEN
and INDA were added at 50, 100 and 150 % level.
Precision
The system precision of the method was verified by
five replicate injections of standard solution
containing ATEN and INDA. The method precision
was carried out the analyte five times using the
proposed method. Repeatability was measured by
multiple injections of a homogenous sample of
ATEN and INDA.
Linearity
The linearity was determined separately for ATEN
and INDA. Linearity of the method was studied by
injecting 5 concentrations of both drugs prepared in
methanol and calibration curves were constructed by
plotting peak area against the respective
concentrations
Limit of detection and Limit of quantitation
Sensitivity of the proposed method was estimated in
terms of Limit of Detection (LOD) and Limit of
Quantitation (LOQ). LOD = 3.3 x ASD/S and LOQ =
10 x ASD/S, Where, ‘ASD’ is the average standard
deviation and ‘S’ is the slope of the line.
Robustness
Robustness was evaluated by making deliberate
variations in few method parameters such as variation
of wave length; flow rate and change in mobile phase
composition. The robustness of the method was
studied for ATEN and INDA.
RESULTS
Selection of Chromatographic Conditions and
Optimization of Mobile Phase
Mobile phase was optimized to separate ATEN and
INDA using Symmetry C8 column (150 mm x 4.6
mm i.d.,5 μm). Initially, ACN and phosphate buffer
in the equal proportions were tried as mobile phase
but the splitting of the peaks for both these drugs was
observed. Therefore, after adjustment of pH of mixed
phosphate buffer to 3.0 with ortho-phosphoric acid,
and mobile phase composition (ACN and phosphate
buffer in 40:60 % v/v) was tried for resolution of
both drugs. Good resolution and symmetric peaks
were obtained for both drugs when the pH of the
mobile phase (buffer) was adjusted to 3.0. The flow
rate of the mobile phase was 0.7 mL min-1. Under
optimum chromatographic conditions, the retention
time for ATEN and INDA was found to be 2.1 and
3.6 min, respectively when the detection was carried
out at 240 nm
A typical chromatogram of two drugs is shown in
(Figure -4).
Table-1 Accuracy data for Atenolol and Indapamide:
Injection
Atenolol Indapamide
50% 100% 150% 50% 100% 150%
Inj-1 3058153 4141888 5193545 464090 614631 751157
Inj-2 3086875 4139942 5991256 460733 617416 764616
Inj-3 3039485 4128889 5134625 463249 602389 774998
AVG 3061504 4136906 5151290 462690.7 611478.7 763590.3
S.D 23872.09 7011.059 36865.34 1746.758 7994.097 11953.55
%R.S.D 0.78 0.17 0.72 0.38 1.31 1.57
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Table-2 Accuracy(Recovery) result for Atenolol and Indapamide :
Drug Name Spike
level
Area Amount
Added(mg)
Amount
Found(mg)
%
Recovery
% of mean
recovery
Atenolol
50%
3028171 90 89.8 99.23
100.74
100%
4136906 120 121.2 102
150%
5151290 150 150.9 101
Indapamide 50%
462690 4.50 4.524 101.33
99.93100%
611478 6 5.98 99.33
150%
763590 7.50 7.47 99.33
Table-3 System Precision Result for Atenolol and Indapamide:
S.No Injections Area of Atenolol Area of Indapamide
1 Injection-1 2015090 1030445
2 Injection-2 2100046 1028130
3 Injection-3 2065369 1001212
4 Injection-4 2096138 1017377
5 Injection-5 2103317 1031363
Average 2075992 1021705.4
Standard deviation 37259.27 12744.02
%RSD 1.79 1.27
Table-4 Method precision (reproducibility) of Atenolol and Indapamide:
S.No Injections Area of Atenolol Area of Indapamide
1 Injection-1 2038600 1086110
2 Injection-2 2069689 1066922
3 Injection-3 2086267 1095482
4 Injection-4 2147805 1085921
5 Injection-5 2075926 1083763
Average 2083657.4 1083640
Standard deviation 40021.19 10380.79
%RSD 1.92 0.96
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Table-5 LINEARITY RESULTS OF Atenolol and Indapamide:
ATENOLOL INDAPAMIDE
Conc(mcg/ml) Area Conc(mcg/ml) Area
20 913226 1 29279
40 1482271 2 153131
60 2147805 3 312399
80 2747059 4 454118
100 3416501 5 613618
Figure-5: Linearity Graphs of Atenolol and Indapamide
Linearity graph of Atenolol
Linearity graph of Indapamide
y = 14696x - 12839
R² = 0.999
0
100000
200000
300000
400000
500000
600000
700000
0 1 2 3 4 5 6
ABSORBANCEAREA
…
CALIBRATION CURVE
y = 146967x - 128391
R² = 0.9984
0
100000
200000
300000
400000
500000
600000
700000
0 1 2 3 4 5 6
ABSORBANCEAREA
…
CALIBRATION CURVE
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Table-6 Results of LOD and LOQ
S.No Drug name Standard deviation Slope LOD LOQ
1 Atenolol 21246 313566 0.223595 0.677561
2 Indapamide 12744 146966 0.286155 0.867139
Table -7 Robustness Result For Atenolol and Indapamide At Different Condition
S.No Parameter Atenolol Indapamide
Theoretical
plates per
column
Tailing
factor
Resolution Theoretical
plates per
column
Tailing
factor
Resolution
1 Less
flow(0.63ml/min)
1341 1.319 - 3057 1.143 5.291
2 Accuracy std flow
rate(1.0 ml/min)
2215 1.265 - 2776 1.069 5.109
3 More flow(0.77
ml/min)
1170 1.357 - 2751 1.178 5.000
4 %10 Less organic 1271 1.348 - 3001 1.160 5.396
5 Accuracy std (100%
organic)
2215 1.265 - 2776 1.069 5.109
6 %10 More organic 1188 1.304 - 2750 1.081 5.094
RESULTS AND DISCUSSION
Accuracy
The accuracy of the method studied at three different
concentration levels i.e. 50 %, 100 % and 150 %
showed acceptable % recoveries in the range of
100.74 % for atenolol and 99.93 % for indapamide.
Precision
The precision study of ATEN and INDA was
evaluated on the basis of % RSD value was found to
be in the range 0.7 – 1.8%respectively. As the RSD
values were < 2% therefore developed method was
precise.
Linearity
The linearity was determined separately for ATEN
and INDA. Linearity of the method was studied by
injecting five concentrations of both drugs prepared
in methanol and calibration curves were constructed
by plotting peak area against the respective
concentrations. The ATEN and INDA followed
linearity in the concentration range of 20-100 μg mL-
1 and 1-5 μg mL-1; respectively.
Limit of detection and Limit of quantitation
The LOD was found to be 0.223595 and 0.286155
μg, respectively. The LOQ for ATEN and INDA was
found to be and 0.677561 and 0.867139 μg,
respectively. The low values of LOD and LOQ
indicates high sensitivity of the method.
Robustness study
Robustness of the method was studied by making
deliberate changes in the chromatographic conditions
and the effects on the results were examined. The low
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value changes of theoretical plates, tailing factor
indicating robustness of the method. When the
method was performed by two different analysts
under the same experimental and environmental
conditions it was found to be rugged and % RSD
(less than 2 %) indicating ruggedness of the method.
Analysis of marketed tablet formulation
3 replicates of the samples solutions (20 μL) were
injected for quantitative analysis. The amounts of
ATEN and INDA estimated were found to 100.74 %
and 99.93 %, respectively. A good separation and
resolution of both drugs indicates that there was no
interference from the excipients commonly present in
pharmaceutical formulations.
System Suitability Test
The system suitability parameters such as resolution,
number of theoretical plates and tailing factor were
studied..
Table- 8 ASSAY RESULTS
Assay Results Drug Amount present/tablet % of Assay
Atenolol 25 mg 100.2
Indapamide 2.5mg 99.11
Table-9 System Suitability parameter
CONCLUSION
The developed RP-HPLC method is simple, precise,
accurate, selective and reproducible. The method has
been found to be adequately rugged and robust and
can be used for simultaneous determination of
Atenolol and Indapamidel in tablet formulation. The
method was validated as per ICH guidelines
ACKNOWLEDGEMENTS
I like thankful to Pharmatech research labotatories.,
Hyderabad, India for providing the gift samples of
Atenolol and Indapamide. And also to the principal
Dr.K.Rajeshwar Dutt, Smt. Sarojini Ramulamma
College of Pharmacy, Mahabubnagar, Andhra
pradesh, India and special thanks for Ms.K.Deepti
madam & Ms.Ramathilagam madam as well as my
friends who helped during the project work.
REFERENCES
[1] Indian pharmacopeia 2007.
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[5] ICH, Q1A (R2) Stability testing of new drug substances and products, in: International Conference on
Harmonization, IFPMA, Geneva, (2003).
[6] Practical HPLC method development Lloyd R.Snyder, Joseph J. Kirkland, Joseph L. Glajch, second edition
System suitability parameters Atenolol Indapamide
Retention time(min 2.1 3.6
Tailing factor 1.332 1.1405
Theoretical plates number 1242 2889
Resolution - 5.195
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[8] MeSH Indapamide
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