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.
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.
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.
spectrophotometric estimation of metformin in bulk and in its dosage formsaikiranyuvi
The document describes the development and validation of a UV spectrophotometric method for the estimation of metformin in bulk and tablet dosage forms. Key aspects include determining the absorption maximum of 646 nm for metformin and developing a linear calibration curve within the concentration range of 8-16 μg/ml. The method was validated based on parameters such as accuracy, precision, LOD, LOQ and recovery, demonstrating the method is simple, accurate, precise and can be used to analyze metformin in pharmaceutical formulations.
This document describes the development and validation of an RP-HPLC method for the simultaneous quantification of telmisartan and atorvastatin from tablet formulations. The method utilizes a C18 column with a mobile phase of acetonitrile and phosphate buffer at a ratio of 75:25. Detection is carried out at 220nm. The method was validated per ICH guidelines and found to be linear, precise, accurate, robust and suitable for quality control testing of tablet formulations containing telmisartan and atorvastatin.
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.
Development and Validation of an RP HPLC Method for Analysis of Sitagliptinijtsrd
Sitagliptin is a drug used against type 2 diabetes mellitus and it is a member of class of anti diabetic drugs known as dipeptidyl peptidase 4 inhibitors or gliptins . A simple, sensitive and accurate RP HPLC method has been developed for the determination of Sitagliptin in bulk formulation. The max of the Sitagliptin was found to be 267nm in Methanol phosphate buffer 10mM pH 4.8 60 40 v v . The method shows high sensitivity with linearity 10 to 50µg ml regression equation y = 45765x 239272 r2 = 0.9996 . The various parameters according to ICH guidelines and USP are followed for validating and testing of this method. The Detection limit and quantitation limit were found to be 0.743 µg ml-1 and 2.25µgml-1 respectively. The results demonstrated that the procedure is accurate, specific and reproducible RSD 2 , and also being simple, cheap and less time consuming and appropriate for the determination of Sitagliptin in bulk and pharmaceutical formulation. Pradnya Lokhande "Development and Validation of an RP-HPLC Method for Analysis of Sitagliptin" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-6 , October 2019, URL: https://www.ijtsrd.com/papers/ijtsrd29214.pdf Paper URL: https://www.ijtsrd.com/chemistry/analytical-chemistry/29214/development-and-validation-of-an-rp-hplc-method-for-analysis-of-sitagliptin/pradnya-lokhande
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.
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.
spectrophotometric estimation of metformin in bulk and in its dosage formsaikiranyuvi
The document describes the development and validation of a UV spectrophotometric method for the estimation of metformin in bulk and tablet dosage forms. Key aspects include determining the absorption maximum of 646 nm for metformin and developing a linear calibration curve within the concentration range of 8-16 μg/ml. The method was validated based on parameters such as accuracy, precision, LOD, LOQ and recovery, demonstrating the method is simple, accurate, precise and can be used to analyze metformin in pharmaceutical formulations.
This document describes the development and validation of an RP-HPLC method for the simultaneous quantification of telmisartan and atorvastatin from tablet formulations. The method utilizes a C18 column with a mobile phase of acetonitrile and phosphate buffer at a ratio of 75:25. Detection is carried out at 220nm. The method was validated per ICH guidelines and found to be linear, precise, accurate, robust and suitable for quality control testing of tablet formulations containing telmisartan and atorvastatin.
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.
Development and Validation of an RP HPLC Method for Analysis of Sitagliptinijtsrd
Sitagliptin is a drug used against type 2 diabetes mellitus and it is a member of class of anti diabetic drugs known as dipeptidyl peptidase 4 inhibitors or gliptins . A simple, sensitive and accurate RP HPLC method has been developed for the determination of Sitagliptin in bulk formulation. The max of the Sitagliptin was found to be 267nm in Methanol phosphate buffer 10mM pH 4.8 60 40 v v . The method shows high sensitivity with linearity 10 to 50µg ml regression equation y = 45765x 239272 r2 = 0.9996 . The various parameters according to ICH guidelines and USP are followed for validating and testing of this method. The Detection limit and quantitation limit were found to be 0.743 µg ml-1 and 2.25µgml-1 respectively. The results demonstrated that the procedure is accurate, specific and reproducible RSD 2 , and also being simple, cheap and less time consuming and appropriate for the determination of Sitagliptin in bulk and pharmaceutical formulation. Pradnya Lokhande "Development and Validation of an RP-HPLC Method for Analysis of Sitagliptin" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-6 , October 2019, URL: https://www.ijtsrd.com/papers/ijtsrd29214.pdf Paper URL: https://www.ijtsrd.com/chemistry/analytical-chemistry/29214/development-and-validation-of-an-rp-hplc-method-for-analysis-of-sitagliptin/pradnya-lokhande
Method Development and Validation for Simultaneous Estimation of Dasatinib an...YogeshIJTSRD
The document describes the development and validation of an isocratic reverse phase HPLC method for the simultaneous quantification of Dasatinib and Erlotinib in pharmaceutical formulations. The method was optimized using a response surface methodology with a central composite design to evaluate the effects of varying the methanol percentage, pH, and flow rate on the separation. The optimized conditions provided good resolution of Dasatinib, Erlotinib and the internal standard within 9 minutes. The method was validated as per ICH guidelines and successfully applied to the analysis of commercial tablet and capsule formulations containing the two drugs.
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.
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 the development and validation of an RP-HPLC method for the simultaneous estimation of atorvastatin and olmesartan tablets. The method was developed using a BDS hypersil C18 column with a mobile phase of ACN-TEA 40-60-0.1 pH 4.0 and detection at 235 nm. The method was validated for parameters such as linearity, precision, accuracy, robustness and system suitability and found to be suitable for the simultaneous quantification of atorvastatin and olmesartan in combined tablet dosage forms.
Rapid Reverse-phase High-performance Liquid Chromatography Estimation of Meth...BRNSS Publication Hub
A simple, sensitive, and selective reverse-phase high-performance liquid chromatography (RP-HPLC) method with ultraviolet (UV) detection for the estimation of methotrexate in pharmaceutical formulation and in spiked plasma developed and validated in the present work. Chromatographic separation of drug is performed with a 250 mm × 4.6 mm, 5 μm diameter particles RP C-18 column and the mobile phase consisted of a mixture of methanol and water (80:20, v/v), containing 0.1% HPLC-grade glacial acetic acid for the adjustment of pH to 4.5. Isocratic elution at a flow rate of 1 ml/min with UV detection at 256 nm at ambient temperature is used in this method. The proposed RP-HPLC method is successfully applied for the determination of methotrexate in pharmaceutical preparation and spiked plasma samples. The validation studies are carried out and it’s fulfilling ICH requirements. The method is found to be specific, linear, precise (including both intra- and inter-day precision), accurate, and robust. This proposed method may represent a valuable aid in the laboratory monitoring of the toxicity of anticancer chemotherapy.
IOSRPHR(www.iosrphr.org) IOSR Journal of Pharmacyiosrphr_editor
A simple reverse phase liquid chromatographic method was developed and validated for the simultaneous estimation of lornoxicam and paracetamol from their pharmaceutical dosage forms. The method utilized a C18 column with a mobile phase of potassium dihydrogen phosphate (pH 7.3) and acetonitrile (70:30) and detected compounds at 257nm. The method was linear over 20-60μg/ml for paracetamol and 0.2-1.8μg/ml for lornoxicam. Retention times were 2.33 minutes for paracetamol and 7.61 minutes for lornoxicam. The method was validated per ICH guidelines and demonstrated good precision, accuracy, reproducibility
UV Spectrophotometric Method Development and Validation for Quantitative Esti...Sagar Savale
This document describes the development and validation of a UV spectrophotometric method for the quantitative estimation of paracetamol. Paracetamol was found to exhibit maximum absorption at 244 nm in methanol. The method was validated according to ICH guidelines and showed good linearity (R2 = 0.9999), recovery (99.78-100.54%), precision (<0.06% RSD), ruggedness (<0.02% RSD), and sensitivity (LOD = 0.37 μg/ml, LOQ = 0.98 μg/ml). The developed method is simple, rapid, economical and suitable for the analysis of paracetamol in bulk drug samples.
Spectrophotometric Estimation of Dronedarone Hydrochloride in Pharmaceutical ...Jing Zang
An accurate and precise UV spectrophotometric method with multivariate calibration technique for the determination of dronedarone hydrochloride in pharmaceutical dosage forms has been described. The term multivariate calibration refers to the process of constructing a mathematical model that relates a property such as content or identity to the absorbance of a set of known reference samples at more than one wavelength. Dronedarone shows maximum wavelength at 288 nm using methanol as a solvent and obeyed Beer’s law in the linear range of 10-35μg/ml. The present method was found to be accurate, precise, and can be successfully used for quantitative estimation of dronedarone in drug and tablet dosage form compare to other complex techniques.
VALIDATED RP - HPLC METHOD FOR THE ESTIMATION OF LIRAGLUTIDE IN TABLET DOSAGEIJSIT Editor
This document presents a validated RP-HPLC method for the estimation of Liraglutide in tablet dosage forms. The method utilizes a C18 column with a mobile phase of 0.1% ortho phosphoric acid, acetonitrile and methanol. Liraglutide was detected at 245nm with a retention time of 4.447 minutes. The method was validated in terms of linearity, precision, accuracy and specificity according to ICH guidelines. The method was successfully applied to analyze Liraglutide levels in commercial tablets.
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.
Life presents problems but also solutions. While the past cannot be changed, one can create a successful future. It is better to solve problems than worry about them. Learn from mistakes and use experience to find success. Remain calm through challenges and celebrate victories. Difficult times can make you stronger if you accept what you cannot control and keep moving forward.
PLEZI by PortisEd., c'est disposer tout à la fois des compétences éditoriales de PortisEd. et de la solution d'inbound marketing et de marketing automation PLEZI.
Method Development and Validation for Simultaneous Estimation of Dasatinib an...YogeshIJTSRD
The document describes the development and validation of an isocratic reverse phase HPLC method for the simultaneous quantification of Dasatinib and Erlotinib in pharmaceutical formulations. The method was optimized using a response surface methodology with a central composite design to evaluate the effects of varying the methanol percentage, pH, and flow rate on the separation. The optimized conditions provided good resolution of Dasatinib, Erlotinib and the internal standard within 9 minutes. The method was validated as per ICH guidelines and successfully applied to the analysis of commercial tablet and capsule formulations containing the two drugs.
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.
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 the development and validation of an RP-HPLC method for the simultaneous estimation of atorvastatin and olmesartan tablets. The method was developed using a BDS hypersil C18 column with a mobile phase of ACN-TEA 40-60-0.1 pH 4.0 and detection at 235 nm. The method was validated for parameters such as linearity, precision, accuracy, robustness and system suitability and found to be suitable for the simultaneous quantification of atorvastatin and olmesartan in combined tablet dosage forms.
Rapid Reverse-phase High-performance Liquid Chromatography Estimation of Meth...BRNSS Publication Hub
A simple, sensitive, and selective reverse-phase high-performance liquid chromatography (RP-HPLC) method with ultraviolet (UV) detection for the estimation of methotrexate in pharmaceutical formulation and in spiked plasma developed and validated in the present work. Chromatographic separation of drug is performed with a 250 mm × 4.6 mm, 5 μm diameter particles RP C-18 column and the mobile phase consisted of a mixture of methanol and water (80:20, v/v), containing 0.1% HPLC-grade glacial acetic acid for the adjustment of pH to 4.5. Isocratic elution at a flow rate of 1 ml/min with UV detection at 256 nm at ambient temperature is used in this method. The proposed RP-HPLC method is successfully applied for the determination of methotrexate in pharmaceutical preparation and spiked plasma samples. The validation studies are carried out and it’s fulfilling ICH requirements. The method is found to be specific, linear, precise (including both intra- and inter-day precision), accurate, and robust. This proposed method may represent a valuable aid in the laboratory monitoring of the toxicity of anticancer chemotherapy.
IOSRPHR(www.iosrphr.org) IOSR Journal of Pharmacyiosrphr_editor
A simple reverse phase liquid chromatographic method was developed and validated for the simultaneous estimation of lornoxicam and paracetamol from their pharmaceutical dosage forms. The method utilized a C18 column with a mobile phase of potassium dihydrogen phosphate (pH 7.3) and acetonitrile (70:30) and detected compounds at 257nm. The method was linear over 20-60μg/ml for paracetamol and 0.2-1.8μg/ml for lornoxicam. Retention times were 2.33 minutes for paracetamol and 7.61 minutes for lornoxicam. The method was validated per ICH guidelines and demonstrated good precision, accuracy, reproducibility
UV Spectrophotometric Method Development and Validation for Quantitative Esti...Sagar Savale
This document describes the development and validation of a UV spectrophotometric method for the quantitative estimation of paracetamol. Paracetamol was found to exhibit maximum absorption at 244 nm in methanol. The method was validated according to ICH guidelines and showed good linearity (R2 = 0.9999), recovery (99.78-100.54%), precision (<0.06% RSD), ruggedness (<0.02% RSD), and sensitivity (LOD = 0.37 μg/ml, LOQ = 0.98 μg/ml). The developed method is simple, rapid, economical and suitable for the analysis of paracetamol in bulk drug samples.
Spectrophotometric Estimation of Dronedarone Hydrochloride in Pharmaceutical ...Jing Zang
An accurate and precise UV spectrophotometric method with multivariate calibration technique for the determination of dronedarone hydrochloride in pharmaceutical dosage forms has been described. The term multivariate calibration refers to the process of constructing a mathematical model that relates a property such as content or identity to the absorbance of a set of known reference samples at more than one wavelength. Dronedarone shows maximum wavelength at 288 nm using methanol as a solvent and obeyed Beer’s law in the linear range of 10-35μg/ml. The present method was found to be accurate, precise, and can be successfully used for quantitative estimation of dronedarone in drug and tablet dosage form compare to other complex techniques.
VALIDATED RP - HPLC METHOD FOR THE ESTIMATION OF LIRAGLUTIDE IN TABLET DOSAGEIJSIT Editor
This document presents a validated RP-HPLC method for the estimation of Liraglutide in tablet dosage forms. The method utilizes a C18 column with a mobile phase of 0.1% ortho phosphoric acid, acetonitrile and methanol. Liraglutide was detected at 245nm with a retention time of 4.447 minutes. The method was validated in terms of linearity, precision, accuracy and specificity according to ICH guidelines. The method was successfully applied to analyze Liraglutide levels in commercial tablets.
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.
Life presents problems but also solutions. While the past cannot be changed, one can create a successful future. It is better to solve problems than worry about them. Learn from mistakes and use experience to find success. Remain calm through challenges and celebrate victories. Difficult times can make you stronger if you accept what you cannot control and keep moving forward.
PLEZI by PortisEd., c'est disposer tout à la fois des compétences éditoriales de PortisEd. et de la solution d'inbound marketing et de marketing automation PLEZI.
Investigational new drug ,orange book,understanding on 505(b) (2) applicationsswrk
This document discusses investigational new drug applications, the Orange Book, and 505(b)(2) applications. It provides an overview of the IND process including when an IND is needed, the content of an IND application, annual reporting requirements, and classifications of INDs. It also describes the Orange Book's listing of approved drugs and their therapeutic equivalence ratings. Finally, it gives a brief explanation of 505(b)(2) applications, including what products are allowed and examples of 505(b)(2) NDAs.
Documentation relating to product development,sop's,cleaning methods,quality ...swrk
COMPLAINT HANDLING IN PHARMACEUTICAL COMPANIES,PRODUCT RECALL,RETENTION RECORDS, DISTRIBUTION RECORDS.prepared by s.susena,m.pharmacy pharmaceutical analysis&QA,ssj college of pharmacy
RP-HPLC method development and validation of ritonavir in bulk and pharmaceut...SriramNagarajan17
This document describes the development and validation of an RP-HPLC method for the quantification of the HIV protease inhibitor ritonavir (RIT) in bulk and pharmaceutical dosage forms. A simple isocratic RP-HPLC method was developed using a C18 column, mobile phase of 0.02M potassium dihydrogen phosphate buffer and acetonitrile (70:30 v/v), and detection at 237 nm. The method was validated per ICH guidelines and showed good linearity from 25-150 μg/mL, precision <0.5% RSD, accuracy of 99.3-100.6% recovery, and ability to quantify RIT in pharmaceutical tablets without interference from excipients.
This document describes the development and validation of a reverse phase HPLC method for the simultaneous estimation of metformin and linagliptin in pure form and pharmaceutical formulations. The method utilizes a C18 column, mobile phase of phosphate buffer and acetonitrile (60:40) at a flow rate of 1 mL/min. Metformin and linagliptin were well separated with retention times of 3.048 and 4.457 minutes respectively. The method was validated per ICH guidelines and showed good linearity, accuracy, precision and recovery for both drugs. The method can be used to simultaneously quantify metformin and linagliptin in tablet formulations.
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.
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.
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
Manuscripts should be carefully checked for grammatical and punctuation errors. All papers undergo peer review. Please note that all articles published in this journal represent the opinions of the authors and do not necessarily reflect the official policy of the Journal of Indo-American Journal of Pharma and Bio Sciences of the journalism research.
Analytical Method Development and Validation of Tolvaptan in Bulk and Tablet ...pharmaindexing
This document describes the development and validation of a reverse phase high performance liquid chromatographic (RP-HPLC) method for the estimation of Tolvaptan in pharmaceutical dosage forms. A C18 column was used with a mobile phase of sodium dihydrogen phosphate and acetonitrile. The method was validated per ICH guidelines and showed good linearity, accuracy, precision, specificity, and robustness. Recovery of Tolvaptan from formulations ranged from 99.74-99.87% indicating the method is accurate for quantifying Tolvaptan in tablets.
A newly validated HPLC method development for simultaneous estimation of rito...SriramNagarajan19
The aim of the present work was to develop a isocratict RP-HPLC for simultaneous analysis of ritonavir and lopinavir in tablet dosage form. Method: chromatographic system was optimized using a Agilent XDB C18(150 x 4.6mm,5µm) column with potassium dihydrogen phosphate (pH 4.6) and acetonitrile in the ratio of 45;55, as a mobile phase, at a flow rate of 1.0 ml/min. detection was carried out at 215nm by a photodiode array detector. Result: ritonavir and lopinavir were eluted with retention times of 4.821 and 3.814mins respectively. Beer’s lambert’s law was obeyed over the concentration ranges of 12.5 to 50µg/ml and 50 to 200µg/ml for ritonavir and lopinavir, respectively. Conclusion: the high recovery and low coefficients of variation confirm the suitability of the method for simultaneous analysis of both drugs in a tablet dosage form. Statistical analysis proves that the method is sensitive and significant for the analysis of ritonavir and lopinavir in pure and in pharmaceutical dosage form without any interference from the excipients. The method was validated in accordance with ICH guidelines. Validation revealed the method is specific, rapid, accurate, precise, reliable, and reproducible.
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.
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.
A simple visible spectrophotometric method is proposed for the determination
of ulipristal acetate present in bulk and tablet formulation. The currently
proposed method is established based on MBTH oxidation by ferric ions to
form an active coupling species (electrophile), followed by its coupling with
the ulipristal in acidic medium to form high intensiϑied green colored chromophore
having max at 609 nm. Validated the method as per the current
guidelines of ICH. Beer’s law was obeyed in the concentration range of 6.25 –
37.50 g mL 1 with a high regression coefϑicient (r > 0.999). Reproducibility,
accuracy, and precision of the method are evident from the low values of R.S.D.
This method can be used in quality control laboratories for routine analysis of
ulipristal acetate in bulk drug and pharmaceutical dosage forms.
IOSRPHR(www.iosrphr.org) IOSR Journal of Pharmacyiosrphr_editor
A simple reverse phase liquid chromatographic method was developed and validated for the simultaneous estimation of lornoxicam and paracetamol from their pharmaceutical dosage forms. The method utilized a C18 column with a mobile phase of potassium dihydrogen phosphate (pH 7.3) and acetonitrile (70:30) and detected compounds at 257nm. The method was linear over 20-60μg/ml for paracetamol and 0.2-1.8μg/ml for lornoxicam. Retention times were 2.33 minutes for paracetamol and 7.61 minutes for lornoxicam. The method was validated per ICH guidelines and demonstrated good precision, accuracy, reproducibility
1. RESEARCH ARTICLE Am. J. PharmTech Res. 2013; 3(3) ISSN: 2249-3387
Please cite this article in press as: Susena S. et al., A Novel validated RP-HPLC method for the
estimation of Liraglutide in bulk and Parenteral Dosage form. American Journal of PharmTech Research
2013.
A Novel validated RP-HPLC method for the estimation of
Liraglutide in bulk and Parenteral Dosage form
S. Susena*1
, K. Vanitha Prakash1
, T.Radika1
, R.Tejaswini1
,E.Manasa1
1. SSJ College of Pharmacy, V.N. Pally, Gandipet, Hyderabad-500075(India).
Department: Pharmaceutical Analysis & Quality assurances)
ABSTRACT
A simple, accurate, precise and rapid reversed-phase high performance liquid chromatographic
(RP-HPLC) method has been developed and subsequently validated for the estimation of
Liraglutide in bulk and Parenteral Dosage form. The proposed method is based on the separation
of drugs in reversed-phase mode using Waters HPLC 22695 model, Inertsil ODS column (250 x
4.6 mm, 5µm particle size).The optimum mobile phase consisted of methanol: phosphate buffer
in the ratio of 85:15 v/v(Phosphate buffer pH 5.5) was selected as a mobile phase, flow rate of
1.0 ml/min and UV detection was set at 246 nm. The retention time was 3.25.The method was
validated according to ICH guidelines. It was found to be accurate and reproducible. Linearity
was obtained in the concentration range of 20-80 μg/ml . The percentage RSD for precision and
accuracy of the method was found to be less than 2%. The proposed method can be successfully
applied in the quality control of bulk and pharmaceutical dosage forms.
Keywords:, Liraglutide ,RP-HPLC, Validation
*Corresponding Author Email: susenaswrk@gmail.com
Received 10 April 2013, Accepted 14 May 2013
Journal home page: http://www.ajptr.com/
2. Susena et. al., Am. J. PharmTech Res. 2013; 3(3) ISSN: 2249-3387
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INTRODUCTION
Liraglutide is a long-acting glucagon-like peptide-1 (GLP-1) analog that has been developed by
Novo Nordisk for the treatment of type2 diabetes. The product was approved by the European
Medicines Agency (EMA) on July 3, 2009, and by the U.S. Food and Drug Administration
(FDA) on January 25, 2010.
Liraglutide intended to help lower blood sugar levels along with diet, exercise, and selected other
diabetes medicines. It is not recommended as initial therapy in patients who have not achieved
adequate diabetes control on diet and exercise alone. Liraglutide is an incretin mimetic. This
means that it mimics the actions of incretin hormones in the body. As an incretin mimetic,
liraglutide increases insulin production in response to meals and decreases the amount of glucose
(sugar) that the liver produces. The medicine also slows the emptying of food from the stomach
and decreases the amount of food that people eat.
Figure 1: Structure of Liraglutide
MATERIALS AND METHOD
Apparatus:
Waters HPLC 22695 series consisting 4 pump, Auto sampler, equipped with PDA detector,
thermostat column connected with waters (alliance) Empower software ,Inertsil ODS C18
column (250x4.6mm, 5μm in particle size), Ohaus weighing balance and bath sonicator, borosil
glass apparatus were used for experimental purpose.
Chemicals and reagents:
Liraglutide pure drug was obtained as a gift sample from HETERO LABS LIMITED.
Hyderabad. Methanol and phosphate Buffer (PH-5.5) were purchased from S.D. Fine (P) Ltd.
Mumbai. All chemicals and reagents used were of analytical HPLC grade.
Preparation of mobile phase:
Isocratic elution with Methanol: phosphate Buffer (PH-5.5) 85:15(V/V) was used at a flow rate
of 1.0ml/min. The mobile phase was prepared freshly and degassed by sonicating for 5 min
before use.
3. Nagariya et. al., Am. J. PharmTech Res. 2013; 3(3) ISSN: 2249-3387
3 www.ajptr.com
Preparation of standard and test solutions
Liraglutide standard stock solution:
10 mg Liraglutide was accurately weighed and dissolved in 10 ml methanol then transferred to a
10 ml volumetric flask sonicate it for 5 min, finally volume was made up to the mark with
methanol to make 1000μg/ml stock solution.
Working solution:
1ml of the above stock solution was pipetted into a 10ml volumetric flask and diluted up to the
mark with HPLC grade Methanol. The contents were mixed well and filtered through 0.45μm
nylon filter paper to get this stock solution (100 μg/ml).
Preparation of sample solution:
For the analysis of the dosage form, Liraglutide in injection form manufactured by novonordisk
Ltd. was Selected. By using Liraglutide injection 1.7ml(i.e.10mg)of solution is transferred to
10ml volumetric flask finally volume was made up to the mark with methanol to make
1000μg/ml sample solution
Method validation
The method was validated in accordance with ICH guidelines17. The parameters assessed were
linearity, accuracy, and limit of detection (LOD), limit of quantification (LOQ), precision,
reproducibility and robustness.
RESULTS AND DISCUSSIONS
Linearity
The calibration curve obtained by plotting peak area against concentration showed linearity in
the concentration range of 20-80 μg/ml Linear regression data for the calibration curves are
given in Figure 2.
Figure 2: Linear regression data for the calibration curve
0
1000000
2000000
3000000
4000000
5000000
6000000
7000000
8000000
0 20 40 60 80 100
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Accuracy
The % mean recovery obtained for Liraglutide was 101% .The %RSD is less than 2, results were
given in Table 1.
Table 1: Accuracy data for proposed method
Spiked level of
drug (%)
Amount of drug
added (μg/ml)
Amount of drug
found (μg/ml)
%
Recovery
50 20 20.29 105.0
100 40 40.2 101.0
150 60 60.7 98.0
Detection limit and quantification limit
LOD for Liraglutide was 0.24 μg/ml respectively, while LOQ was 0.72 μg/ml
Precision
Results for repeatability expressed as %RSD, results were given in Table 2. The low values of
%RSD indicate that the method is precise. Reproducibility was checked by analyzing the
samples by another analyst using same instrument and same laboratory. There was no significant
difference between the %RSD values, which indicates that the proposed method was
reproducible, results were showed in Table 2.
Table 2: Precision of the proposed HPLC method
Conc. of Liraglutide
(40 μg/ml)
Peak area of Liraglutide
Intra-day Inter-day
Injection-1 3218338 3318621
njection-2 3230606 3326451
Injection-3 3250591 3412131
Injection-4 3242511 3332153
Injection-5 3257321 3365143
Average 3239873.4 3350899.8
Standard Deviation 7802.8 14435.5
% RSD 0.2 0.4
Table 3: Results of robustness for proposed method
Factor Level Retention time Asymmetry
A: Flow rate (ml/min)
0.8 -0.2 3.90 1.34
1.0 0 3.25 1.32
1.2 +0.2 2.89 1.28
%RSD 0.3 0.7
B: % of methanol (ml)
84 -1 3.70 1.34
85 0 3.26 1.32
86 +1 3.10 1.28
%RSD 0.2 0.7
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Detection limit and quantification limit
LOD for Liraglutide was 0.24 μg/ml respectively, while LOQ was 0.72 μg/ml
Robustness
There was no significant change in the peak areas and retention times of Liraglutide, when the
composition of mobile phase ±1ml and flow rate was varied by ±0.2 ml. The results are showed
in Table 3.
Specificity
No interference from any of the excipients was found at retention times of the examined drugs.
In addition, the chromatogram of each drug in the sample solution was found identical to the
hromatogram received by the standard solution at the wavelengths applied. These results
demonstrate the absence of interference from other materials in the pharmaceutical formulations
and therefore confirm the specificity of the proposed method.
System suitability
The acceptance criteria are % RSD of peak areas and retention time less than 2%, theoretical
plates numbers (N) at least 4500 per each peak and tailing factors less than 1.5 for Liraglutide the
results are shown in the Table 4.
Table 4: System suitability parameters
Parameters Liraglutide
Linearity (μg/ml) 20.-80
Correlation coefficient 0.998
Theoretical plates 9248
Tailing factor 1.32
LOD (μg/ml) 0.24
LOQ (μg/ml) 0.72
Quantification of Liraglutide in parentral dosage form
The proposed method was applied to the estimation of Liraglutide in parentral dosage form. The
results of the assay 99.84±0.24%, of label claim of the injection. The assay results showed that
the method was selective for the estimation of Liraglutide without interference from the
excipients used in the injection form. The results are shown in the Table 5.
Table 5: Results of sample analysis for proposed method
Brand name Analyte Label claim per
injection (mg)
% Analyte
estimated
(mean±SD)
%RSD
VICTOZA Liraglutide 10 99.84±0.24 0.193
In order to achieve the estimation of the Liraglutide initial trials was performed with the
objective of selecting adequate and optimum chromatographic conditions. Parameters, such as
6. Susena et. al., Am. J. PharmTech Res. 2013; 3(3) ISSN: 2249-3387
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ideal mobile phase and their proportions, detection wave length and concentrations of the
standard solutions were carefully studied. Several solvents were tested in varying proportions.
Finally, a mixture of methanol: Phosphate buffer (85:15 v/v) was selected as the optimum mobile
phase. The optimized chromatographic conditions were selected based on sensitivity, retention
times and peak shape. The method was validated in terms of linearity, accuracy, precision, LOD,
LOQ, robustness and specificity as per ICH guidelines. The accuracy data shows that the method
is accurate within desired range. The LOD and LOQ values were low which indicates that the
method is sensitive. The method was robust as minor changes in the chromatographic parameters
did not bring about any significant changes in peak area and retention times of Liraglutide
Name Retention
Time
Area % Area Height USP
Tailing
Symmetry
Factor
USP Plate
Count
Liraglutide 3.259 3250591 100.00 374481 1.329972 1.339972 9283
Figure. 3: Typical chromatogram of Liraglutide standard
CONCLUSION
A validated RP-HPLC method has been developed for the determination of Liraglutide in
injection form. The proposed method is simple, rapid, accurate, precise and specific. Its
chromatographic run time of 10 min allows the analysis of a large number of samples in short
period of time. Therefore, it is suitable for the routine analysis of Liraglutide in pharmaceutical
dosage form. The limit of detection for Liraglutide was found to be 0.24 μg/ml and the limit of
quantification was found to be 0.72 μg/ml. It proves the sensitivity of method.
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