A new, simple sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Clopidogrel bisulphate was chromatographed on a reverse phase C18column (150 mm x 4.5 mm, i.d 5μm) in a mobile phase consisting of acetonitrile and phosphate buffer (pH: 3.0) in the ratio of 60:40 % v/v. The mobile phase was pumped at a flow rate of 1 ml/min with detection at 224 nm. The detector response was linear in the concentration of 50-150 μg /ml. The limit of detection and limit of quantitation was found to be 1.3 and 4.2 µg/ml, respectively. The intra and inter day variation was found to be less than 2%. The mean recovery of the drug from the solution was 99.79%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for routine quality control analysis of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Key words: Clopidogrel bisulphate, RP-HPLC, Validation, Accuracy, Precision.
Spectrophotometric Determination of Drugs and Pharmaceuticals by Cerium (IV) ...IOSR Journals
Simple, sensitive, accurate, and precise spectrophotometric methods for quantitative determination of drugs, viz., Darifenacin (DAR), Esmolol Hydrochloride (ESM), Montelukast Sodium (MON), Sildenafil citrate (SIL),Terbinafine (TER) and Tramadol Hydrochloride (TRA) were developed. The method of each drug depends upon oxidation of drugs by Ce (IV) (Excess) and estimating the amount of unreacted Ce (IV) by amaranth dye at 523nm. The calibration curves obeyed Beer’s law over the concentration range of 1.4-7.0 μg ml-1 (DAR), 2-14 μg ml-1 (ESM), 2-10 μg ml-1 (MON), 20-70 μg ml-1 (SIL), 3-21 μg ml-1 (TER) & 2-14 μg ml-1 (TRA). The methods have been validated in terms of guidelines of ICH and applied to analysis of pharmaceuticals.
Development and validation of a stability-indicating HPLC method for the simultaneous determination of Losartan potassium, hydrochlorothiazide, and their degradationproducts
Spectrophotometric Determination of Drugs and Pharmaceuticals by Cerium (IV) ...IOSR Journals
Simple, sensitive, accurate, and precise spectrophotometric methods for quantitative determination of drugs, viz., Darifenacin (DAR), Esmolol Hydrochloride (ESM), Montelukast Sodium (MON), Sildenafil citrate (SIL),Terbinafine (TER) and Tramadol Hydrochloride (TRA) were developed. The method of each drug depends upon oxidation of drugs by Ce (IV) (Excess) and estimating the amount of unreacted Ce (IV) by amaranth dye at 523nm. The calibration curves obeyed Beer’s law over the concentration range of 1.4-7.0 μg ml-1 (DAR), 2-14 μg ml-1 (ESM), 2-10 μg ml-1 (MON), 20-70 μg ml-1 (SIL), 3-21 μg ml-1 (TER) & 2-14 μg ml-1 (TRA). The methods have been validated in terms of guidelines of ICH and applied to analysis of pharmaceuticals.
Development and validation of a stability-indicating HPLC method for the simultaneous determination of Losartan potassium, hydrochlorothiazide, and their degradationproducts
Determination of Chloramphenicol in Bulk Drug and Pharmaceutical Dosage Forms...iosrphr_editor
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).
Simultaneous estimation of metformin hydrochloride and glibenclamide by rphpl...IJSIT Editor
A high performance reverse phase liquid chromatographic procedure is developed for simultaneous
estimation of Metformin hydrochloride and Glibenclamide in combined tablet dosage form. The method was carried
out on a Agilent Hypersil ODS (25cm x 4.6mm, i.d. 5µ) column with a mobile phase used consisting of acetonitrile:
mono basic sodium phosphate Buffer (50:50) and the pH of buffer was adjusted to 2.5 using 2M Orthophosphoric acid.
The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and
column oven temperature at 300C. The retention times of Metformin HCl & Glibenclamide were 2.709& 9.216 minutes
respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of
quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.
Notes* for the subject 'Advanced Pharmaceutical Analysis'Sanathoiba Singha
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis) 1st semester.
*not all topics have been included in this collection of notes.
Development and validation of GC-MS method for analysis of chloropyramine hyd...iosrphr_editor
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).
Analytical Method Development and Validation for the Estimation of Zolmitript...ijtsrd
In this work the authors have proposed a simple, specific, economic and accurate reverse phase liquid chromatographic method for the estimation of Zolmitriptan as an active pharmaceutical ingredient and in pharmaceutical formulation. The main objective of the current research paper is to To develop simple, precise and accurate RP HPLC method for Zolmitriptan also to validate the developed method as per ICH guideline Q2R1 and to explore the applicability of the method in finished product formulation for estimation of Zolmitriptan during its lifecycle. The objective was achieved by optimized condition with Phonemenex C18 column 150mm×4.6mm , 5µm. And mobile phase Phosphate buffer pH 3.5 85 Methanol 15. The separation was done with a flow rate of 0.9ml min, detection with 224nm. The retention was found to be 3.57 minute. LOD and LOQ were found to be 2.45 and 7.42 respectively. So in order to obtain the correct results various validations methods are performed to get the results. The results obtained from those validation methods are plotted in the form of the charts as well as the different curves. Mr. Rahul M. Sagde | Mr. Pawan N. Karwa | Mr. Vivek M. Thorat | Sanjay S. Jadhav "Analytical Method Development and Validation for the Estimation of Zolmitriptan by RP HPLC Method" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-5 , August 2019, URL: https://www.ijtsrd.com/papers/ijtsrd26474.pdfPaper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/26474/analytical-method-development-and-validation-for-the-estimation-of-zolmitriptan-by-rp-hplc-method/mr-rahul-m-sagde
Method Development and Validation of Naftopidil by Reverse Phase-HPLC in Bulk...SriramNagarajan15
A new simple, accurate, rapid and precise isocratic High performance liquid chromatographic (HPLC) method was developed and validated for the determination of Etomidate (ETO) injection. The Method employs Waters HPLC system on Develosil –ods-UG column (300 x 3.9 mm x 5µm) and flow rate of 1.5 mL/min with a load of 20 µL. Acetonitrile and Phosphate buffer was used as mobile phase in the composition of 40:60. The Detection was carried out at 254 nm. Linearity ranges for Etomidate was 40-240 µg/ml respectively. Retention Time of Etomidate was found to be 12.061 minutes respectively. Percent recovery study values of Etomidate were found to be within 98-102 %. This newly developed method was successfully utilized for the Quantitative estimation of Etomidate in injectables. This method was validated for accuracy, precision, linearity and Robustness as per ICH guidelines.
Stability indicating method development and validation for the estimation of ...SriramNagarajan18
Stability indicating method development and validation for the estimation of Doxorubicin by using RP-HPLC method in a bulk and pharmaceutical dosage form
Validated RP-HPLC Method for the Determination of Nelaribine in Bulk and Tabl...ijtsrd
A novel, simple and economic reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the estimation of Nelaribine in bulk and tablet dosage form with greater precision and accuracy. Separation was achieved on Cosmiscil C18 column (150X4.6mm i.d.,5-µm) in isocratic mode using Triflouro acetic acid PH-3.6 buffer and Acetonitrile in the ratio of 90:10(v/v) as mobile phase, pumped in to the column at flow rate of 1.0 mL min-1and the detection of eluent from the column was carried out using variable wavelength UV detector at 248 nm. The total run time was 15 min and the column was maintained at ambient temperature. The retention time of Nelaribine was 4.003 min. The standard curves were linear over the concentration range of 25-150 -µg/ml with R2 0.999 and the LOD and LOQ values for Nelaribine were 0.04 -µg/ml and 0.12 -µg/ml , respectively. The percentage recovery was found to be 101.76 “ 98.72 %, the % RSD was found to be 0.43. The percentage amount of a marketed tablet formulation of Nelaribine was found to be 101.2 %. The method was validated as per ICH guidelines. Validation studies demonstrated that the proposed RP-HPLC method is simple, specific, rapid, reliable and reproducible. Hence the proposed method can be applied for the routine quality control analysis of Nelaribine in bulk and tablet dosage forms. Mrs.P.D.Chaithanya Sudha | Prof.D.Gowri Sankar"Validated RP-HPLC Method for the Determination of Nelaribine in Bulk and Tablet Dosage Form" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-1 | Issue-4 , June 2017, URL: http://www.ijtsrd.com/papers/ijtsrd181.pdf http://www.ijtsrd.com/pharmacy/analytical-chemistry/181/validated-rp-hplc-method-for-the-determination-of-nelaribine-in-bulk-and-tablet-dosage-form/mrspdchaithanya-sudha
Method development and validation of escitalopram and estizolam in tablet dos...SriramNagarajan19
A simple and selective LC method is described for the determination of Escitalopram oxalate and Etizolam 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 238 nm. Linearity was observed in the range 60-140 µg/ml for Escitalopram oxalate (r2 =0.999) and 6-14 µg /ml for Etizolam (r2 =0.996) 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.
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.
Analytical method development and validation for the estimation of quinapril ...SriramNagarajan19
A simple and selective LC method is described for the determination of Quinapril and Tolcapone tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a Mixed Phosphate buffer (KH2PO4 +K2HPO4): Acetonitrile 40:60, with detection of 239 nm. Linearity was observed in the range 50 - 150 µg /ml for Quinapril (r2 =0.995) and 62.5- 187.5µg /ml for Tolcapone (r2 =0.999) 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.
Determination of Chloramphenicol in Bulk Drug and Pharmaceutical Dosage Forms...iosrphr_editor
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).
Simultaneous estimation of metformin hydrochloride and glibenclamide by rphpl...IJSIT Editor
A high performance reverse phase liquid chromatographic procedure is developed for simultaneous
estimation of Metformin hydrochloride and Glibenclamide in combined tablet dosage form. The method was carried
out on a Agilent Hypersil ODS (25cm x 4.6mm, i.d. 5µ) column with a mobile phase used consisting of acetonitrile:
mono basic sodium phosphate Buffer (50:50) and the pH of buffer was adjusted to 2.5 using 2M Orthophosphoric acid.
The detection of the combined dosage form was carried out at 228 nm and a flow rate employed was 1 ml/min and
column oven temperature at 300C. The retention times of Metformin HCl & Glibenclamide were 2.709& 9.216 minutes
respectively. The developed method was validated in terms of accuracy, precision, linearity, limit of detection, limit of
quantification as per ICH norms. The proposed method can be used for the estimation of these combined drugs.
Notes* for the subject 'Advanced Pharmaceutical Analysis'Sanathoiba Singha
As per the syllabus prescribed by Rajiv Gandhi University of Health Sciences, Karnataka, for M. Pharm (Pharmaceutical Analysis) 1st semester.
*not all topics have been included in this collection of notes.
Development and validation of GC-MS method for analysis of chloropyramine hyd...iosrphr_editor
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).
Analytical Method Development and Validation for the Estimation of Zolmitript...ijtsrd
In this work the authors have proposed a simple, specific, economic and accurate reverse phase liquid chromatographic method for the estimation of Zolmitriptan as an active pharmaceutical ingredient and in pharmaceutical formulation. The main objective of the current research paper is to To develop simple, precise and accurate RP HPLC method for Zolmitriptan also to validate the developed method as per ICH guideline Q2R1 and to explore the applicability of the method in finished product formulation for estimation of Zolmitriptan during its lifecycle. The objective was achieved by optimized condition with Phonemenex C18 column 150mm×4.6mm , 5µm. And mobile phase Phosphate buffer pH 3.5 85 Methanol 15. The separation was done with a flow rate of 0.9ml min, detection with 224nm. The retention was found to be 3.57 minute. LOD and LOQ were found to be 2.45 and 7.42 respectively. So in order to obtain the correct results various validations methods are performed to get the results. The results obtained from those validation methods are plotted in the form of the charts as well as the different curves. Mr. Rahul M. Sagde | Mr. Pawan N. Karwa | Mr. Vivek M. Thorat | Sanjay S. Jadhav "Analytical Method Development and Validation for the Estimation of Zolmitriptan by RP HPLC Method" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-5 , August 2019, URL: https://www.ijtsrd.com/papers/ijtsrd26474.pdfPaper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/26474/analytical-method-development-and-validation-for-the-estimation-of-zolmitriptan-by-rp-hplc-method/mr-rahul-m-sagde
Method Development and Validation of Naftopidil by Reverse Phase-HPLC in Bulk...SriramNagarajan15
A new simple, accurate, rapid and precise isocratic High performance liquid chromatographic (HPLC) method was developed and validated for the determination of Etomidate (ETO) injection. The Method employs Waters HPLC system on Develosil –ods-UG column (300 x 3.9 mm x 5µm) and flow rate of 1.5 mL/min with a load of 20 µL. Acetonitrile and Phosphate buffer was used as mobile phase in the composition of 40:60. The Detection was carried out at 254 nm. Linearity ranges for Etomidate was 40-240 µg/ml respectively. Retention Time of Etomidate was found to be 12.061 minutes respectively. Percent recovery study values of Etomidate were found to be within 98-102 %. This newly developed method was successfully utilized for the Quantitative estimation of Etomidate in injectables. This method was validated for accuracy, precision, linearity and Robustness as per ICH guidelines.
Stability indicating method development and validation for the estimation of ...SriramNagarajan18
Stability indicating method development and validation for the estimation of Doxorubicin by using RP-HPLC method in a bulk and pharmaceutical dosage form
Validated RP-HPLC Method for the Determination of Nelaribine in Bulk and Tabl...ijtsrd
A novel, simple and economic reverse phase high performance liquid chromatography (RP-HPLC) method has been developed for the estimation of Nelaribine in bulk and tablet dosage form with greater precision and accuracy. Separation was achieved on Cosmiscil C18 column (150X4.6mm i.d.,5-µm) in isocratic mode using Triflouro acetic acid PH-3.6 buffer and Acetonitrile in the ratio of 90:10(v/v) as mobile phase, pumped in to the column at flow rate of 1.0 mL min-1and the detection of eluent from the column was carried out using variable wavelength UV detector at 248 nm. The total run time was 15 min and the column was maintained at ambient temperature. The retention time of Nelaribine was 4.003 min. The standard curves were linear over the concentration range of 25-150 -µg/ml with R2 0.999 and the LOD and LOQ values for Nelaribine were 0.04 -µg/ml and 0.12 -µg/ml , respectively. The percentage recovery was found to be 101.76 “ 98.72 %, the % RSD was found to be 0.43. The percentage amount of a marketed tablet formulation of Nelaribine was found to be 101.2 %. The method was validated as per ICH guidelines. Validation studies demonstrated that the proposed RP-HPLC method is simple, specific, rapid, reliable and reproducible. Hence the proposed method can be applied for the routine quality control analysis of Nelaribine in bulk and tablet dosage forms. Mrs.P.D.Chaithanya Sudha | Prof.D.Gowri Sankar"Validated RP-HPLC Method for the Determination of Nelaribine in Bulk and Tablet Dosage Form" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-1 | Issue-4 , June 2017, URL: http://www.ijtsrd.com/papers/ijtsrd181.pdf http://www.ijtsrd.com/pharmacy/analytical-chemistry/181/validated-rp-hplc-method-for-the-determination-of-nelaribine-in-bulk-and-tablet-dosage-form/mrspdchaithanya-sudha
Method development and validation of escitalopram and estizolam in tablet dos...SriramNagarajan19
A simple and selective LC method is described for the determination of Escitalopram oxalate and Etizolam 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 238 nm. Linearity was observed in the range 60-140 µg/ml for Escitalopram oxalate (r2 =0.999) and 6-14 µg /ml for Etizolam (r2 =0.996) 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.
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.
Analytical method development and validation for the estimation of quinapril ...SriramNagarajan19
A simple and selective LC method is described for the determination of Quinapril and Tolcapone tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a Mixed Phosphate buffer (KH2PO4 +K2HPO4): Acetonitrile 40:60, with detection of 239 nm. Linearity was observed in the range 50 - 150 µg /ml for Quinapril (r2 =0.995) and 62.5- 187.5µg /ml for Tolcapone (r2 =0.999) 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 Reversed Phase-High-Performance Liquid Chromato...BRNSS Publication Hub
A simple, accurate, precise, and robust in vitro methods developed and validated for measurement of drug release in Aminocaproic Acid tablets. High-performance liquid chromatography (HPLC) method for quantification of drug in dissolution samples of Aminocaproic Acid tablet is developed and validated. 0.1 N Hydrochloric acid is used as dissolution medium and Basket (USP-I) as apparatus at 100 rpm. The sample was withdrawn after 60 min. The developed HPLC method was used for quantitative estimation of drug release in dissolution samples of Aminocaproic Acid tablet. Chromatogram was run through Inertsil ODS 3V, (250 × 4.6 mm), 5 μm. Mobile phase containing buffer solution and methanol in the pumped through column at a flow rate of 1 ml/min. Buffer used in this method was 13.3 g sodium dihydrogen phosphate monohydrate, 500 mg of Heptane-1-sulfonic acid sodium salt, and 1.0 mL of Triethylamine buffer with pH 2.20 adjusted by orthophosphoric acid. Optimized wavelength for Aminocaproic acid was 210 nm. Retention time of Aminocaproic acid was found about 4.0 min; linearity range was 132.605 μg/ml–828.787 μg/ml. The new method was evaluated according to ICH guideline and as far as validation results are concern correlation coefficient value was 0.9999 for the very compound, percentage recovery 100.0%, repeatability results relative standard deviation 0.9 for Aminocaproic acid. The developed HPLC method was found to be a simple and rapid one for regular analysis in professional laboratory.
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.
Dissolution Method Validation with Reverse Phase Chromatographic Method for D...BRNSS Publication Hub
The present analytical work is a unique method development and validation for the determination of dissolution of Eltrombopag using reverse phase high-performance liquid chromatography (HPLC) with isocratic elution technique. HPLC method for quantification of drug in dissolution samples of Eltrombopag tablet is developed and validated. About 0.5% polysorbate 80 in phosphate buffer of pH −6.8 is used as dissolution medium and paddle (USP-II) as apparatus at 50 rpm. The sample was withdrawn after 45 min. The developed HPLC method was used for quantitative estimation of drug release in dissolution samples of Eltrombopag tablet. Here, the stationary phase used was Xbridge C18 (50 mm × 4.6 mm × 5 μm), mobile phase was 25% ammonium formate and 75% acetonitrile. pH of the buffer solution was maintained at 3.0, flow rate 1.0 ml/min. Eluted material underwent for monitoring at the detector wavelength of 230 nm. Retention time for Eltrombopag was found to be 2.16 min; and linearity range was 3.516 µg/mL–131.862 µg/mL. The new method was evaluated according to the ICH guideline and as far as validation results are concern correlation coefficient value that was 1.0000 for the compound, percentage recovery 99.4%, and repeatability results relative standard deviation 0.6 for Eltrombopag. The developed HPLC method was found to be a simple and rapid one for regular analysis in professional laboratory.
Formulation, characterization and Evaluation of Transdermal Film Containing N...SriramNagarajan15
Transdermal drug delivery system has numerous advantages over the more traditional drug delivery systems. This includes high bioavailability, steady drug plasma concentration, absence of first pass hepatic metabolism effect. Transdermal film is an adhesive film that has a coating of a drug that is placed on the skin to deliver a specific dose of the drug into the bloodstream over a period. The aim of present study an attempt was made to design the transdermal drug delivery system of naproxen with Ethyl Cellulose polymer in various concentrations. Transdermal films were prepared by solvent casting method by using Dibutylpthalate as plasticizer. The prepared films were characterized in physical appearance, thickness, drug content, weightvaration, Folding endurance, percentage moisture uptake and in-vitro release study.
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.
Antibacterial activity on leaf extracts of Syzgium jambalonamSriramNagarajan15
The purpose of this investigation was to extract the bioactive agents from the Methanol, Acetone extracts were examined for their activities against pathogenic microorganism (Proteus vulgaris, Staphyloccus aureus, Bacillus subtilis and E.coli). The most of the incidence of infections caused by pathogenic microorganism in our routine life and the importance of using novel synergistic drug has become important. In the present study enhanced inhibitory effects were achieved by employing solvent extracts of Syzgium jambalonam. These MIC were compared with well known antibacterial plant of Neem extract (Biological source-Azadirachta indica, Family-Meliaceae).
Bilayer tablet is new era for the successful development of controlled release formulation along with various features to provide a way of successful drug delivery system. Bi-layer tablets developing a combination of two or more Active Pharmaceutical Ingredients (API) in a single dosage form (bilayer tablet) has increased in the pharmaceutical industry, promoting patient convenience and compliance. For a variety of reasons: patent extension, therapeutic, marketing to name a few. To reduce capital investment, quite often existing but modified tablet presses are used to develop and produce such tablets. This article explains why the development and production of quality bi-layer tablets needs to be carried out on purpose-built tablet presses to overcome common bi-layer problems, such as layer-separation, insufficient hardness, inaccurate individual layer weight control, cross-contamination between the layers, reduced yield, etc. Using a modified tablet press may therefore not be your best approach to producing bilayer tablet under GMP-condition. Especially when in addition high production output is required.
Spectrophotometric Estimation of Rosuvastatin Calcium in Bulk and Pharmaceuti...SriramNagarajan15
Rosuvastatin calcium of the class statins is used for primary hyperlipidemias. It is a selective and competitive inhibitor of HMG-CoA reductase. In the present work, simple, sensitive and economic spectrophotometric method has been developed for quantitative determination of Rosuvastatin calcium. In the present spectrophotometric method Rosuvastatin calcium was dissolved in double distilled water. It exhibited an absorption maximum at 241 nm and obeyed Beer’s law in the concentration range of 5-25g/ml. The results of analysis have been validated and found to be sensitive, precise and accurate for quantitative determination of Rosuvastatin calcium in bulk drug and pharmaceutical formulations.
Analytical method development and its application to extractive spectrophotom...SriramNagarajan15
The reagent was synthesized and characterization was carried out by FTIR, NMR, elemental analysis as well as Mass spectrometry. The synthesized reagent was then applied for the development of the analytical method for the extractive spectrophotometric determination of cobalt (II). Cobalt metal forms pale yellow coloured complex, which can be extracted in chloroform at pH 9.4 having absorption maxima at 415 nm. Beer’s law is obeyed in the concentration range 1-8.00 μg. The molar absorptivity and Sandell’s Sensitivity of the extracted species are 7.1724 X 103 Lit mol-1 cm-2 and 8.2165 X 10-3μg cm-2 respectively. The developed method is highly sensitive, selective, simple, rapid, accurate, and has been satisfactorily applied for the determination of cobalt in the synthetic mixtures, pharmaceutical samples, and alloys.
Analytical Method Development and Validation of Dutasteride and Tamsulosin Hc...SriramNagarajan15
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Tom Selleck, an enduring figure in Hollywood. has captivated audiences for decades with his rugged charm, iconic moustache. and memorable roles in television and film. From his breakout role as Thomas Magnum in Magnum P.I. to his current portrayal of Frank Reagan in Blue Bloods. Selleck's career has spanned over 50 years. But beyond his professional achievements. fans have often been curious about Tom Selleck Health. especially as he has aged in the public eye.
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Introduction
Many have been interested in Tom Selleck health. not only because of his enduring presence on screen but also because of the challenges. and lifestyle choices he has faced and made over the years. This article delves into the various aspects of Tom Selleck health. exploring his fitness regimen, diet, mental health. and the challenges he has encountered as he ages. We'll look at how he maintains his well-being. the health issues he has faced, and his approach to ageing .
Early Life and Career
Childhood and Athletic Beginnings
Tom Selleck was born on January 29, 1945, in Detroit, Michigan, and grew up in Sherman Oaks, California. From an early age, he was involved in sports, particularly basketball. which played a significant role in his physical development. His athletic pursuits continued into college. where he attended the University of Southern California (USC) on a basketball scholarship. This early involvement in sports laid a strong foundation for his physical health and disciplined lifestyle.
Transition to Acting
Selleck's transition from an athlete to an actor came with its physical demands. His first significant role in "Magnum P.I." required him to perform various stunts and maintain a fit appearance. This role, which he played from 1980 to 1988. necessitated a rigorous fitness routine to meet the show's demands. setting the stage for his long-term commitment to health and wellness.
Fitness Regimen
Workout Routine
Tom Selleck health and fitness regimen has evolved. adapting to his changing roles and age. During his "Magnum, P.I." days. Selleck's workouts were intense and focused on building and maintaining muscle mass. His routine included weightlifting, cardiovascular exercises. and specific training for the stunts he performed on the show.
Selleck adjusted his fitness routine as he aged to suit his body's needs. Today, his workouts focus on maintaining flexibility, strength, and cardiovascular health. He incorporates low-impact exercises such as swimming, walking, and light weightlifting. This balanced approach helps him stay fit without putting undue strain on his joints and muscles.
Importance of Flexibility and Mobility
In recent years, Selleck has emphasized the importance of flexibility and mobility in his fitness regimen. Understanding the natural decline in muscle mass and joint flexibility with age. he includes stretching and yoga in his routine. These practices help prevent injuries, improve posture, and maintain mobilit
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Method Development and Validation of Clopidogrel Bisulphate by Reverse Phase-HPLC in Bulk and Pharmaceutical Dosage Forms
1. 1
* Corresponding author:
E-mail address: mouni.568@gmail.com
IJPAR |Volume 1 | Issue 1 | Dec - 2012
Available Online at: www.ijpar.com
[Research article]
Method Development and Validation of Clopidogrel Bisulphate by Reverse
Phase-HPLC in Bulk and Pharmaceutical Dosage Forms
*A.Mounika, N.Sriram
Smt. Sarojini Ramulamma College of Pharmacy, shesadrinagar, mahabubnagar-509001.
Andrapradesh, India,.
ABSTRACT
A new, simple sensitive, rapid, accurate and precise RP-HPLC method was developed for the estimation of
Clopidogrel bisulphate in bulk drug and pharmaceutical formulation. Clopidogrel bisulphate was
chromatographed on a reverse phase C18column (150 mm x 4.5 mm, i.d 5μm) in a mobile phase consisting of
acetonitrile and phosphate buffer (pH: 3.0) in the ratio of 60:40 % v/v. The mobile phase was pumped at a flow
rate of 1 ml/min with detection at 224 nm. The detector response was linear in the concentration of 50-150 μg
/ml. The limit of detection and limit of quantitation was found to be 1.3 and 4.2 µg/ml, respectively. The intra
and inter day variation was found to be less than 2%. The mean recovery of the drug from the solution was
99.79%. The proposed method is simple, fast, accurate, precise and reproducible hence, it can be applied for
routine quality control analysis of Clopidogrel bisulphate in bulk drug and pharmaceutical formulation.
Key words: Clopidogrel bisulphate, RP-HPLC, Validation, Accuracy, Precision.
INTRODUCTION
Clopidogrel is an oral, thienopyridine class
antiplatelet agent used to inhibit blood clots in
coronary artery disease, peripheral vascular
disease, and cerebrovascular disease. Clopidogrel is
a prodrug, the action of which may be related to an
ADP receptor on platelet cell membranes. The drug
specifically and irreversibly inhibits the P2Y12
subtype of ADP receptor, which is important in
activation of platelets and eventual cross-linking by
the protein fibrin. The blockade of this receptor
inhibits platelet aggregation by blocking activation
of the glycoprotein IIb/IIIa pathway. The IIb/IIIa
complex functions as a receptor, mainly for
fibrinogen and vitronectin but also for fibronectin
and von Willebrand factor. Activation of this
receptor complex is the "final common pathway"
for platelet aggregation and is important in the
cross-linking of platelets by fibrin.
Clopidogrel bisulphate is chemically (S)-(+)-
Methyl 2 - (2-chlorophenyl) -2- (6,7-dihydro-4H-
thieno [3,2-c] pyridin-5-yl) acetate hydrogen
sulfate[1].
The molecular formula of Clopidogrel
bisulphate is C16H16ClNO2S.H2SO4. The molecular
mass of is Clopidogrel bisulphate 419.03 g/mol. It
is an official drug in British Pharmacopoeia. It is
completely soluble in water, methyl alcohol, grain
alcohol and glacial acetic acid bit soluble in
acetone or chloroform[2].
The structure of
Clopidogrel was shown in fig 1.
Clopidogrel bisulphate was determined by HPLC
in normal mode [5]
and in reversed-phase ion pair
mode [15].
Clopidogrel bisulphate was also
determined in combination with other drugs like
2. 2
A.Mounica et al / Int. J. of Pharmacy and Analytical Research Vol-1(1) 2012 [1-7]
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aspirin [11]
and stability indicating HPLC of
Clopidogrel bisulphate [13]
and also by UV
spectrophotometric techniques [10,12,9],
and
impurities present in Clopidogrel[7,14]
and
potentiometric technique[6]
.
MATERIALS AND METHODS
Quantitative HPLC was performed on a isocratic
high pressure liquid chromatography (Waters
model 2695) Equipped with a photodiode array
detector capable of operating in the range of 190
nm to 400 nm Hypersil BDS C18 (150mm x
4.5mm, 5μm)
REAGENTS AND CHEMICALS
Sodium di hydrogen phosphate, ortho phosphoric
acid of AR grade, methanol of HPLC grade,
acetonitrile of HPLC grade and water HPLC grade
were obtained from Rankem Chemicals Ltd.,
Mumbai. Clopidogrel bisulphate was obtained as a
gift sample from Sun Pharma, India. The
commercially available Clopidogrel bisulphate
tablets were procured from the local market.
PREPARATION OF BUFFER SODIUM
DIHYDROGEN PHOSPHATE BUFFER (PH-
3.0)
Sodium dihydrogen phosphate buffer was prepared
by dissolving 158 gm of disodium hydrogen
Phosphate in 1000 ml of double distilled water and
the pH was adjusted to 3.0 with ortho-phosphoric
acid.
CHROMATOGRAPHIC CONDITIONS
The mobile phase consisting of acetonitrile and
sodium di hydrogen phosphate buffer (pH: 3.0) in
the ratio of 60:40 % v/v was filtered through 0.45μ
membrane filter before use, degassed and pumped
from the solvent reservoir into the column at a flow
rate of 1 ml/min. The detection was monitored at
224nm, and the run time was 20 minutes. The
volume of the injection loop was 10 μl and prior to
the injection of the drug solution; the column was
equilibrated for at least 30 minutes with the mobile
phase flowing through the system. The column and
the HPLC system were kept in 35°c temperature.
Stock standard solution of Clopidogrel bisulphate
was prepared by dissolving a quantity of
Clopidogrel bisulphate hydrochloride equivalent to
10.0 mg of Clopidogrel bisulphate in 10.0 mL of
diluent to obtain a solution having a known
concentration of 1.0 mg/mL Clopidogrel
bisulphate. Nominal (working) standard solution
was prepared by diluting 1 mL of stock standard
solution to 10 mL diluent to obtain a solution
having a known concentration of 100µg/mL
Clopidogrel bisulphate. Nominal solutions of the
formulated Clopidogrel bisulphate tablet solution
prepared by taking 75mg equivalent powder in 10
mL volumetric flask and dissolve with water from
that take 1.5 mL of solution transferred into 10 mL
volumetric flask and volume filled with water.
RESULTS
METHOD DEVELOPMENT
AC18 column (150mm x 4.5mm, 5μm) as a
stationary phase with a mobile phase of acetonitrile
and phosphate buffer pH3.0 (60:40, v/v) at a flow
rate of 1.0mL/min and a detection wavelength of
224 nm afforded the best separation of Clopidogrel
bisulphate. The standard solutions prepared as
above were injected into the 10 μl loop, and the
chromatogram was recorded as shown in fig 2. The
retention time of Clopidogrel was found to be
9.182 min. The calibration curve was constructed
by plotting concentration versus peak area ratio.
The amount of Clopidogrel present in the sample
was calculated through the standard calibration
curve.
ASSAY
Twenty tablets each containing 75 mg were
weighed accurately and powdered. A quantity
equivalent to10 mg of Clopidogrel was weighed
accurately and transferred to 10 ml volumetric flask
containing 3 ml of water. The contents were
sonicated for 20 min. and made up to the mark with
the water. The resulting solution is filtered through
13 mm × 0.45µm PVDF. 1.5mL of the above
solution was pipette into 10mL volumetric flask
and made up with water. The solution obtained was
diluted with the water to obtain a concentration in
the range of linearity previously determined for the
pure drug. The 10µl sample solution was injected
under the chromatographic conditions, and the
chromatogram was recorded. The amount of
Clopidogrel present in tablet formulation was
determined by comparing the peak area from the
standard. The results were furnished in Table 1.
METHOD VALIDATION
The linearity, precision, accuracy, limit of
detection, limit of quantitation, ruggedness and
robustness has been validated for the determination
of Clopidogrel. [3, 4]
3. 3
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LINEARITY AND RANGE
The linearity experiment was carried out in
triplicate to ascertain accuracy and precision of the
method. The standard curve was obtained in the
concentration range of 50-150 μg /ml The peak
area ratios of the drug versus concentration were
found to be linear, and the results are furnished in
Table 2. The linearity was evaluated by linear
regression analysis using the least square method.
It was found that correlation coefficient and
regression analysis are within the limits. The
linearity graph was shown in fig 3.
ACCURACY
Accuracy of the method was performed by
preparing the placebo of the drug formulation
according to the formulation procedure. To the
required quantity of placebo, a known quantity of
Clopidogrel with the same proportion as in the
drug, formulation was added to get three
concentrations (50, 100, 150 µg/mL of
Clopidogrel). Results have shown that the recovery
of Clopidogrel is within 98.0–102%, and the RSD
is lower than 2.0%. The results are shown in Table
3.
PRECISION
Repeatability
Repeatability of the method was evaluated by
calculating the RSD of the peak areas of six
replicate injections for the standard concentration
(100%) of Clopidogrel, which was found to be
0.43%.The results are furnished in Table 4.
Intermediate precision (ruggedness)
The Intermediate precision method was also
evaluated by analyzing six samples of Clopidogrel
by two analysts in the same laboratory using
different HPLC systems. Results of this study
showed that the RSD of the percentage of
Clopidogrel in Clopidogrel tablets for the 12
samples (6 samples from each analyst) was 0.8%
and 0.4% indicating a good intermediate precision
of the method Table 5.
LIMIT OF DETECTION (LOD) AND LIMIT
OF QUANTITATION (LOQ)
The LOD and LOQ for Clopidogrel were predicted
basing on the parameters of standard error of
estimate and slope, calculated from linearity of the
response data of Clopidogrel Bisulphate. The
results were shown in Table 6.
ROBUSTNESS
The robustness was checked by changing the flow
rate to 0.8 and 1.2 ml/ min, the mobile phase pH
2.8 to 3.2, and column oven temperature 30°c to
40°c the method suits best, and the results are
shown in Table 7.
Fig 1: Structure of Clopidogrel bisulphate
4. 4
A.Mounica et al / Int. J. of Pharmacy and Analytical Research Vol-1(1) 2012 [1-7]
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Fig 2.Chromatogram of Clopidogrel Bisulphate standard solution
Fig 3: Linearity graph for Clopidogrel Bisulphate
Table 1: Quantitative Estimation of Clopidogrel Bisulphate in tablet dosage form
Table 2: Linearity data of Clopidogrel bisulphate
S.
NO.
Tablet Sample
Label Claim in
mg/tablet
Peak Area
Amount found
mg/tablet
Percentage
content of DrugTest Standard
1
Clopidogrel
bisulphate
75 1229063 1515350 74.9 99.86
Concentration(µg/ml) Area
50 842089
75 1063739
100 1495425
125 1788165
150 2417255
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Table 3: Accuracy data of Clopidogrel Bisulphate
Sample Mean area counts Amt added
(µg/ml)
Amt recovered (µg/ml) %recovery Mean
50%-Rec-1 604982 50 49.9 99.8 99.86
50%-Rec-2 833740 50 50.1 100.2
50%-Rec-3 660589 50 49.8 99.6
100%-Rec-1 1518091 100 99.9 99.9 99.93
100%-Rec-2 1519697 100 99.8 99.8
100%-Rec-3 1525624 100 100.1 100.1
150%-Rec-1 2502382 150 149.8 99.8 99.6
150%-Rec-2 2517458 150 149.5 99.6
150%-Rec-3 2519699 150 149.2 99.4
Table 4: Repeatability data of Clopidogrel Bisulphate
Injection number Area of Clopidogrel bisulphate
1 1515163
2 1512512
3 1506778
4 1517826
5 1526474
6 1513348
Mean 1515350.17
SD 6564.30275
%RSD 0.433187186
Table 5: Ruggedness of Clopidogrel Bisulphate
S.No. System suitability
Observed value
Acceptance criteria
Analyst-1 Analyst-2
1
%RSD for Clopidogrel bisulphate in standard solution
0.4 0.8 NMT 2.0%
2 The Tailing factor 1.18 1.21 NMT 2.0
Table 6: LOD and LOQ data of Clopidogrel Bisulphate
S.NO Name LOD Value (µg/ml) LOQ Value (µg/ml)
1. Clopidogrel bisulphate 1.3 4.2
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Table 7: Robustness data of Clopidogrel bisulphate
CONCLUSION
The developed method is cheap, easy, and it gives
the sharp peak with high resolution. The developed
method is applied for the determination of
Clopidogrel bisulphate. The assay results are with
the label claim of the formulation. The developed
method is validated as per ICH guidelines using
parameters like Accuracy, Precision, Linearity, and
Range, Specificity, Ruggedness, LOD, LOQ and
Robustness. Hence the developed method is found
to be satisfactory, and it complies with all
validation parameters. So this developed method
can be used for the routine analysis of Clopidogrel
bisulphate in tablet dosage form.
REFERENCE
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Para meter Tailing factor %RSD
Buffer pH
2.8 1.17 0.3
3 1.18 0.8
3.2 1.21 0.4
Flow rate (ml/min)
0.8 1.22 1.1
1 1.18 0.7
1.2 1.25 0.2
Temperature(°C)
30 1.23 0.2
35 1.21 0.4
40 1.2 0.1
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