1. A new RP-HPLC method was developed and validated for the estimation of Clopidogrel bisulphate in bulk drug and pharmaceutical formulations.
2. The method involved using a C18 column, mobile phase of acetonitrile and phosphate buffer at a ratio of 60:40, and detection at 224 nm.
3. The method was found to be linear, precise, accurate, specific, robust and suitable for the routine analysis of Clopidogrel bisulphate in quality control labs.
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.
Patient compliance: Challenges in management of cardiac diseases in Kuala Lum...pharmaindexing
Background
The objective of this study was to investigate the degree of compliance among cardiac patients who attend the health facilities in Kuala Lumpur and Perak, Malaysia. The reasons for non-compliance and recommendations from healthcare professionals were also evaluated.
Method
A cross-sectional study of 400 patients and 100 healthcare professionals was carried out. This study utilizes variables on external factors and internal factors as the measurement tools. The questionnaire which consists of Morisky self-reported medication adherence questions was administered to patients and causes for non-compliance sought. Questionnaire for healthcare professionals was used to determine strategies that can improve compliance rate.
Results
The study revealed a 15.8% of high adherence rate, 54.3% of moderate adherence rate and 30% of poor adherence to cardiovascular disease medications. The chi-square tests showed the strong association between dependent and independent variables. The model chosen for testing the patient compliance through external and internal factors gives an R2 value of 85.0% with an adjusted R2 of 84.7%. The F value (317.187) was also significant (p=0.000) which means that the variables have better fit in the multivariate model. The major reasons determined for non-adherence were attitudes and beliefs, lifestyle, side effects and cost of medications. The study recommends that pharmacists and dispensing technicians should be adequately qualified to provide proper counselling to cardiac patients on their medicines and disease conditions.
Conclusion
The result of this study is of value to health care providers. Compliance to cardiovascular medications will avoid treatment failures encountered in therapy.
Overview on Recurrence Pregnancy Loss etiology and risk factorspharmaindexing
Recurrent pregnancy loss (RPL) can be defined as more than two to three consecutive miscarriages before 20 weeks’ gestation; it affects approximately 1% to 2% of women. RPL is a multifactorial disease. It is very important to study the etiology and risk factors of RPL to find the best diagnostic tests and suitable therapeutic intervention. This article will discuss the current understanding etiologies and risk factors of RPL.
Novel treatments for asthma: Corticosteroids and other anti-inflammatory agents.pharmaindexing
Asthma management is a challenge due to the prevalence of disease in the world. Based on the immunological and inflammatory mechanisms of asthma, corticosteroids and anti-inflammatory participate greatly in the treatment plan. Due to different reasons, there is still an unmet need to develop new agents in this field. A lot of compounds with anti-inflammatory effect are investigated in both pre-clinical and clinical studies.
A review on liver disorders and screening models of hepatoprotective agentspharmaindexing
The liver is a vital organ present in vertebrates and some other animals. It has a wide range of functions, including detoxification, protein synthesis, and production of bio chemicals necessary for digestion. The liver is necessary for survival; there is currently no way to compensate for the absence of liver function long term, although liver dialysis can be used short term.
Carbamazepine induced Steven Johnson syndrome: A case reportpharmaindexing
Drugs are the most common cause that induces Steven Johnson syndrome (SJS) and includes antiepileptic drugs, antiretroviral drugs, anti-tuberculosis drugs, Sulphonamides, fluoroquinolones, penicillins, non-Steroidal anti-inflammatory drugs, Multivitamins. The genetic markers are also the cause for carbamazepine induced Steven Johnson Syndrome. In our study, the antiepileptic drug (Carbamazepine) is the cause for Steven Johnson Syndrome. A female patient aged 25 years came to the hospital with the complaints of bubbling over the skin and all over the body with papillary vesicles associated with pain and irritation, fever, myalgia, and nausea. The patient is known case of Phenytoin induced Steven Johnson Syndrome. In this case the patient developed the Steven Johnson Syndrome approximately after one month after starting the carbamazepine.By the withdrawal of the drug, the condition of the patient was improved.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Monoherbal formulation development for laxative activitypharmaindexing
The Ayurvedic Pharmacopoeia specifically approves flaxseed as a poultice for boils externally and demulcent or laxative internally. In this study monoherbal formulation development for laxative activity of flaxseed was undertaken. The plantLinumusitatissimumhasshowed higher percentage of total ash as well as alcohol soluble extractive values. The aqueous extract of Linumusitatissimumwas prepared by using pilot scale extraction plant and spray drying unit. The qualitative phytochemical studies reveal the presence of amino acids, carbohydrates, vitamins and proteins. From the available literatures it was found that Linumusitatissimum contains more number of amino acids. The formulated tablets showed acceptable pharmacopoeial limits and complies with specifications for thickness, hardness, friability and weight variation. The formulation has showed better laxative activity indicating additive property of the combined phytoconstituents of the plant.
Pneumonia and respiratory failure from swine origin influenza H1n1pharmaindexing
Swine influenza (swine flu) became alarming health concern when World Health Organization declared as “public health emergency of international concern” on April 25, 2009. After documentation of human-to-human transmission of the virus in at least three countries of two WHO regions, the WHO raised the pandemic level to 6.1 During the 1918, flu pandemic infected one-third of the world's population (an estimated 500 million people) and caused approximately 50 million deaths.2 In 1976, an outbreak of swine influenza occurred in New Jersey, USA, which involved more than 200 cases, some of them severe, resulting in one death.3 In 1988, another fatality was reported as a complication of swine influenza.
A descriptive study on newborn care among postnatal mothers in selected mater...pharmaindexing
The newborn health challenge faced by India is more formidable than that experienced by any other country in the world. The newborn health is inevitably affected by the traditional care practices of the mothers causing high infant morbidity and mortality.The aim of the study were determine the knowledge, attitude and practice of postnatal mothers regarding new born care and find out the association between knowledge, attitude and practice of postnatal mothers regarding new born care and to determine the association between these as well as with the selected demographic variables. A descriptive study was conducted to assess the knowledge, attitude and practice of postnatal mothers regarding new born care in selected maternity centres in Madurai. Survey approach was employed to select sample and it consisted of 100 postnatal mothers. Data was collected using structured interview schedule. Findings of the study showed that 65% of postnatal mothers had moderate knowledge; 61% had favourable attitude and 57% of them had high practice of new born care. There was a significant association between knowledge and attitude (r=+0.567), knowledge and practice (r=+0.388), attitude and practice (r=+0.321) .There was a significant association between knowledge and education, monthly family income and obstetrical score at p<0.05. Findings of the study indicated the need to conduct frequent assessment of knowledge, attitude and practice of postnatal mothers regarding new born care. Awareness and attitude of the mothers towards new born care still has lots of lacunae especially in those who belong to the lower socio economic statusand poorly educated postnatal mothers. So it is imperative to provide comprehensive training in the field of new born care for mothers during pregnancy
Late 19th century was evident of intelligent biomaterial; which has changed researcher’s perspective towards science and technology. This intelligent biomaterial are envisioned to have huge impact on Healthcare from sequential signalling of biomedical molecule, mimicking natural gene, an effective drug carrier, to high resolution diagnostic tool.From drug discovery aspect many of NCE fail to reach therapeutic potential due to PK/ PD profile. Nanotechnology has changed the face of drug discovery form chemical evaluation to structure of proteins in signalling pathways and development of chemical antibody. Nanotechnology from lab to market approval is long process due to regulatory evaluation. Though it seems to be bright future market it has to go through a long process from being innovation to complete market product. This makes whole process expensive making investor reluctant to invest in big projects.Western world is aware of dramatic potential of nano-projects; which has its limitation in financial investments; with major challenge of transforming nano science to commercial pharmaceutical product.
The Flaws in health practice in post-operative management of a patient in ter...pharmaindexing
Introduction
Congenital urinary tract obstructions are common cause of kidney damage sometimes which sometimes presents itself without symptoms leading to abnormalities in blood filtration and consequently retarded kidney function. A cohort study was conducted in such patient to find out the short comings in treatment strategy.
Case presentation
A four years old child, weighing 14 kg was brought with severe constipation, fever, chest congestion and cough later developed left eye disorientation after admission to hospital, diagnosed with urinary tract obstruction, indicating acidosis and loss of electrolytes due to excessive loss of water. His therapy management included surgical treatment, dialysis and to improve his electrolyte levels within the normal with the treatment chest congestion and fever.
Conclusion
This case study reports the post operative treatment of congenital urinary tract obstructions in a tertiary care hospital and highlights the discrepancies observed. Antibiotic rationality and irrational prescribing was observed. The case study highlights the need of a clinical pharmacist in the health care team.
Corticosteroid induced disorders – An overviewpharmaindexing
Glucocorticoids are important in the treatment of many inflammatory, allergic, immunologic, and malignant disorders, and the toxicity of glucocorticoids is one of the commonest causes of iatrogenic illness associated with chronic inflammatory disease.Glucocorticoid-induced muscle atrophy is characterized by fast-twitch or type II muscle fiber atrophy. Corticosteroid (CS) therapy is widely used in the treatment of rheumatic diseases.Osteoporosis remains one of its major complications.Steroid induced glaucoma is a form of open angle glaucoma occurring as an adverse effect of corticosteroid therapy. Glucocorticoids induce hepatic and extrahepatic insulin resistance.Glucocorticoid treatment impairs both glucose transport in fat and muscle cells. Corticosteroid-induced psychosis represents a spectrum of psychological changes that can occur at any time during treatment. Cushing’s syndrome describes the signs and symptoms associated with prolonged exposure to inappropriately high levels of the hormone cortisol. Physicians must be aware of these adverse effects and be equipped to manage them.
Anti-inflammatory activity of pupalia lappacea L. Jusspharmaindexing
Pupalia lappacea (L) Juss is an erect shrub used in folklore medicine to treat bone fractures and in inflammatory conditions. Methanolic extract of aerial parts shown is claimed in traditional medicine that the leaves of the plant are used in the treatment of inflammation. In the present study, the methanolic extract of Pupalia lappacea was screened for its anti-inflammatory activity using carageenan induced rat paw edema egg white induced paw oedema models. The methanolic extract at the dose of 200 mg/kg p.o exhibited significant anti-inflammatory activity in carrageenan induced paw edema model (p<0.01). In egg white induced model, methanolic extract at the dose of 200 mg/kg inhibited paw oedema significantly (p<0.01) indicating that both test samples inhibit the increase in number of fibroblasts and synthesis of collagen and mucopolysaccharides during prostaglandin formation during the inflammation. These experimental results have established a pharmacological evidence for the folklore claim of the drug to be used as an anti inflammatory agent. HPTLC analysis of the extract shows the presence of gallic acid 1.24mg/ml, ferulic acid 2.00mg/ml, chlorogenic acid 46.25mg/ml and rutin 7.02mg/ml of the extract which were responsible for the claimed anti-inflammatory action in the animal models studied.
Lucinactant: A new solution in treating neonatal respiratory distress syndrom...pharmaindexing
Lucinactant is a novel synthetic surfactant, approved by the FDA on March 6th 2012, for use in treatment of RDS. It’s superiority as compared to the previously approved surfactants lie in containing sinapultide, a 21-amino acid peptide also known as KL4 peptide, which has been designed to mimic the activity of human surfactant protein. Lucinactant is completely devoid of any animal derived components. It is the fifth drug approved by the FDA for the treatment of RDS. It has shown immense efficacy in phase two clinical trials and animal model studies and exhibited better efficiency when compared to other surfactants in both 24 hour and two week mortality rates of infants in RDS. Lucinactant tends reduce the surface tension at the air-liquid interface of alveolar surfaces and allows lungs to function normally. It was observed that the side effects were lesser with Lucinactant when compared with other naturally derived surfactants.
Bioactivity screening of Soil bacteria against human pathogenspharmaindexing
Microorganisms have a profound effect on medical science as they not only infect & cause disease but also produce metabolic products that can cure infections. Soil happens to be a source for a variety of microorganisms. Most of the bacteria, particularly actinomycetes produce biologically active secondary metabolites. Though there are a number of antibiotics available, there is a pressing need for the discovery of new source for antimicrobials against the pathogens due to the development of drug resistance of the pathogenic microorganisms. In addition to, new pathogenic strains are also developing and causing infection to human beings. Bioactive compounds are compounds that are produced by any living organism and are known to exhibit various biological activities both in-vitro & in-vivo. Bioactivity may be antimicrobial, antineoplastic, anticancerous, immunomodulation, antifertility & others. Soil bacteria were isolated by standard technique and by making use of selective media. The isolates were identified and subjected for preliminary screening to look for their ability to produce bioactive materials. A total of 96 strains were isolated from three different soil samples. 14 of them were found to have antibacterial activity against the human pathogens like Staphylococcus aureus, Streptococcus faecalis, E.coli, Klebsiella aerogenes, Proteus vulgaris, Pseudomonas aureginosa and Salmonella typhi by preliminary screening. Further the selected (3) bacteria were grown in the suitable culture media for the production of bioactive metabolites by using rotary shake flask. The active metabolites was isolated by solvent extraction and concentrated by evaporation under reduced pressure. The antimicrobial screening of the active metabolites showed prominent effect against the clinical pathogens under the study.
A study on sigmoid Volvulus presentation and managementpharmaindexing
A study on sigmoid volvulus presentation and management was a 2yr retrospective study done at RMMCH.The diagnosis of sigmoid volvulus was made from a history of large bowel obstruction (constipation, abdominal distension, and abdominal pain), which were often recurrent and plain abdominal radiographs.The morbidity associated isSuperficial wound infection occurred in four patients. All the infected wounds eventually healed with conservative measures. Clinical anastomotic dehiscence was noted in 1 patient for which during relaparotomy proximal colostomy and mucous fistula was done. The mortality associated is shown is there were 9 deaths of which 7 were due to sepsis and 2 were due to comorbid illness. Two out of eight patients for whom a colopexy was done had a recurrent attack of sigmoid volvulus. The duration of hospital stay ranged between 10 and 21 days. Use of sigmoidoscopic detorsion for viable colon should be encouraged. Sigmoidopexy, which is associated with a recurrence rate of 20% in our series of patients, should be used selectively.Hartmann’s procedure is a safe option in sigmoid volvulus with gangrenous bowel. Primary anastomosis in emergency situation can be carried out with morbidity and mortality in patients with viable colon
Evaluation of Preliminary phytochemical on various some medicinal plantspharmaindexing
The present study was carried out to evaluate the physical status and percentage yield of methanolic extract and its fractions of whole plant of Leucas cephalotes, leaves of Hiptage benghalensis and leaves of Kydia calycina were recorded for future references and Preliminary phytochemical screening of MLC, MHB and MKC revealed the presence of carbohydrates, glycosides, saponins, flavonoids, steroidal and phenolic compounds. MLC revealed the presence of all the above mentioned phytoconstituents except saponins and also MKC steroidal compounds. The fractions of MLC, MHB and MKC revealed the presence of glycosides, phenolic compounds, steroids and flavonoids.
Comparision of in vitro antibacterial activity of cefoperazone and levofloxac...pharmaindexing
Cefoperazone (a third generation cephalosporin) has effective in vitro activity against majority of pathogens. Levofloxacin (a flouroquinolone) is one which prescribed more due to its increased antibacterial activity against Gram-positive, Gram-negative, and atypical bacteria. Microbial resistance to antibiotics is now prevalent and poses a serious clinical threat. An attempt has been made to evaluate sensitivity of Cefoperazone and Levofloxacin against Escherichia coli, Staphylococcus aureus, Pseudomonas aeruginosa and Salmonella typhi. A total of 120 isolates were collected from different pathological laboratories and medical centers in Karachi, Pakistan. The above stated clinical isolates were extracted from urine/stool, skin, blood and sputum samples. Results show least resistance of Levofloxacin as compare to Cefoperazone against Escherichia coli (32.5% and 42.5%) and Pseudomonas aeruginosa (36% and 48%) while Staphylococcus aureus is still susceptible towards Cefoperazone and least sensitive to Levofloxacin by showing 26.6% and 50% resistance respectively. Study concluded that the prevalent pathogens are still susceptible towards Levofloxacin and Cefoperazone but the gradual increase in resistance is alarming to the general practice of prescribing antibiotic which require routine evaluation and surveillance to ensure the effectiveness of the antibacterial agents.
Concept of srotas from ayurvedic perspective with special reference to neurologypharmaindexing
Ayurveda is a life science. The researchers of ayurveda could rule out the presence of srotas (channels) spreading throughout the human body. These srotas (channels) are governed by vayu which is using all the srotas (channels) of the body to carry out the functional and physiological activities of the human body without which the human society will not exist. Several synonymous words have been described by the ayurvedicacharyas for srotas. Some are micro and some are macro in structures and they adopt the same colour of the particular dhatus of the body to which it belongs. The aim of the study is to justify that srotas are nothing but innurmerable channels or pathways of the nervous system governed by electric current without which no functional and physiological activities of the human body will develope.
Health promotion survey in overweight and obese students of universities in n...pharmaindexing
Introduction
Overweight and obesity is one of the major health problems in the UK and worldwide. Approximately two-thirds of the population in the UK is either overweight or obese. Overweight and obesity is an important issue that causes distress to most women. Health promotion is the best method to educate overweight and obese women. It is defined as the process enabling people to increase control over and to improve their health by Ottawa Charter for Health Promotion. It is aimed to enhance the well-being of the individuals and their positive attitudes towards prevention of various diseases. In order to make any improvement to the health promotion for overweight and obesity, the risk factors and the opinions from the public should first be identified and addressed.
Methods
Cross-sectional survey design was selected with a questionnaire that consisted of 20 open and close ended questions. A sample size of 196 was determined. The data thus gathered was analyzed using SPSS V20 (Statistical Package for Social Science version 20). Descriptive statistics (fx) and (SD) were used and Chi-square X2 test for association was employed.
Results
Out of the total 196 responses, only (40%) of the students had normal weight (SD 1.1), (25%) students had a good understanding of health promotion (SD 1.6), half (50%) appeared concerned about their weight (SD 0.5), (60%) had an obese family member (0.5). The BMI of students was associated with the presence of an obese member in their family and their weight as a concern for them. (P-value <0.05).
Conclusion
The health promotion service is beneficial as it was found to have raised concerns in the mind of the students regarding over weight and obesity. However it was observed that the understanding of health promotion service was different among students and this is the root of the problem.
Report Back from SGO 2024: What’s the Latest in Cervical Cancer?bkling
Are you curious about what’s new in cervical cancer research or unsure what the findings mean? Join Dr. Emily Ko, a gynecologic oncologist at Penn Medicine, to learn about the latest updates from the Society of Gynecologic Oncology (SGO) 2024 Annual Meeting on Women’s Cancer. Dr. Ko will discuss what the research presented at the conference means for you and answer your questions about the new developments.
Ethanol (CH3CH2OH), or beverage alcohol, is a two-carbon alcohol
that is rapidly distributed in the body and brain. Ethanol alters many
neurochemical systems and has rewarding and addictive properties. It
is the oldest recreational drug and likely contributes to more morbidity,
mortality, and public health costs than all illicit drugs combined. The
5th edition of the Diagnostic and Statistical Manual of Mental Disorders
(DSM-5) integrates alcohol abuse and alcohol dependence into a single
disorder called alcohol use disorder (AUD), with mild, moderate,
and severe subclassifications (American Psychiatric Association, 2013).
In the DSM-5, all types of substance abuse and dependence have been
combined into a single substance use disorder (SUD) on a continuum
from mild to severe. A diagnosis of AUD requires that at least two of
the 11 DSM-5 behaviors be present within a 12-month period (mild
AUD: 2–3 criteria; moderate AUD: 4–5 criteria; severe AUD: 6–11 criteria).
The four main behavioral effects of AUD are impaired control over
drinking, negative social consequences, risky use, and altered physiological
effects (tolerance, withdrawal). This chapter presents an overview
of the prevalence and harmful consequences of AUD in the U.S.,
the systemic nature of the disease, neurocircuitry and stages of AUD,
comorbidities, fetal alcohol spectrum disorders, genetic risk factors, and
pharmacotherapies for AUD.
MANAGEMENT OF ATRIOVENTRICULAR CONDUCTION BLOCK.pdfJim Jacob Roy
Cardiac conduction defects can occur due to various causes.
Atrioventricular conduction blocks ( AV blocks ) are classified into 3 types.
This document describes the acute management of AV block.
- Video recording of this lecture in English language: https://youtu.be/lK81BzxMqdo
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- Link to NephroTube social media accounts: https://nephrotube.blogspot.com/p/join-nephrotube-on-social-media.html
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Tom Selleck Health: A Comprehensive Look at the Iconic Actor’s Wellness Journeygreendigital
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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The prostate is an exocrine gland of the male mammalian reproductive system
It is a walnut-sized gland that forms part of the male reproductive system and is located in front of the rectum and just below the urinary bladder
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A healthy human prostate measures (4cm-vertical, by 3cm-horizontal, 2cm ant-post ).
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Generalised disease of the prostate due to hormonal derangement which leads to non malignant enlargement of the gland (increase in the number of epithelial cells and stromal tissue)to cause compression of the urethra leading to symptoms (LUTS
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]
www.ijpar.com
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
A.Mounica et al / Int. J. of Pharmacy and Analytical Research Vol-1(1) 2012 [1-7]
www.ijpar.com
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
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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
[1] United states pharmacopeia, National Formulary 25 volume 32, 2005 p.no 1802
[2] The merck index, twelfth edition p. no 406
[3] Validation of analytical procedure, methodology as per ICH harmonized tripartite guidelines 1996,
Q2A having reached step 4 of the ICH process at the ICH steering committee meeting on 27th
October ,
1994, pg.no.1-8.
[4] Ludwig Huber. Validation and Qualification in Analytical Laboratories, Second Edition, Germany,
2007 pg no 160-170
[5] G. Radha Krishna Reddy, Prof. V. Surya Narayana Rao, Jayam Naga Sateesh, Development and
validation of stability indicating related Substances method for clopidogrel bisulphate drug substance
by normal phase hplc, Journal of Global Trends in Pharmaceutical Sciences Vol.2, Issue 4, (2011) pp -
367-379
[6] Amr lotfy saber, Mohmed alaa elmosallamy, Alaa alside ami and Hamada mohmed ahmed Killa,
Liquid Chromatographic and Potentiometric Methods For Determinations of Clopidogrel, Journal of
Food and Drug Analysis, Vol. 16, No. 2,(2008) , Pages 11-18
[7] D. Antić, S. Filipić, and D. Agbaba, A simple and sensitive tlc method for determination of
clopidogrel and its impurity SR 26334 in pharmaceutical products, Acta chromatographica, (2007) p.
no. 18.
[8] Venkanna Bayya, Sreedhara Chaganty, M. Ajitha, A rapid and rugged bio analytical method
Development and validation of clopidogrel in Human plasma using liquid chromatography/ Tandem
mass spectrometry, American journal of pharmaceutical research volume 1, issue 2, (2011).
[9] Saadet dermiş and Ekrem aydoğan, Rapid and accurate determination of clopidogrel in Tablets by
using spectrophotometric and Chromatographic techniques, commun.fac.sci.univ.ank.series b v.55 (1)
(2009) p no. 1-16,.
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
7. 7
A.Mounica et al / Int. J. of Pharmacy and Analytical Research Vol-1(1) 2012 [1-7]
www.ijpar.com
[10] Pravin B. Cholke, Raihan Ahmed, S. Z. Chemate1 and K. R. Jadhav, Development and Validation of
Spectrophotometric Method for Clopidogrel bisulfate in pure and in film coated tablet dosage form,
Scholars Research Library Archives of Applied Science Research, 4 (1)(2012), Pg.no 59-64.
[11] Getu Kahsay, Ann Van Schepdael, Erwin Adams, Development and validation of a liquid
chromatographic method for purity control of clopidogrel–acetylsalicylic acid in combined oral dosage
forms, Journal of Pharmaceutical and Biomedical Analysis, volume 61,( 2012) pg no 271– 276.
[12] Suhas Gurav, R. Venkatamahesh, Development and Validation of Derivative UVSpectropotometric
Methods for Quantitative Estimation of Clopidogrel in Bulk and Pharmaceutical Dosage For,
International Journal of ChemTech Research, Vol.4, No.2, (2010), pp 497-50.
[13] Sanjay D.Renapurkar Dr. U.C.Mashelkar, A LCMS Compatible Stability-Indicating HPLC Assay
Method for Clopidogrel bisulphate, International Journal of ChemTech Research Vol.2, No.2 (2010),
pp 822-829.
[14] P. Aparnaa, Sumathi V. Raoa, K. M. Thomasa,K. Mukkantib and Kishore Deoc, Non chiral High
Performance Liquid Chromatography method for monitoring unknown impurities generated during
stability of Clopidogrel tablets, Scholars Research Library s2(4),(2010), pp 244-252.
[15] Sagar S.Panda, Ion-Pairing RP-HPLC Method for Simultaneous determination of Aspirin and
Clopidogrel bisulphate in Tablet and Capsule Dosage Form, International Journal of PharmTech
Research Vol.2, No.1, (2010) pp 269-273.
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