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.
Multiple Method Development and Validation for Simultaneous Estimation of Chl...ijtsrd
A simple, precise and accurate multiple analytical method has been developed for the simultaneous estimation of Chlorzoxazone and Nimesulide in bulk and tablet formulations by reversed-phase liquid chromatographic and UV-Visible spectrophotometric techniques. The chromatographic separation was achieved on C18 analytical column. A mixture of Methanol 0.1 Ortho-phosphoric acid 75 25 was used as mobile phase, at a flow rate of 1mL min and detection wavelength at 295 nm. The retention time of Chlorzoxazone and Nimesulide was found to be 4.69 and 5.45 min respectively. The linear dynamic ranges for HPLC were from 2-10 µg mL and for simultaneous equation method, derivative spectroscopy, Q-ratio Absorbance method, Dual wavelength it was 10-30 µg mL for both Chlorzoxazone and Nimesulide. The percentage recovery obtained for Chlorzoxazone and Nimesulide were 100.93 and 102.19 respectively for RP-HPLC, 9.7 and 100.1 for simultaneous equation method of CZ and NIM respectively, 99.97 and 99.78 for derivative spectroscopy of CZ and NIM respectively, 101.37 and 99.48 for Q-ratio Absorbance method of CZ and NIM respectively, 100.13 and 99.96 for dual wavelength method of CZ and NIM respectively. The validation of the proposed methods were carried out for linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The developed method can be used for routine quality control analysis of titled drugs in combination in tablet formulation. Swetha Yarramsetti | A. Elphine Prabahar | Rama Rao Nadendla "Multiple Method Development and Validation for Simultaneous Estimation of Chlorzoxazone and Nimesulide in Bulk and Pharmaceutical Dosage Form" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-2 , February 2019, URL: https://www.ijtsrd.com/papers/ijtsrd21503.pdf
Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/21503/multiple-method-development-and-validation-for--simultaneous-estimation-of-chlorzoxazone-and--nimesulide-in-bulk-and-pharmaceutical-dosage-form/swetha-yarramsetti
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
New RP HPLC method for the simultaneous estimation of rosuvastatin and aspiri...SriramNagarajan19
A simple and selective LC method is described for the determination of Rosuvastatin and Aspirin tablet dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of A mixture of 60 volumes of 20mM Phosphate buffer pH 3.5: 20 volumes of Acetonitrile and 20 voulmes of Methanol. With detection of 232 nm. Linearity was observed in the range 12-28 µg /ml for Rosuvastatin (r2 =0.9977) and 90-210 µg /ml for Aspirin (r2 =0.9953) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing % RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
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.
Multiple Method Development and Validation for Simultaneous Estimation of Chl...ijtsrd
A simple, precise and accurate multiple analytical method has been developed for the simultaneous estimation of Chlorzoxazone and Nimesulide in bulk and tablet formulations by reversed-phase liquid chromatographic and UV-Visible spectrophotometric techniques. The chromatographic separation was achieved on C18 analytical column. A mixture of Methanol 0.1 Ortho-phosphoric acid 75 25 was used as mobile phase, at a flow rate of 1mL min and detection wavelength at 295 nm. The retention time of Chlorzoxazone and Nimesulide was found to be 4.69 and 5.45 min respectively. The linear dynamic ranges for HPLC were from 2-10 µg mL and for simultaneous equation method, derivative spectroscopy, Q-ratio Absorbance method, Dual wavelength it was 10-30 µg mL for both Chlorzoxazone and Nimesulide. The percentage recovery obtained for Chlorzoxazone and Nimesulide were 100.93 and 102.19 respectively for RP-HPLC, 9.7 and 100.1 for simultaneous equation method of CZ and NIM respectively, 99.97 and 99.78 for derivative spectroscopy of CZ and NIM respectively, 101.37 and 99.48 for Q-ratio Absorbance method of CZ and NIM respectively, 100.13 and 99.96 for dual wavelength method of CZ and NIM respectively. The validation of the proposed methods were carried out for linearity, accuracy, precision, limit of detection, limit of quantitation and robustness. The developed method can be used for routine quality control analysis of titled drugs in combination in tablet formulation. Swetha Yarramsetti | A. Elphine Prabahar | Rama Rao Nadendla "Multiple Method Development and Validation for Simultaneous Estimation of Chlorzoxazone and Nimesulide in Bulk and Pharmaceutical Dosage Form" Published in International Journal of Trend in Scientific Research and Development (ijtsrd), ISSN: 2456-6470, Volume-3 | Issue-2 , February 2019, URL: https://www.ijtsrd.com/papers/ijtsrd21503.pdf
Paper URL: https://www.ijtsrd.com/pharmacy/analytical-chemistry/21503/multiple-method-development-and-validation-for--simultaneous-estimation-of-chlorzoxazone-and--nimesulide-in-bulk-and-pharmaceutical-dosage-form/swetha-yarramsetti
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
New RP HPLC method for the simultaneous estimation of rosuvastatin and aspiri...SriramNagarajan19
A simple and selective LC method is described for the determination of Rosuvastatin and Aspirin tablet dosage forms. Chromatographic separation was achieved on a C18 column using mobile phase consisting of A mixture of 60 volumes of 20mM Phosphate buffer pH 3.5: 20 volumes of Acetonitrile and 20 voulmes of Methanol. With detection of 232 nm. Linearity was observed in the range 12-28 µg /ml for Rosuvastatin (r2 =0.9977) and 90-210 µg /ml for Aspirin (r2 =0.9953) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing % RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
Analytical method development and validation for the estimation of aspirin an...SriramNagarajan19
A simple and selective LC method is described for the determination of Aspirin and Omeprazole in tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of 30 volumes of ammonium acetate buffer, 40 volumes of acetonitrile and 30 volumes of Methanol with detection of 233 nm. Linearity was observed in the range 18-42 µg/ml for Aspirin (r2 =0.983) and 6-14 µg /ml for Omeprazole (r2 =0.970) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
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
Differential spectrophotometric method for estimation and validation of verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, Beers law limits 5-25µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamil in simple, precise and economically and it recommended for the routine drug quality analysis investigation
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 Cardiovascular DrugsIJMER
International Journal of Modern Engineering Research (IJMER) is Peer reviewed, online Journal. It serves as an international archival forum of scholarly research related to engineering and science education.
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research...iosrphr_editor
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research paper publishing, where to publish research paper, journal publishing, how to publish research paper, Call for research paper, international journal, publishing a paper, call for paper 2012, journal of pharmacy, how to get a research paper published, publishing a paper, publishing of journal, research and review articles, Pharmacy journal, International Journal of Pharmacy, hard copy of journal, hard copy of certificates, online Submission, where to publish research paper, journal publishing, international journal, publishing a paper
Development and Validation of the HPLC Method for the Analysis of Ametridio...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).
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
New spectrophotometric methods for the quantitative estimation of oxolamine i...IJSIT Editor
Five simple, sensitive and economical spectrophotometric methods have been developed for the
determination of Oxolamine in commercial dosage forms. The methods were based on the formation of
colored complex of Oxolamine with different reagents. The absorbance of the formed color complex is
measured at the wavelength of maximum absorbance of the complex against the reagent blank treated
similarly. All these method have different linearity ranges. Statistical analysis proves that the proposed
methods are reproducible and selective for the estimation of Oxolamine in bulk drug and in its tablet dosage
form.
Stability indicating analytical method development and validation for estimat...SriramNagarajan18
Stability indicating analytical method development and validation for estimation of Ceftazidime and Avibactam in bulk and pharmaceutical dosage form using RP-HPLC
Analytical method development and validation for the estimation of aspirin an...SriramNagarajan19
A simple and selective LC method is described for the determination of Aspirin and Omeprazole in tablet dosage forms. Chromatographic separation was achieved on a c18 column using mobile phase consisting of a mixture of 30 volumes of ammonium acetate buffer, 40 volumes of acetonitrile and 30 volumes of Methanol with detection of 233 nm. Linearity was observed in the range 18-42 µg/ml for Aspirin (r2 =0.983) and 6-14 µg /ml for Omeprazole (r2 =0.970) for the amount of drugs estimated by the proposed methods was in good agreement with the label claim. The proposed methods were validated. The accuracy of the methods was assessed by recovery studies at three different levels. Recovery experiments indicated the absence of interference from commonly encountered pharmaceutical additives. The method was found to be precise as indicated by the repeatability analysis, showing %RSD less than 2. All statistical data proves validity of the methods and can be used for routine analysis of pharmaceutical dosage form.
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
Differential spectrophotometric method for estimation and validation of verap...roshan telrandhe
The aimed of current research to development of the simple, rapid and sensitive Differential spectrophotometric method for the estimation of Verapamil in tablet dosage form. In this method two medium was use acid and alkaline and the difference spectrum was calculated. 0.1N HCL and 0.1N NaOH was used in this differential method. The λmax 278, Beers law limits 5-25µg/ml, regression equation Y= 0.024x-0.009, slope 0.024, intercept 0.09, correlation coefficient (r2) 0.998, %RSD <1.5, % Recovery (Tablet) 100.46% was shows the good efficacy and results. This method future scope in quality control of the verapamil in simple, precise and economically and it recommended for the routine drug quality analysis investigation
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 Cardiovascular DrugsIJMER
International Journal of Modern Engineering Research (IJMER) is Peer reviewed, online Journal. It serves as an international archival forum of scholarly research related to engineering and science education.
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research...iosrphr_editor
IOSR Journal of Pharmacy (IOSRPHR), www.iosrphr.org, call for paper, research paper publishing, where to publish research paper, journal publishing, how to publish research paper, Call for research paper, international journal, publishing a paper, call for paper 2012, journal of pharmacy, how to get a research paper published, publishing a paper, publishing of journal, research and review articles, Pharmacy journal, International Journal of Pharmacy, hard copy of journal, hard copy of certificates, online Submission, where to publish research paper, journal publishing, international journal, publishing a paper
Development and Validation of the HPLC Method for the Analysis of Ametridio...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).
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
New spectrophotometric methods for the quantitative estimation of oxolamine i...IJSIT Editor
Five simple, sensitive and economical spectrophotometric methods have been developed for the
determination of Oxolamine in commercial dosage forms. The methods were based on the formation of
colored complex of Oxolamine with different reagents. The absorbance of the formed color complex is
measured at the wavelength of maximum absorbance of the complex against the reagent blank treated
similarly. All these method have different linearity ranges. Statistical analysis proves that the proposed
methods are reproducible and selective for the estimation of Oxolamine in bulk drug and in its tablet dosage
form.
Stability indicating analytical method development and validation for estimat...SriramNagarajan18
Stability indicating analytical method development and validation for estimation of Ceftazidime and Avibactam in bulk and pharmaceutical dosage form using RP-HPLC
RP-HPLC Assay Method Validation for the estimation of new Anti-retroviral dru...SriramNagarajan15
A Reverse phase HPLC method was developed for estimation of the Lamivudine in bulk and tablet formulation by using ODS column (250mm×4.6mm, 5µm) and Acetate buffer: acetonitrile (50:50) as mobile phase, at a flow rate of 1.5ml/min. The detection was carried at the 272nm the retention time of the Lamivudine is 1.850. The developed method was validated for the various parameters as per the ICH guidelines like accuracy precision, linearity and range, Robustnes. Linearity was obtained in the concentration range of 10µg/ml to 50µg/ml with correlation coefficient of 0.999. The accuracy of the method was assessed by recovery studies at three different concentration levels. The percentage recovery of Lamivudine was found to be in the range of 98% -102%. The method was found to be precise as indicated by the repeatability, inter-day, intra-day analysis, showing %RSD less than 2. Key words: RP-HPLC, Lamivudine, Pharmaceutical dosage form.
RP-HPLC Assay Method Validation for the estimation of new Anti-retroviral dru...SriramNagarajan15
A Reverse phase HPLC method was developed for estimation of the Lamivudine in bulk and tablet formulation by using ODS column (250mm×4.6mm, 5µm) and Acetate buffer: acetonitrile (50:50) as mobile phase, at a flow rate of 1.5ml/min. The detection was carried at the 272nm the retention time of the Lamivudine is 1.850. The developed method was validated for the various parameters as per the ICH guidelines like accuracy precision, linearity and range, Robustnes. Linearity was obtained in the concentration range of 10µg/ml to 50µg/ml with correlation coefficient of 0.999. The accuracy of the method was assessed by recovery studies at three different concentration levels. The percentage recovery of Lamivudine was found to be in the range of 98% -102%. The method was found to be precise as indicated by the repeatability, inter-day, intra-day analysis, showing %RSD less than 2. Key words: RP-HPLC, Lamivudine, Pharmaceutical dosage form.
A Simple Rp- HPLC Method for Simultaneous Estimation of Six Cardiovascular Dr...iosrjce
A simple, convenient Rp-HPLC method has been developed and validated for the simultaneous
estimation of Metolazone, Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone. The column
used was an Inertsil ODS 3 V column of 250 mm length × 4.6 mm ID, with 3 micron particle size of adsorbent.
Separation was achieved using isocratic elution in a buffer-acetonitrile-methanol mobile phase at a flow rate of
1.2 ml/min. The detection was performed at wavelength of 225 nm using a UV detector. The column temperature
was 450C and injection volume was 20µl. The method was validated for precision, linearity and accuracy. The
% RSD for all the drugs was found to be less than 2 %. The correlation coefficient (r2
) was not less than 0.999
for all drugs. The mean percent recovery of the drugs from tablet placebo at 50%, 100% and 150% were within
limits. The marketed formulations of the drugs were analyzed and the mean assay results were found to be
within limits. The developed method can thus be employed for routine simultaneous analysis of Metolazone,
Indapamide, Nebivolol, Rosuvastatin, Olmesartan and Spironolactone in bulk and in their marketed
formulations
Method Development and Validation of Clopidogrel Bisulphate by Reverse Phase-...SriramNagarajan15
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.
Similar to Stability indicating analytical method development and Validation for Isoniazide, Thiacetazone and Pyridoxine by RP-HPLC UV method (20)
Stability indicating method and validation for the simultaneous estimation of...SriramNagarajan18
Stability indicating method and validation for the simultaneous estimation of metformin and empagliflozin by using RP-HPLC in a bulk and pharmaceutical dosage forms
- Video recording of this lecture in English language: https://youtu.be/lK81BzxMqdo
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Basavarajeeyam is an important text for ayurvedic physician belonging to andhra pradehs. It is a popular compendium in various parts of our country as well as in andhra pradesh. The content of the text was presented in sanskrit and telugu language (Bilingual). One of the most famous book in ayurvedic pharmaceutics and therapeutics. This book contains 25 chapters called as prakaranas. Many rasaoushadis were explained, pioneer of dhatu druti, nadi pareeksha, mutra pareeksha etc. Belongs to the period of 15-16 century. New diseases like upadamsha, phiranga rogas are explained.
Recomendações da OMS sobre cuidados maternos e neonatais para uma experiência pós-natal positiva.
Em consonância com os ODS – Objetivos do Desenvolvimento Sustentável e a Estratégia Global para a Saúde das Mulheres, Crianças e Adolescentes, e aplicando uma abordagem baseada nos direitos humanos, os esforços de cuidados pós-natais devem expandir-se para além da cobertura e da simples sobrevivência, de modo a incluir cuidados de qualidade.
Estas diretrizes visam melhorar a qualidade dos cuidados pós-natais essenciais e de rotina prestados às mulheres e aos recém-nascidos, com o objetivo final de melhorar a saúde e o bem-estar materno e neonatal.
Uma “experiência pós-natal positiva” é um resultado importante para todas as mulheres que dão à luz e para os seus recém-nascidos, estabelecendo as bases para a melhoria da saúde e do bem-estar a curto e longo prazo. Uma experiência pós-natal positiva é definida como aquela em que as mulheres, pessoas que gestam, os recém-nascidos, os casais, os pais, os cuidadores e as famílias recebem informação consistente, garantia e apoio de profissionais de saúde motivados; e onde um sistema de saúde flexível e com recursos reconheça as necessidades das mulheres e dos bebês e respeite o seu contexto cultural.
Estas diretrizes consolidadas apresentam algumas recomendações novas e já bem fundamentadas sobre cuidados pós-natais de rotina para mulheres e neonatos que recebem cuidados no pós-parto em unidades de saúde ou na comunidade, independentemente dos recursos disponíveis.
É fornecido um conjunto abrangente de recomendações para cuidados durante o período puerperal, com ênfase nos cuidados essenciais que todas as mulheres e recém-nascidos devem receber, e com a devida atenção à qualidade dos cuidados; isto é, a entrega e a experiência do cuidado recebido. Estas diretrizes atualizam e ampliam as recomendações da OMS de 2014 sobre cuidados pós-natais da mãe e do recém-nascido e complementam as atuais diretrizes da OMS sobre a gestão de complicações pós-natais.
O estabelecimento da amamentação e o manejo das principais intercorrências é contemplada.
Recomendamos muito.
Vamos discutir essas recomendações no nosso curso de pós-graduação em Aleitamento no Instituto Ciclos.
Esta publicação só está disponível em inglês até o momento.
Prof. Marcus Renato de Carvalho
www.agostodourado.com
Knee anatomy and clinical tests 2024.pdfvimalpl1234
This includes all relevant anatomy and clinical tests compiled from standard textbooks, Campbell,netter etc..It is comprehensive and best suited for orthopaedicians and orthopaedic residents.
Adv. biopharm. APPLICATION OF PHARMACOKINETICS : TARGETED DRUG DELIVERY SYSTEMSAkankshaAshtankar
MIP 201T & MPH 202T
ADVANCED BIOPHARMACEUTICS & PHARMACOKINETICS : UNIT 5
APPLICATION OF PHARMACOKINETICS : TARGETED DRUG DELIVERY SYSTEMS By - AKANKSHA ASHTANKAR
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
Local Advanced Lung Cancer: Artificial Intelligence, Synergetics, Complex Sys...Oleg Kshivets
Overall life span (LS) was 1671.7±1721.6 days and cumulative 5YS reached 62.4%, 10 years – 50.4%, 20 years – 44.6%. 94 LCP lived more than 5 years without cancer (LS=2958.6±1723.6 days), 22 – more than 10 years (LS=5571±1841.8 days). 67 LCP died because of LC (LS=471.9±344 days). AT significantly improved 5YS (68% vs. 53.7%) (P=0.028 by log-rank test). Cox modeling displayed that 5YS of LCP significantly depended on: N0-N12, T3-4, blood cell circuit, cell ratio factors (ratio between cancer cells-CC and blood cells subpopulations), LC cell dynamics, recalcification time, heparin tolerance, prothrombin index, protein, AT, procedure type (P=0.000-0.031). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and N0-12 (rank=1), thrombocytes/CC (rank=2), segmented neutrophils/CC (3), eosinophils/CC (4), erythrocytes/CC (5), healthy cells/CC (6), lymphocytes/CC (7), stick neutrophils/CC (8), leucocytes/CC (9), monocytes/CC (10). Correct prediction of 5YS was 100% by neural networks computing (error=0.000; area under ROC curve=1.0).
- Video recording of this lecture in English language: https://youtu.be/kqbnxVAZs-0
- Video recording of this lecture in Arabic language: https://youtu.be/SINlygW1Mpc
- Link to download the book free: https://nephrotube.blogspot.com/p/nephrotube-nephrology-books.html
- Link to NephroTube website: www.NephroTube.com
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NVBDCP.pptx Nation vector borne disease control programSapna Thakur
NVBDCP was launched in 2003-2004 . Vector-Borne Disease: Disease that results from an infection transmitted to humans and other animals by blood-feeding arthropods, such as mosquitoes, ticks, and fleas. Examples of vector-borne diseases include Dengue fever, West Nile Virus, Lyme disease, and malaria.
Basavarajeeyam is a Sreshta Sangraha grantha (Compiled book ), written by Neelkanta kotturu Basavaraja Virachita. It contains 25 Prakaranas, First 24 Chapters related to Rogas& 25th to Rasadravyas.
micro teaching on communication m.sc nursing.pdfAnurag Sharma
Microteaching is a unique model of practice teaching. It is a viable instrument for the. desired change in the teaching behavior or the behavior potential which, in specified types of real. classroom situations, tends to facilitate the achievement of specified types of objectives.
Stability indicating analytical method development and Validation for Isoniazide, Thiacetazone and Pyridoxine by RP-HPLC UV method
1. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
225
International Journal of Farmacia
Journal Home page: www.ijfjournal.com
Stability indicating analytical method development and Validation for
Isoniazide, Thiacetazone and Pyridoxine by RP-HPLC UV method
Amena shafia rasheed*
Deccan School of Pharmacy, Dar-Us-Salam, Aghapura, Near Nampally, Hyderabad
Corresponding Author: Amena Shafia Rasheed
Email: awsumshas@gmail.com
ABSTRACT
A simple, rapid and precise liquid chromatographic method for simultaneous determination of isoniazid
thiacetazone and pyridoxine, in a tablet dosage form has been developed. Chromatographic analysis was performed
on a HYPERSIL ODS column (C18) column (150*4.6 mm) of 5µ particle size, applying isocratic elution with a
mobile phase. A mixture of 40 volumes of Ammonium Formate Buffer: 60 volumes of Acetonitrile were prepared.
The mobile phase was sonicated for 10min to remove gases Wave length: 254nm Injection volume:20µl Column
temperature: 25o
C. UV detection was performed at 254 nm. The total run time was 8 min. Retention times for
isoniazid thiacetazone and pyridoxine are 2.7428, 3.6267, 8.217 mins, respectively. The method was validated with
respect to linearity, accuracy, precision, specificity and sensitivity in accordance with ICH guidelines. The percent
recovery for Isoniazide is 99.99%, Thiacetazone 99.14% and Pyridoxine 99.4%. The linearity was determined at
five levels over the range of 50%-150% of standard concentration in diluents. The concentration range at which
linearity was established is 200-600 g/ml for Isoniazide Thiacetazone 100-300 and Pyridoxine 2-6g/ml. The
coefficient of correlation (R2
= 0.998) for Isoniazide, and Thiacetazone for (R2
= 0.997) and (R2
= 0.996) for
Pyridoxine. The plate count was found to be more than 2000, tailing for the same peak is not more than 2.0 and %
RSD is not more than 2.0%. High recovery and low coefficients of variance confirmed the suitability of the method
for the simultaneous analysis of the three considered drugs. Isoniazide, Thiacetazone and Pyridoxine was subjected
to various stress conditions like hydrolytic degradation, thermal degradation, Peroxide degradation, photolytic
degradation. The developed method was found to be stable in all the conditions. The developed method is stability
indicating and can be used or routine analysis of Isoniazide, Thiacetazone and Pyridoxine free of interference from
their degradation products in suspension formulation.
INTRODUCTION
Isoniazid (Laniazid, Nydrazid), also known
as isonicotinylhydrazine (orINH), is an organic
compound that is the first-line medication in
prevention and treatment of tuberculosis. Isoniazid
(INH) is a synthetic, bactericidal anti tubercular agent
that is active against many mycobacterium's,
primarily those that are actively dividing.
Thioacetazone is used in the treatment of tuberculosis
[1], it has only weak activity against Mycobacterium
tuberculosis and is only useful in preventing
resistance to more powerful drugs
like isoniazid and rifampicin [2]. It is never used on
its own to treat tuberculosis. Pyridoxine is one form
of vitamin B6. Its hydrochloride salt pyridoxine
hydrochloride is used as vitamin B6 dietary
supplement [3].
2. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
226
EXPERIMENTAL WORK
Chemicals
Water HPLC Grade
Methanol HPLC Grade
Potassium Dihydrogen ortho Phosphate AR Grade
Acetonitrile HPLC Grade
Di potassium hydrogen ortho phosphate AR Grade
Ammonium acetate AR Grade
Ammonium formate AR Grade
Instrument and chromatographic condition
All solvent used in this work are HPLC & AR
grade. Instrument and chromatographic condition RP-
HPLC Shimadzu LC20AT infinity series separation
model equipped with UV Detector was employed in
this method. The Lab solutions software was used for
LC peak integration along data acquisition and data
processing [4]. The column used for separation of
analyte is Hypersil ODS (150×4.6mm) 5µ. Mobile
phase consisting of phosphate buffer: Acetonitrile in
the ratio of 60:40 % v/v at flow rate 1 ml/min [5]. it
was filter through 0.45 μm nylon filter and sonicated
for 5 min in ultrasonic bath. Sample was analyzed at
231 nm at an injection volume of 20μl [6].
Preparation of phosphate buffer
1.625 gm of Potassium Di Hydrogen ortho
phosphate and 0.3 gms of Di Potassium Hydrogen
ortho phosphate was weighed and dissolve in 100 ml
of water and volume was made up to 550 ml with
water. Adjust the PH
using ortho phosphoric acid. The
buffer was filtered through 0.45µ filters to remove all
fine particles and gases [7].
PREPARATION OF SOLUTIONS
Preparation of Mixed Standard Solution: (400
µg/ml, 200 µg/ml & 4µg/ml)
Weigh accurately 37.5mg of Thiacetazone and
75mg of Isoniazide and 0.75mg of Pyridoxine in 100
ml of volumetric flask and dissolve in 10ml of mobile
phase and make up the volume with mobile phase
From above stock solution 200µg/ml of Thiacetazone
and 400µg/ml of Isoniazide and 4µg/ml of Pyridoxine
is prepared by diluting 5.3ml to 10ml with mobile
phase. This solution is used for recording
chromatogram [8].
Preparation of Sample Solution
10 tablets (each tablet contains 37.5mg of
Thiacetazone and 75mg of Isoniazide and 0.75mg of
Pyridoxine) were weighed and taken into a mortar
and crushed to fine powder and uniformly mixed [9].
Tablet stock solutions of Thiacetazone (200μg/ml)
and Isoniazide (400μg/ml) and Pyridoxine (4µg/ml)
were prepared by dissolving weight equivalent to
37.5mg of Thiacetazone and 75mg of Isoniazide and
0.75mg of Pyridoxine and dissolved in sufficient
mobile phase [10]. After that filtered the solution
using 0.45-micron syringe filter and Sonicated for 5
min and dilute to 100ml with mobile phase. Further
dilutions are prepared in 5 replicates of 200μg/ml of
Thiacetazone and 400μg/ml of Isoniazide and 4µg/ml
of Pyridoxine was made by adding 5.3ml of stock
solution to 10 ml of mobile phase [11-12].
Table 1: Summary of Chromatographic conditions
Column ODS Hypersil C-18 (150*4.6mm) 5μ
Pump mode Isocratic
Flow rate 1.0 ml/min
Wave length 254 nm
Injection volume 20μl
Column temperature 25o
C
Mobile phase ratio Ammonium formate: Acetonitrile (40:60)
3. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
227
Fig: 3 Typical chromatogram of Thiacetazone, Isoniazide & Pyridoxine
Method validation
The validation of method was carried out as per
ICH guideline. The parameters assessed were
specificity, linearity, precision, accuracy, stability,
LOD and LOQ. Specificity Specificity is the ability of
the analytical method to measure the analyte response
in the presence of interferences including degradation
product and related substances.
Accuracy
The accuracy was determined by calculating %
recoveries of Thiacetazone, Isoniazide & Pyridoxine.
It was carried out by adding known amount of each
analyte corresponding to three conc. Levels (80, 100,
120) of the label claims to the excipients. At each
level, six determinations were performed and the
accuracy results were expressed as percent analyte
recovered by proposed method.
Precision
Method precision
Precision of an analytical method is usually
expressed as the standard deviation. Method precision
was demonstrated by preparing six samples as per test
method representing single batch and were
chromatographed. The precision of the method was
evaluated by computing the %RSD of the results. The
individual values and the low % RSD observed on the
values are within acceptance criteria and indicates that
method is precise.
Linearity
The purpose of the test for linearity is to
demonstrate that the entire analytical system
(including detector and data acquisition) exhibits
linear responses and directly proportional over the
relevant conc. Range for the target conc. of the
analyte. The linear regression data for the calibration
plot is the indicative of a good linear relationship
between peak and concentration over wide range. The
correlation coefficient was indicative of high
significance.
Robustness
Robustness of method was investigated under a
variety of conditions including changes of
composition of buffer in the mobile phase, flow rate
and temperature. This deliberate change in the method
has no effect on the peak tailing, peak area and
theoretical plates finally the method was found to be
robust.
Ruggedness
The ruggednss of the method was studied by the
determining the analyst to analyst variation by
performing the Assay by two different analysts. %
RSD Assay values between two analysts not greater
than 2.0%, hence the method was rugged.
Limit of Detection and Limit of Quantitation:
The LOD can be defined as the smallest level of
analyte that gives a measurable responses and LOQ
was determined as the lowest amount of the analyte
that was reproducibly quantified. These two
parameters were calculated using formula based on
standard deviation of the response and slope. LOD
and LOQ were calculated by equation, LOD=3.3 x ϭ/s
and LOQ= 10 x ϭ/s, where s = standard deviation, S =
slope of calibration curve.
4. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
228
Assay of Thiacetazone, Isoniazide &
Pyridoxine in pharmaceutical dosage form
Assay of marketed product was carried out by
using the developed method. Sample solutions were
prepared and injected into RP –HPLC system. The
sample solution was scanned at 254 nm. The
percentage drug estimated was found to be 99.91% ,
99.84% and 99.39% respectively as Thiacetazone,
Isoniazide & Pyridoxine. The chromatogram showed
two single peaks of Thiacetazone, Isoniazide &
Pyridoxine was observed with retention time 2.570,
5.457 & 6.643 min respectively.
Forced degradation studies
Stress studies are performed according to ICH
guidelines under following conditions.
Acid degradation
To 5 ml of sample solution add 1ml of 0.1N HCL
and sonicate place it aside for 3hrs, then neutralize the
solution with 1 ml of base and then transfer above
solution into10 ml volumetric flask dilute with mobile
phase and record the chromatogram .
Alkaline degradation
To 5 ml of sample solution add 1ml of 0.1N
NaOH and sonicate place it aside for 3hrs, then
neutralize the solution with 1 ml of acid and then
transfer above solution into 10 ml volumetric flask
dilute with mobile phase and record the
chromatogram.
Peroxide degradation
To 5 ml of sample solution add 1ml of 3% H2 O 2
and sonicate place it aside for 3hrs, then transfer the
above solution into 10 ml volumetric flask dilute with
mobile phase and record the chromatogram.
Photolytic degradation
Expose about 100 mg of sample in UV light
chamber at 365 nm for 3hrs. Weigh accurately this
powder equivalent to 10 mg of Ornidazole and 15 mg
of Diloxanidefuroate into a 100ml volumetric flask
and make up the volume and sonicate for 30 minutes
with intermittent shaking and volume is made up to
the mark with mobile phase and record the
chromatogram.
Thermal degradation
Expose about 100 mg of sample in to dry heat to
80˚ C for 3hrs. Weigh accurately this powder
equivalent to 10 mg of Ornidazole and 15 mg of
Diloxanide furoate into a 100ml volumetric flask and
make up the volume and sonicate for 30 minutes with
intermittent shaking and volume is made up to the
mark with mobile phase and record the
chromatogram. Record the peak area of stressed
samples then compare it with peak area of unstressed
sample to determine the % degradation.
% degradation = Response of unstressed sample – response of stressed sample
------------------------------------------------------------------------------ X100
Response of unstressed sample
RESULTS AND DISCUSSION
The HPLC separation and quantification were
achieved on thermohypersil BDS (4.6 x 150mm, 5).
The mobile phase was prepared by mixing
ammoniumformate buffer and acetonitrile in the ratio
of (40: 60 )v/v that run isocratic ally at the flow rate
of 1.0ml/min. The wavelength at which detector was
set is 254nm. The optimized chromatographic
conditions and chromatogram is shown in table 4.1.8
and figure 4.1.9 respectively. Calibration curve at
five levels over the range of 50%-150% of standard
concentration in a diluents whose concentration was.
The calibration curves were obtained by plotting the
peak area Vs concentration. The calibration curves are
shown in figure 4.1.2.14 & 4.15 and table 4.17.
Accuracy is determined at three different levels
50%, 100%, 150%. The percent recovery for
Isoniazide, Thiacetazone and Pyridoxine is 99.84%,
99.91% and 99.39% respectively, which is presented
in the table 4.1.29,4.1.30 and 4.1.30. The precision of
each method was ascertained separately from the peak
area obtained by actual determination of six replicates
of a fixed amount of drug i.e. (37.5g/ml of isoniazid,
75g/ml of thiacetazone and 0.75g/ml of
pyridoxine). The % RSD were calculated for
Isoniazide, Thiacetazone and Pyridoxine and
presented in the table 4.1.42.
Robustness of the method was studied by
deliberate variations of the analytical parameters such
as flow rate (± 0.2ml/min) & wavelength (± 2o
C). The
5. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
229
chromatograms and results of robustness is given in
figure 4.24 and table 4.29 & 4.30 respectively.
In the forced degradation studies it was found that
Isoniazide showed no degradation in acid (0.1M HCl),
base (0.1M NaOH), peroxide, heat and UV. In case of
Thiacetazone showed showed no degradation in acid
(0.1M HCl), base (0.1M NaOH), peroxide, heat and
sunlight. Pyridoxine is unstable in acidic degradation
and in UV degradation but overall the net degradation
was within the limits.
Results of linearity
Fig: 4 Linearity curve of Isoniazide
Fig: 5 Linearity curve of Thiacetazone
y = 16.733x + 531.56
R² = 0.998
0.000
2000.000
4000.000
6000.000
8000.000
10000.000
12000.000
0 200 400 600 800
Series1
Linear…
Linearity of Isoniazide
y = 18.928x - 40.756
R² = 0.9978
0.000
1000.000
2000.000
3000.000
4000.000
5000.000
6000.000
0 100 200 300 400
Area
Conc
9. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
233
Per Oxide Degradation 140.23 3632.527 99.42 1.78
UV Degradation 141.31 3645.933 99.02 2.18
PYRIDOXINE
Conditions Sample weight(mg) Peak Area % claim %
Degradation
Sample Control 142.897 173.685 100.98 -
Alkali Degradation 140.23 143.296 95.12 5.86
Acid Degradation 144.36 159.423 92.52 8.46
Thermal Degradation 139.98 151.135 94.26 6.72
Per Oxide Degradation 140.63 172.775 100.87 0.11
UV Degradation 143.25 154.546 92.23 8.75
CONCLUSION
In order to achieve simple, precise, accurate
method development simultaneous elution of three
components initial trials were performed with an
objective to select adequate and optimum
chromatographic conditions. Parameters such as ideal
mobile phase and their proportions, detection
wavelength, optimum pH, different columns and
concentration of the standard solutions were carefully
studied. Solvent and buffer (ammonium formate-
Acetonitrile) were tested by using different
proportions, such as ammonium formate - acetonitrile
in the ratio of (50:50v/v), (30:70 v/v), (60:40 v/v) .
Finally, a mixture of ammonium formate and
acetonitrile in the proportion of 40:60 v/v was
selected as the optimum mobile phase and a flow rate
of 0.1ml/min. The separation was achieved on
thermohypersil BDS (4.6 x 150mm, 5). Under these
conditions, the analyte peaks were well resolved and
free from tailing. The tailing factor was < 1.5 for both
the analytes. The retention time obtained for
Isoniazide was 2.742 min for thiacetazone it was
3.626 and for Pyridoxine it was 8.217. The developed
method was validated by evaluating system
suitability, recovery, linearity, precision, robustness,
specificity. System suitability was evaluated by
injecting 10 l of standard solution six times, the
chromatogram were recorded. System suitability
parameter like, plate count and tailing factor were also
recorded. The plate count was found to be more than
2000, tailing for the same peak is not more than 2.0
and % RSD is not more than 2.0%. The linearity was
determined at five levels over the range of 50%-150%
of standard concentration in a diluents. The
concentration range at which linearity was established
is 200-600 g/ml for Isoniazide Thiacetazone 100-
300 and Pyridoxine 2-6g/ml. The coefficient of
correlation (R2
= 0.998) for Isoniazide, and
Thiacetazone for (R2
= 0.997) and (R2
= 0.996) for
Pyridoxine.
Accuracy is determined at three different levels
50%, 100%, 150%. The recovery experiment was
carried out by standard addition method. The percent
recovery for Isoniazide is 99.99%, Thiacetazone
99.14% and Pyridoxine 99.4%. The precision of each
method was ascertained separately from the peak area
obtained by actual determination of six replicates of a
fixed amount of drug i.e. (37.5 g/ml of Isoniazide,
75g/ml Thiacetazone and 0.75g/ml of Pyridoxine).
The RSD of Isoniazide, Thiacetazone and Pyridoxine
is found to be 0.40 and 0.76 and 0.29 respectively.
Robustness of the method was studied by deliberate
variations of the analytical parameters such as flow
rate (± 0.2ml/min) & wavelength (± 2nm). it was
found that even if the most critical parameters like
flow rate and temperature is changed, all system
suitability parameters were within the acceptance
criteria. Isoniazide, Thiacetazone and Pyridoxine was
subjected to various stress conditions like hydrolytic
degradation, thermal degradation, Peroxide
degradation, photolytic degradation. The developed
method was found to be stable in all the conditions.
The developed method is stability indicating and can
be used or routine analysis of Isoniazide,
Thiacetazone and Pyridoxine free of interference from
their degradation products in suspension formulation.
All these factors make this method suitable for
quantification of Isoniazide, Thiacetazone and
Pyridoxine in pharmaceutical dosage form. It can
therefore be concluded that use of the method can
10. Amena S R et al / Int. J. of Farmacia, 2016; Vol-(2) 4: 225-234
234
save much time and money and it can be used in small
laboratories with high accuracy and wide linear range.
The method can be successfully used for routine
analysis of Isoniazide, Thiacetazone and Pyridoxine
in marketed formulation without interference.
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[1]. Alfonso R Gennaro -Remington the science and practice of pharmacy- II, edition-20, 587.
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