Pub Date : 2023-06-03DOI: 10.52711/2231-5675.2023.00018
V. Ravikumar, Chillara Sandhya, R. Sri. S
A simple, rapid, specific and accurate reverse phase high performance liquid chromatographic method has been developed for the validated of Letrozole in bulk as well as in marketed pharmaceutical dosage form. This separation was performed on a Symmetry ODS C18 (4.6×250mm, 5µm) column with Methanol: Phosphate Buffer (35:65) V/V as mobile phase at a flow rate of 1.0mL min−1 with UV detection at 240nm; the constant column temperature was Ambient. The runtime under these chromatographic conditions was less than 8 min. The retention time of Letrozole was found to be 2.252. The calibration plot was linear over the concentration range of 6–14μg mL−1 with limits of detection and quantification values of 1.2 and 3.6ng mL−1 respectively. The mean % assay of marketed formulation was found to be 99.86%, and % recovery was observed in the range of 98-102%. Relative standard deviation for the precision study was found <2%. The developed method is simple, precise, specific, accurate and rapid, making it suitable for estimation of Letrozole in bulk and marketed pharmaceutical dosage formdosage form.
{"title":"A New Analytical RP-HPLC Method for the Estimation of Letrozole in Pure and Tablet form","authors":"V. Ravikumar, Chillara Sandhya, R. Sri. S","doi":"10.52711/2231-5675.2023.00018","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00018","url":null,"abstract":"A simple, rapid, specific and accurate reverse phase high performance liquid chromatographic method has been developed for the validated of Letrozole in bulk as well as in marketed pharmaceutical dosage form. This separation was performed on a Symmetry ODS C18 (4.6×250mm, 5µm) column with Methanol: Phosphate Buffer (35:65) V/V as mobile phase at a flow rate of 1.0mL min−1 with UV detection at 240nm; the constant column temperature was Ambient. The runtime under these chromatographic conditions was less than 8 min. The retention time of Letrozole was found to be 2.252. The calibration plot was linear over the concentration range of 6–14μg mL−1 with limits of detection and quantification values of 1.2 and 3.6ng mL−1 respectively. The mean % assay of marketed formulation was found to be 99.86%, and % recovery was observed in the range of 98-102%. Relative standard deviation for the precision study was found <2%. The developed method is simple, precise, specific, accurate and rapid, making it suitable for estimation of Letrozole in bulk and marketed pharmaceutical dosage formdosage form.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"4 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82927098","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-03DOI: 10.52711/2231-5675.2023.00020
Prithviraj. B. Chavan, Mahesh. H. Kolhe, Kavita. V. Dhamak, Rohit. J. Bhor
Carvedilol and ivabradine is a drug combination used to treat cardiovascular diseases like hypertension, chronic stable angina pectoris and, chronic heart failure. Both are different in their mode of action. Carvedilol prevents exercise-induced tachycardia via inhibition of beta-adrenoreceptor carvedilol also acting on alpha-1 adrenergic receptors and an overall reduction in blood pressure. In case of a higher dose also shows antioxidant and calcium channel blocking activity. Ivabradine is a heart rate reducing drug that works by blocking cardiac pacemaker currents (If) selectively and specifically. The major goal of this review paper is to emphasize the characteristics of carvedilol and ivabradine, such as their pharmacological profiles, mechanisms of action, pharmacokinetic and pharmacodynamic studies, and previously described analytical methodologies for carvedilol and ivabradine determination. Various methods such as UV spectroscopy HPLC, RP-HPLC, UPLC. This review deals with the various analytical method reported and adopted for the estimation of carvedilol and ivabradine.
{"title":"Analytical Technique for Carvedilol and Ivabradine determination from pure and Pharmaceutical Dosage Forms: A Review","authors":"Prithviraj. B. Chavan, Mahesh. H. Kolhe, Kavita. V. Dhamak, Rohit. J. Bhor","doi":"10.52711/2231-5675.2023.00020","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00020","url":null,"abstract":"Carvedilol and ivabradine is a drug combination used to treat cardiovascular diseases like hypertension, chronic stable angina pectoris and, chronic heart failure. Both are different in their mode of action. Carvedilol prevents exercise-induced tachycardia via inhibition of beta-adrenoreceptor carvedilol also acting on alpha-1 adrenergic receptors and an overall reduction in blood pressure. In case of a higher dose also shows antioxidant and calcium channel blocking activity. Ivabradine is a heart rate reducing drug that works by blocking cardiac pacemaker currents (If) selectively and specifically. The major goal of this review paper is to emphasize the characteristics of carvedilol and ivabradine, such as their pharmacological profiles, mechanisms of action, pharmacokinetic and pharmacodynamic studies, and previously described analytical methodologies for carvedilol and ivabradine determination. Various methods such as UV spectroscopy HPLC, RP-HPLC, UPLC. This review deals with the various analytical method reported and adopted for the estimation of carvedilol and ivabradine.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"71 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81675152","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-03DOI: 10.52711/2231-5675.2023.00014
Aditya Mathur, Ravikumar Vejendla
The aim of this study is to develop and validate a method for the quantitative analysis of Rivastigmine tartarate capsules 1.5mg. An isocratic HPLC method using a reverse phase C-8 column and a mobile phase along with buffer (pH 3.0) was developed, optimized and validated. The analysis was carried out with a flow rate of 1.5 ml/min at 500C and was monitored at λmax - 220nm. Chromatogram of Rivastigmine tartarate was observed at 11min. The complete elution of Rivastigmine tartarate was achieved in 11.29 min at 220nm. This HPLC method showed good linearity, accuracy, selectivity, and other validation parameters. The recovery (accuracy) at all concentration levels was found to be more than 100% within the range of 102%. System suitability was determined by calculating the percent relative deviation (%RSD) for area five replicates injection of 120ppm in HPLC. All the peaks were resolved from the API with significantly different RT. Rivastigmine tartarate was subjected for stability indicating assay method which must be validated invariably calls for a forced degradation conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Rivastigmine tartarate was found to degrade significantly in base degradation condition and little in thermal, thermal humidity, photolytic, acid and oxidative stress degradation conditions.
{"title":"Novel Method Development, Validation and Stability Indicating Assay Method for Rivastigmine Tartarate Capsule by HPLC","authors":"Aditya Mathur, Ravikumar Vejendla","doi":"10.52711/2231-5675.2023.00014","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00014","url":null,"abstract":"The aim of this study is to develop and validate a method for the quantitative analysis of Rivastigmine tartarate capsules 1.5mg. An isocratic HPLC method using a reverse phase C-8 column and a mobile phase along with buffer (pH 3.0) was developed, optimized and validated. The analysis was carried out with a flow rate of 1.5 ml/min at 500C and was monitored at λmax - 220nm. Chromatogram of Rivastigmine tartarate was observed at 11min. The complete elution of Rivastigmine tartarate was achieved in 11.29 min at 220nm. This HPLC method showed good linearity, accuracy, selectivity, and other validation parameters. The recovery (accuracy) at all concentration levels was found to be more than 100% within the range of 102%. System suitability was determined by calculating the percent relative deviation (%RSD) for area five replicates injection of 120ppm in HPLC. All the peaks were resolved from the API with significantly different RT. Rivastigmine tartarate was subjected for stability indicating assay method which must be validated invariably calls for a forced degradation conditions of oxidative, acid, base, hydrolytic, thermal and photolytic degradation. Rivastigmine tartarate was found to degrade significantly in base degradation condition and little in thermal, thermal humidity, photolytic, acid and oxidative stress degradation conditions.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"41 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90246670","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-03DOI: 10.52711/2231-5675.2023.00016
Adhao Vaibhav S., Ambhore Jaya P., Thenge Raju R.
A new simple, specific, accurate and precise RP-HPLC method was developed for determination of Leflunomide. In the present study, stress testing of Leflunomide was carried out according to ICH guidelines Q1A (R2). Leflunomide was subjected to stress conditions of hydrolysis, oxidation, photolysis and neutral decomposition. Effective separation of drug and degradant was achieved was achieved on a Hypersil BDS C18 column (250mm × 4.6mm, 5.0μ particle size) under specific stress conditions using acetonitrile – 0.02M ammonium acetate buffer (60: 40, v/v) as a solvent system with a flow rate of 1.0mL/min. Quantification and linearity was achieved at 260nm over the concentration range of 5-30μg/mL for Leflunomide. The investigated method was validated as per guidelines.
{"title":"Development and Validation of Stability Indicating High Performance Liquid Chromatography Method for Determination of Leflunomide","authors":"Adhao Vaibhav S., Ambhore Jaya P., Thenge Raju R.","doi":"10.52711/2231-5675.2023.00016","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00016","url":null,"abstract":"A new simple, specific, accurate and precise RP-HPLC method was developed for determination of Leflunomide. In the present study, stress testing of Leflunomide was carried out according to ICH guidelines Q1A (R2). Leflunomide was subjected to stress conditions of hydrolysis, oxidation, photolysis and neutral decomposition. Effective separation of drug and degradant was achieved was achieved on a Hypersil BDS C18 column (250mm × 4.6mm, 5.0μ particle size) under specific stress conditions using acetonitrile – 0.02M ammonium acetate buffer (60: 40, v/v) as a solvent system with a flow rate of 1.0mL/min. Quantification and linearity was achieved at 260nm over the concentration range of 5-30μg/mL for Leflunomide. The investigated method was validated as per guidelines.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"26 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80150172","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-06-03DOI: 10.52711/2231-5675.2023.00015
K. Pravalika, M. Swamy, J. S. Reddy, K. A. Saraswathy, Samyuktha Metta
From this article, bio-analytical styles are extensively used to find the amount of medicines and their intermediate derivatives in tube matrices and the styles should be practical to acquisition in areas of mortal clinical and in human study. Bio-analytical system employed for the quantitative estimation of medicines and their metabolites in natural media and plays an essential portion in computation and rendition of BE, PK, and TK survey. The leading BA part is system improvement, system confirmation, and statistical distribution investigation. Ways similar as HPLC and LC conjugated LCMS- MS are utilized for the BA of medicines in body.
{"title":"Bioanalytical Method Developments for Bioanalysis of Drugs","authors":"K. Pravalika, M. Swamy, J. S. Reddy, K. A. Saraswathy, Samyuktha Metta","doi":"10.52711/2231-5675.2023.00015","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00015","url":null,"abstract":"From this article, bio-analytical styles are extensively used to find the amount of medicines and their intermediate derivatives in tube matrices and the styles should be practical to acquisition in areas of mortal clinical and in human study. Bio-analytical system employed for the quantitative estimation of medicines and their metabolites in natural media and plays an essential portion in computation and rendition of BE, PK, and TK survey. The leading BA part is system improvement, system confirmation, and statistical distribution investigation. Ways similar as HPLC and LC conjugated LCMS- MS are utilized for the BA of medicines in body.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"23 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"78171032","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.52711/2231-5675.2023.00004
Jyoti D. Ghogare, Pranita Panchal, Sayali P. Rathod, U. T. Jadhao
Chromatography is non-destructive procedure for resolving a multi-component mixture of solids, gases, Liquids. HPTLC is use of validated methods for qualitative and quantitative analysis. HPTLC is playing an important role in analytical world and a complementary method for HPLC. The analytical method was evaluated by using parameters such as Linearity, Precision, Accuracy, Limit of detection and Limit of quantification, Specificity, Robustness. In this method 100ng µL-1 and 750ng µL-1 volume of standard stock solutions of Nortriptyline and Pregabalin were taken, respectively. The mobile phase contains Toluene: Ethyl acetate: Methanol (6: 2: 1, v/v/v). Standard stock solutions were applied by over spotting on HPTLC plate with the help of CAMAG 100µl sample syringe, Linomat 5 sample applicator. The development chamber was saturated for 15 min. The plate was scanned at 210nm. The retention factors of PREGA and NORT were found to be PREGA: 0.48±0.03, NORT: 0.70±0.07. The % drug content (mean±S.D.) were found to be 99.32±1.39 for NORT and 99.75±1.15 for PREGA. The results of stress degradation studies revealed that NORT was prone to hydrolysis, oxidative, thermal and photolytic degradation whereas PREGA was found susceptible to hydrolysis, oxidative, thermal degradation but stable under photolytic stress conditions.
{"title":"Stability Indicating HPTLC Method Development and Validation for Estimation of Nortriptyline and Pregabalin in Tablet Dosage Form","authors":"Jyoti D. Ghogare, Pranita Panchal, Sayali P. Rathod, U. T. Jadhao","doi":"10.52711/2231-5675.2023.00004","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00004","url":null,"abstract":"Chromatography is non-destructive procedure for resolving a multi-component mixture of solids, gases, Liquids. HPTLC is use of validated methods for qualitative and quantitative analysis. HPTLC is playing an important role in analytical world and a complementary method for HPLC. The analytical method was evaluated by using parameters such as Linearity, Precision, Accuracy, Limit of detection and Limit of quantification, Specificity, Robustness. In this method 100ng µL-1 and 750ng µL-1 volume of standard stock solutions of Nortriptyline and Pregabalin were taken, respectively. The mobile phase contains Toluene: Ethyl acetate: Methanol (6: 2: 1, v/v/v). Standard stock solutions were applied by over spotting on HPTLC plate with the help of CAMAG 100µl sample syringe, Linomat 5 sample applicator. The development chamber was saturated for 15 min. The plate was scanned at 210nm. The retention factors of PREGA and NORT were found to be PREGA: 0.48±0.03, NORT: 0.70±0.07. The % drug content (mean±S.D.) were found to be 99.32±1.39 for NORT and 99.75±1.15 for PREGA. The results of stress degradation studies revealed that NORT was prone to hydrolysis, oxidative, thermal and photolytic degradation whereas PREGA was found susceptible to hydrolysis, oxidative, thermal degradation but stable under photolytic stress conditions.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"28 11","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"72607859","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.52711/2231-5675.2023.00001
Shweta Ubale, Mayuri V. Bhosale, S. K. Parajne
Aim of this study is to develop a new, precise, sensitive, simple, efficient, selective, and accurate high-performance liquid chromatographic method for the separation and determination of Deferiprone and its impurity in the capsule dosage form. A wide-range of literature survey disclosed no method for estimation said as the above. The chromatographic separation was achieved on Agilent Zorbax Bonus-RP (250 x 4.6mm, 5µ) with a mobile phase of Methanol: 0.1% O-Phosphoric acid (10:90, % v/v) combination in 1000ml of Methanol: Water (50: 50, % v/v) using a diluent. The flow rate of 1mL/min and UV detection at 280nm use as wavelength. The developed method was validated as reported by ICH guidelines. The linearity of the calibration curve for deferiprone and its process-related impurity in the concentration range of 4.0-6.0μg/ml. There exists a good correlation between peak area and analyte concentration. The retention time for deferiprone was discovered to be 2.29 min and its impurity was 8.65min. Deferiprone's relative standard deviation value is 0.45 and its process-related impurity is 0.17. All the results tell that the proposed method was highly sensitive, simple, precise, accurate, and fast. A large number of samples can be analyzed in a shorter time due to shorter retention times, so it can be successfully applied for routine analysis of Deferiprone and related impurity (maltol) in pharmaceutical dosage forms.
本研究的目的是建立一种新的、精确、灵敏、简便、高效、选择性和准确性高的高效液相色谱分离测定胶囊剂型中去铁素及其杂质的方法。广泛的文献调查没有发现上述估计方法。色谱分离采用Agilent Zorbax plus - rp (250 × 4.6mm, 5µ)，流动相为甲醇:0.1% o -磷酸(10:90，% v/v)， 1000ml甲醇:水(50:50，% v/v)，使用稀释剂。流速为1mL/min，波长为280nm紫外检测。所开发的方法根据ICH指南进行了验证。在4.0 ~ 6.0μg/ml范围内，去铁素及其工艺相关杂质的线性关系良好。峰面积与分析物浓度之间存在良好的相关性。结果表明，去铁素的保留时间为2.29 min，杂质保留时间为8.65min。去铁矾的相对标准偏差值为0.45，工艺相关杂质值为0.17。结果表明，该方法灵敏度高，操作简便，精密度高，准确度高，速度快。由于保留时间较短，可在较短时间内分析大量样品，因此可成功应用于药物剂型中去铁素及相关杂质(麦芽糖醇)的常规分析。
{"title":"Development and Validation of RP HPLC Method for Estimation of Deferiprone and its Related Impurityin Pharmaceutical Dosage Form","authors":"Shweta Ubale, Mayuri V. Bhosale, S. K. Parajne","doi":"10.52711/2231-5675.2023.00001","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00001","url":null,"abstract":"Aim of this study is to develop a new, precise, sensitive, simple, efficient, selective, and accurate high-performance liquid chromatographic method for the separation and determination of Deferiprone and its impurity in the capsule dosage form. A wide-range of literature survey disclosed no method for estimation said as the above. The chromatographic separation was achieved on Agilent Zorbax Bonus-RP (250 x 4.6mm, 5µ) with a mobile phase of Methanol: 0.1% O-Phosphoric acid (10:90, % v/v) combination in 1000ml of Methanol: Water (50: 50, % v/v) using a diluent. The flow rate of 1mL/min and UV detection at 280nm use as wavelength. The developed method was validated as reported by ICH guidelines. The linearity of the calibration curve for deferiprone and its process-related impurity in the concentration range of 4.0-6.0μg/ml. There exists a good correlation between peak area and analyte concentration. The retention time for deferiprone was discovered to be 2.29 min and its impurity was 8.65min. Deferiprone's relative standard deviation value is 0.45 and its process-related impurity is 0.17. All the results tell that the proposed method was highly sensitive, simple, precise, accurate, and fast. A large number of samples can be analyzed in a shorter time due to shorter retention times, so it can be successfully applied for routine analysis of Deferiprone and related impurity (maltol) in pharmaceutical dosage forms.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"4 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84667082","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.52711/2231-5675.2023.00003
S. Reddy, L. Thomas, V. P., Arindam Mukhopadhyay, Saral Thangam
A LCMS/MS method for the simultaneous determination of ampicillin and sulbactam in human plasma was described. After protein precipitation using 2mL of acetonitrile, 250µL of supernatant was mixed with 1.000 mL of 0.1% Acetic Acid in Milli-Q-water. 10µL was injected to a Biobasic AX column and eluted with 10mM Ammonium acetate and Acetonitrile: 60:40, v/v at a flow rate of 0.5mL/min. MRM transitions were monitored in negative mode as m/z 348.1 → 206.8 (AMP), 231.9 → 187.8 (SUL) and m/z 353.0 → 211.9 (AMP D5). Sample concentrations were calculated by linear regression analysis using the analyst software1.6.3. An excellent linear response was obtained over the concentration ranges 0.1040µg/mL to 10.1562µg/mL for Ampicillin and 0.0510µg/mL to 6.1552µg/mL for Sulbactam. The intra-day and inter-day precision were within 3.50% for all analytes. The assay accuracy was 96.27 –103.59 %. Mean recoveries were 84.51% and 98.54% for ampicillin and sulbactam, respectively. The limits of detections were 0.026µg/mL and 0.013µg/mL for ampicillin and sulbactam. This method was successfully used for a bioequivalence study.
{"title":"Simultaneous Estimation of Ampicillin and Sulbactam in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry","authors":"S. Reddy, L. Thomas, V. P., Arindam Mukhopadhyay, Saral Thangam","doi":"10.52711/2231-5675.2023.00003","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00003","url":null,"abstract":"A LCMS/MS method for the simultaneous determination of ampicillin and sulbactam in human plasma was described. After protein precipitation using 2mL of acetonitrile, 250µL of supernatant was mixed with 1.000 mL of 0.1% Acetic Acid in Milli-Q-water. 10µL was injected to a Biobasic AX column and eluted with 10mM Ammonium acetate and Acetonitrile: 60:40, v/v at a flow rate of 0.5mL/min. MRM transitions were monitored in negative mode as m/z 348.1 → 206.8 (AMP), 231.9 → 187.8 (SUL) and m/z 353.0 → 211.9 (AMP D5). Sample concentrations were calculated by linear regression analysis using the analyst software1.6.3. An excellent linear response was obtained over the concentration ranges 0.1040µg/mL to 10.1562µg/mL for Ampicillin and 0.0510µg/mL to 6.1552µg/mL for Sulbactam. The intra-day and inter-day precision were within 3.50% for all analytes. The assay accuracy was 96.27 –103.59 %. Mean recoveries were 84.51% and 98.54% for ampicillin and sulbactam, respectively. The limits of detections were 0.026µg/mL and 0.013µg/mL for ampicillin and sulbactam. This method was successfully used for a bioequivalence study.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"120 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"86148933","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.52711/2231-5675.2023.00006
P. Pankaj, Pramod Kumar, Aman Kapoor, P. Priyanka, Puneet Kumar, Saweta Kumari
LC-TOF-MS is powerful analytical technique. It is a combination of two techniques one of which is belongs to chromatography and other is from spectroscopy. Chromatography is separation technique and perform both techniques separately it is very time consuming but combined both techniques to save time and provide better results. This represents the potential of liquid chromatography with (quadrupole) time-of-flight mass spectrometry [LC-(Q)TOF-MS] in examining the presence of pesticide metabolites in food and water samples. This method portrays a quick enhanced screen for blood and urine specimens in post-mortem, driving under the influence and drug facilitated sexual assault forensic toxicology casework. (LC–MS) is an analytical technique that amalgamate the physical separation capability of liquid chromatography with the mass analysis capability of mass-spectrometry (MS).This technique can be used in analysis of pharmacokinetics, proteomics/metabolomics, development drug, analysis of pesticides in vegetables, analysis of medicinal panaxherbs for metabolomic research, identification of diphenhydramine in segment sample, investigation of pesticides metabolites in food and water etc.
{"title":"LC–Tof-Ms an Influential Hyphenated Technique and its Application","authors":"P. Pankaj, Pramod Kumar, Aman Kapoor, P. Priyanka, Puneet Kumar, Saweta Kumari","doi":"10.52711/2231-5675.2023.00006","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00006","url":null,"abstract":"LC-TOF-MS is powerful analytical technique. It is a combination of two techniques one of which is belongs to chromatography and other is from spectroscopy. Chromatography is separation technique and perform both techniques separately it is very time consuming but combined both techniques to save time and provide better results. This represents the potential of liquid chromatography with (quadrupole) time-of-flight mass spectrometry [LC-(Q)TOF-MS] in examining the presence of pesticide metabolites in food and water samples. This method portrays a quick enhanced screen for blood and urine specimens in post-mortem, driving under the influence and drug facilitated sexual assault forensic toxicology casework. (LC–MS) is an analytical technique that amalgamate the physical separation capability of liquid chromatography with the mass analysis capability of mass-spectrometry (MS).This technique can be used in analysis of pharmacokinetics, proteomics/metabolomics, development drug, analysis of pesticides in vegetables, analysis of medicinal panaxherbs for metabolomic research, identification of diphenhydramine in segment sample, investigation of pesticides metabolites in food and water etc.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"148 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"75062934","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Pub Date : 2023-03-22DOI: 10.52711/2231-5675.2023.00009
Nachiket V. Rajput, Manvir V. Rajput, Vikas V. Patil, Pankaj S. Patil, Amol R. Pawar
Chromatography is a technique which is used for the separation of constituents in a mixture. HPLC is an advanced technique of column liquid chromatography. This article represents a short review of HPLC along with its principle and instrumentation. It describes about new trends in HPLC such as RRLC, UPLC, UFLC and Nano LC. Recent developments in chromatographic supports and instrumentation for liquid chromatography (LC) are enabling rapid and highly efficient separations. This new category of analytical separation science retains the practicality and principles of HPLC while increasing the overall interrelated attributes of speed, sensitivity and resolution. Today’s pharmaceutical industries are looking for new ways to cut cost and shorten time for development of drugs while at the same time improving the quality of their products and analytical laboratories are not exception in this trend. New techniques have mainly increased the resolution power for complex sample analysis.
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