首页 > 最新文献

Asian Journal of Pharmaceutical Analysis最新文献

英文 中文
A New Analytical RP-HPLC Method for the Estimation of Letrozole in Pure and Tablet form 用反相高效液相色谱法测定来曲唑的纯度和片剂含量
Pub Date : 2023-06-03 DOI: 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.
建立了一种简便、快速、特异、准确的反相高效液相色谱法,用于来曲唑原料药和市售药品剂型的验证。色谱柱为Symmetry ODS C18 (4.6×250mm, 5µm),流动相为甲醇:磷酸盐缓冲液(35:65),流速为1.0mL min - 1,紫外检测波长为240nm;恒温柱温度为室温。在这些色谱条件下运行时间小于8 min。来曲唑的保留时间为2.252。在6 ~ 14μg mL−1的浓度范围内,校正图呈线性关系,检出限和定量限分别为1.2和3.6ng mL−1。市售制剂的平均含量为99.86%,回收率为98 ~ 102%。精密度研究的相对标准偏差<2%。该方法简便、精密度高、专属性好、准确、快速,适用于来曲唑原料药和市售药品剂型的评价。
{"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}
引用次数: 0
Analytical Technique for Carvedilol and Ivabradine determination from pure and Pharmaceutical Dosage Forms: A Review 卡维地洛和伊伐布雷定纯剂型和制剂剂型的分析技术综述
Pub Date : 2023-06-03 DOI: 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.
卡维地洛和伊伐布雷定是一种用于治疗心血管疾病,如高血压、慢性稳定型心绞痛和慢性心力衰竭的药物组合。两者的行动方式不同。卡维地洛通过抑制肾上腺素受体来预防运动引起的心动过速卡维地洛还对α -1肾上腺素能受体起作用并整体降低血压。在较高剂量的情况下也显示抗氧化和钙通道阻断活性。伊伐布雷定是一种降低心率的药物,通过选择性和特异性地阻断心脏起搏器电流(If)起作用。本文主要介绍了卡维地洛和伊瓦布雷定的药理学特征、作用机制、药代动力学和药效学研究,以及卡维地洛和伊瓦布雷定的分析方法。各种方法,如紫外光谱高效液相色谱,反相高效液相色谱,超高效液相色谱。本文综述了卡维地洛和伊瓦布雷定的各种分析方法。
{"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}
引用次数: 0
Novel Method Development, Validation and Stability Indicating Assay Method for Rivastigmine Tartarate Capsule by HPLC 酒石酸利瓦斯丁胶囊HPLC测定方法的建立、验证及稳定性分析
Pub Date : 2023-06-03 DOI: 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.
本研究旨在建立酒石酸利瓦斯汀胶囊1.5mg的定量分析方法并进行验证。建立了以反相C-8为色谱柱,流动相为缓冲液(pH 3.0)的等容高效液相色谱法,并对其进行了优化和验证。流速为1.5 ml/min,温度为500C,波长为λmax - 220nm。11min时观察酒石酸利瓦斯汀的色谱图。酒石酸利瓦斯汀在220nm下11.29 min被完全洗脱。该方法具有良好的线性、准确度、选择性等验证参数。在102%的范围内,各浓度水平下的回收率(准确度)均大于100%。采用HPLC法计算5区重复120ppm的相对偏差百分比(%RSD)来确定系统的适用性。酒石酸利瓦斯汀的稳定性表明,必须验证的测定方法总是要求氧化、酸、碱、水解、热和光解降解的强制降解条件。酒石酸利瓦斯汀在碱降解条件下降解显著,而在热、热湿、光解、酸和氧化应激条件下降解效果不明显。
{"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}
引用次数: 0
Development and Validation of Stability Indicating High Performance Liquid Chromatography Method for Determination of Leflunomide 来氟米特高效液相色谱测定方法的建立及稳定性验证
Pub Date : 2023-06-03 DOI: 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.
建立了一种简便、特异、准确、精密度高的来氟米特反相高效液相色谱测定方法。在本研究中,来氟米特的压力测试按照ICH指南Q1A (R2)进行。来氟米特经历了水解、氧化、光解和中性分解的应激条件。以乙腈- 0.02M醋酸铵缓冲液(60∶40,v/v)为溶剂体系,流速为1.0mL/min,在特定应力条件下,在Hypersil BDS C18色谱柱(250mm × 4.6mm, 5.0μ粒径)上实现了药物与降解物的有效分离。来氟米特在260nm的浓度范围为5-30μg/mL,在线性范围内定量。根据指南对所研究的方法进行了验证。
{"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}
引用次数: 0
Bioanalytical Method Developments for Bioanalysis of Drugs 药物生物分析的生物分析方法发展
Pub Date : 2023-06-03 DOI: 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.
从这篇文章中可以看出,生物分析方法被广泛应用于药物及其中间衍生物在试管基质中的含量的测定,这种方法应该在致命临床和人体研究领域具有实用性。生物分析系统用于自然介质中药物及其代谢物的定量估计,在BE、PK和TK调查的计算和再现中起着重要作用。BA的主要部分是系统改进、系统确认和统计分布调查。采用类似HPLC和LC共轭LCMS- MS的方法测定药物在体内的BA。
{"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}
引用次数: 0
Stability Indicating HPTLC Method Development and Validation for Estimation of Nortriptyline and Pregabalin in Tablet Dosage Form 高效液相色谱法测定片剂中去甲替林和普瑞巴林含量的方法建立与验证
Pub Date : 2023-03-22 DOI: 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.
色谱法是一种非破坏性的方法,用于分离固体、气体、液体的多组分混合物。HPTLC是使用经过验证的方法进行定性和定量分析。HPTLC作为HPLC的补充方法,在分析界发挥着重要的作用。采用线性度、精密度、准确度、检出限和定量限、特异性、稳健性等指标对分析方法进行评价。本方法取去甲替林标准原液100ngµL-1,普瑞巴林标准原液750ngµL-1体积。流动相为甲苯:乙酸乙酯:甲醇(6:2:1,v/v/v)。在CAMAG 100µl样品注射器、Linomat 5样品涂布器的帮助下,将标准原液在HPTLC板上过点。显影室饱和15分钟。在210nm处扫描板。PREGA和NORT的保留因子分别为:PREGA: 0.48±0.03,NORT: 0.70±0.07。NORT和PREGA的药物含量(平均±S.D.)分别为99.32±1.39和99.75±1.15。应力降解研究结果表明,NORT易被水解、氧化、热、光解降解,而PREGA易被水解、氧化、热降解,但在光解胁迫条件下稳定。
{"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}
引用次数: 0
Development and Validation of RP HPLC Method for Estimation of Deferiprone and its Related Impurityin Pharmaceutical Dosage Form 反相高效液相色谱法测定制剂中去铁素及其相关杂质的方法建立与验证
Pub Date : 2023-03-22 DOI: 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}
引用次数: 0
Simultaneous Estimation of Ampicillin and Sulbactam in Human Plasma by Liquid Chromatography Tandem Mass Spectrometry 液相色谱串联质谱法同时测定人血浆中氨苄西林和舒巴坦
Pub Date : 2023-03-22 DOI: 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.
建立了同时测定人血浆中氨苄西林和舒巴坦含量的LCMS/MS方法。用2mL乙腈沉淀蛋白质后,取250µL上清液与1.000 mL 0.1%醋酸在milliq -water中混合。将10µL注入biobbasic AX柱,用10mM乙酸铵和乙腈:60:40,v/v,流速0.5mL/min洗脱。在负模式下监测MRM转换为m/z 348.1→206.8 (AMP), 231.9→187.8 (SUL)和m/z 353.0→211.9 (AMP D5)。使用分析软件1.6.3进行线性回归分析,计算样品浓度。氨苄西林在0.1040µg/mL ~ 10.1562µg/mL范围内、舒巴坦在0.0510µg/mL ~ 6.1552µg/mL范围内具有良好的线性响应。所有分析物的日内和日内精密度均在3.50%以内。测定准确度为96.27 ~ 103.59%。氨苄西林和舒巴坦的平均加样回收率分别为84.51%和98.54%。氨苄西林、舒巴坦的检出限分别为0.026µg/mL和0.013µg/mL。该方法成功地用于生物等效性研究。
{"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}
引用次数: 0
LC–Tof-Ms an Influential Hyphenated Technique and its Application LC-Tof-Ms连接技术及其应用
Pub Date : 2023-03-22 DOI: 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.
LC-TOF-MS是一种强大的分析技术。它是两种技术的结合,一种属于色谱法,另一种来自光谱学。色谱法是一种分离技术,单独执行两种技术非常耗时,但将两种技术结合起来可以节省时间并提供更好的结果。这代表了液相色谱(四极杆)飞行时间质谱[LC-(Q)TOF-MS]在检测食品和水样中农药代谢物存在方面的潜力。该方法可在尸体解剖、酒后驾车和吸毒导致的性侵犯法医毒理学案件中快速增强血液和尿液样本的筛选。LC-MS是一种将液相色谱的物理分离能力与质谱的质量分析能力相结合的分析技术。该技术可用于药物代谢动力学分析、蛋白质组学/代谢组学分析、药物开发、蔬菜中农药分析、药用人参代谢组学分析、区段样品中苯海拉明的鉴定、食品和水中农药代谢物的调查等。
{"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}
引用次数: 0
Short Review on Comparative Study of Chromatography 色谱比较研究述评
Pub Date : 2023-03-22 DOI: 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.
色谱法是一种用于分离混合物成分的技术。高效液相色谱法是一种先进的柱液相色谱技术。本文简要介绍了高效液相色谱法及其原理和仪器。介绍了高效液相色谱(RRLC)、超高效液相色谱(ulc)、超高效液相色谱(UFLC)和纳米高效液相色谱(Nano LC)的发展趋势。液相色谱(LC)的色谱支架和仪器的最新发展使快速高效的分离成为可能。这种新的分析分离科学保留了HPLC的实用性和原理,同时增加了速度、灵敏度和分辨率的总体相关属性。今天的制药行业正在寻找新的方法来降低成本和缩短药物的开发时间,同时提高产品的质量,分析实验室也不例外。新技术主要提高了复杂样品分析的分辨能力。
{"title":"Short Review on Comparative Study of Chromatography","authors":"Nachiket V. Rajput, Manvir V. Rajput, Vikas V. Patil, Pankaj S. Patil, Amol R. Pawar","doi":"10.52711/2231-5675.2023.00009","DOIUrl":"https://doi.org/10.52711/2231-5675.2023.00009","url":null,"abstract":"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.","PeriodicalId":8547,"journal":{"name":"Asian Journal of Pharmaceutical Analysis","volume":"43 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"85884455","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}
引用次数: 0
期刊
Asian Journal of Pharmaceutical Analysis
全部 Acc. Chem. Res. ACS Applied Bio Materials ACS Appl. Electron. Mater. ACS Appl. Energy Mater. ACS Appl. Mater. Interfaces ACS Appl. Nano Mater. ACS Appl. Polym. Mater. ACS BIOMATER-SCI ENG ACS Catal. ACS Cent. Sci. ACS Chem. Biol. ACS Chemical Health & Safety ACS Chem. Neurosci. ACS Comb. Sci. ACS Earth Space Chem. ACS Energy Lett. ACS Infect. Dis. ACS Macro Lett. ACS Mater. Lett. ACS Med. Chem. Lett. ACS Nano ACS Omega ACS Photonics ACS Sens. ACS Sustainable Chem. Eng. ACS Synth. Biol. Anal. Chem. BIOCHEMISTRY-US Bioconjugate Chem. BIOMACROMOLECULES Chem. Res. Toxicol. Chem. Rev. Chem. Mater. CRYST GROWTH DES ENERG FUEL Environ. Sci. Technol. Environ. Sci. Technol. Lett. Eur. J. Inorg. Chem. IND ENG CHEM RES Inorg. Chem. J. Agric. Food. Chem. J. Chem. Eng. Data J. Chem. Educ. J. Chem. Inf. Model. J. Chem. Theory Comput. J. Med. Chem. J. Nat. Prod. J PROTEOME RES J. Am. Chem. Soc. LANGMUIR MACROMOLECULES Mol. Pharmaceutics Nano Lett. Org. Lett. ORG PROCESS RES DEV ORGANOMETALLICS J. Org. Chem. J. Phys. Chem. J. Phys. Chem. A J. Phys. Chem. B J. Phys. Chem. C J. Phys. Chem. Lett. Analyst Anal. Methods Biomater. Sci. Catal. Sci. Technol. Chem. Commun. Chem. Soc. Rev. CHEM EDUC RES PRACT CRYSTENGCOMM Dalton Trans. Energy Environ. Sci. ENVIRON SCI-NANO ENVIRON SCI-PROC IMP ENVIRON SCI-WAT RES Faraday Discuss. Food Funct. Green Chem. Inorg. Chem. Front. Integr. Biol. J. Anal. At. Spectrom. J. Mater. Chem. A J. Mater. Chem. B J. Mater. Chem. C Lab Chip Mater. Chem. Front. Mater. Horiz. MEDCHEMCOMM Metallomics Mol. Biosyst. Mol. Syst. Des. Eng. Nanoscale Nanoscale Horiz. Nat. Prod. Rep. New J. Chem. Org. Biomol. Chem. Org. Chem. Front. PHOTOCH PHOTOBIO SCI PCCP Polym. Chem.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
×
提示
确定
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1