K. Palandurkar, Richie Bhandre, S. H. Boddu, Minal T. Harde, Sameer S Lakade, Ujjwala Y. Kandekar, Prashant Waghmare
A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.
{"title":"Quality risk assessment and DoE – Practiced validated stability-indicating chromatographic method for quantification of Rivaroxaban in bulk and tablet dosage form","authors":"K. Palandurkar, Richie Bhandre, S. H. Boddu, Minal T. Harde, Sameer S Lakade, Ujjwala Y. Kandekar, Prashant Waghmare","doi":"10.1556/1326.2021.00978","DOIUrl":"https://doi.org/10.1556/1326.2021.00978","url":null,"abstract":"\u0000 A systematic DoE and Analytical Quality by Design (AQbD) approach was utilized for the development and validation of a novel stability indicating high-performance thin–layer chromatographic (HPTLC) method for Rivaroxaban (RBN) estimation in bulk and marketed formulation. A D-optimal design was used to screen the effect of solvents, volume of solvents, time from spotting to development and time for development to scanning. ANOVA results and Pareto chart revealed that toluene, methanol, water and saturation time had an impact on retention time. The critical method and material attributes were further screened by Box-Behnken design (BBD) to achieve optimal chromatographic condition. A stress degradation study was carried out and structure of major alkaline degradant was elaborated. According to the design space, a control strategy was used with toluene: methanol: water (6:2:2) and the saturation time was 15 min. A retention factor (RF) of 0.59 ± 0.05 was achieved for RBN using chromatographic plate precoated with silica gel at detection wavelength 282 nm with optimized conditions. The linear calibration curve was achieved in the concentration range of 200–1,200 ng/band with r\u0000 2 > 0.998 suggesting good coordination between analyte concentration and peak areas. The quadratic model was demonstrated as the best fit model and no interaction was noted between CMAs. The optimized HPTLC method was validated critically as stated in International Conference on Harmonization (ICH) Q2 (R1) guideline and implemented successfully for stress degradation study of RBN. The developed HPTLC method obtained through AQbD application was potentially able to resolve all degradants of RBN achieved through forced degradation study. The obtained results demonstrate that a scientific AQbD approach implementation in HPTLC method development and stress degradation study drastically minimizes the number of trials in experiments, ultimately time and cost of analysis could be minimized.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2022-01-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42402893","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Libin Wang, Kun Shang, Xiaorui Zhang, Xin-Yuan Zhang, Tian Feng, Xu Xiaohui, Fang Wang
A sensitive and accurate LC-MS/MS method was developed and validated for the simultaneous quantification of rivaroxaban (RIV) and sitagliptin (SIT) in rat plasma using apixaban as internal standard (IS). An Agilent Eclipse plus C18 column (2.1 × 100 mm, 3.5 µm, Agilent) was used for chromatographic separation with isocratic elution. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 436.8→144.9 for RIV, m/z 407.7→173.8 for SIT, m/z 459.8→442.8 for IS. The procedure of method validation included selectivity, linearity, precision, accuracy, matrix effect, extraction recovery and stability were conducted according to the guidelines of EMA and FDA. The results indicated that no obvious drug-drug interactions occurred might be owing to their differences in metabolic pathways.
建立了以阿哌沙班为内标(IS)同时定量大鼠血浆中利伐沙班(RIV)和西格列汀(SIT)的灵敏、准确的LC-MS/MS方法。采用Agilent Eclipse加C18色谱柱(2.1 × 100 mm, 3.5µm, Agilent)，等密度洗脱进行色谱分离。多反应监测(MRM)采用正离子ESI模式监测RIV的m/z 436.8→144.9、SIT的m/z 407.7→173.8、IS的m/z 459.8→442.8的离子跃迁。方法验证包括选择性、线性度、精密度、准确度、基质效应、提取回收率和稳定性，验证过程按照EMA和FDA的指导原则进行。结果表明，两种药物之间没有发生明显的相互作用，这可能是由于它们的代谢途径不同所致。
{"title":"Simultaneous determination of rivaroxaban and sitagliptin in rat plasma by LC–MS/MS and its application to pharmacokinetic drug-drug interaction study","authors":"Libin Wang, Kun Shang, Xiaorui Zhang, Xin-Yuan Zhang, Tian Feng, Xu Xiaohui, Fang Wang","doi":"10.1556/1326.2021.00988","DOIUrl":"https://doi.org/10.1556/1326.2021.00988","url":null,"abstract":"\u0000 A sensitive and accurate LC-MS/MS method was developed and validated for the simultaneous quantification of rivaroxaban (RIV) and sitagliptin (SIT) in rat plasma using apixaban as internal standard (IS). An Agilent Eclipse plus C18 column (2.1 × 100 mm, 3.5 µm, Agilent) was used for chromatographic separation with isocratic elution. Multiple reaction monitoring (MRM) using positive-ion ESI mode to monitor ion transitions of m/z 436.8→144.9 for RIV, m/z 407.7→173.8 for SIT, m/z 459.8→442.8 for IS. The procedure of method validation included selectivity, linearity, precision, accuracy, matrix effect, extraction recovery and stability were conducted according to the guidelines of EMA and FDA. The results indicated that no obvious drug-drug interactions occurred might be owing to their differences in metabolic pathways.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44260605","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Yuhki Sato, Ayana Michihara, K. Yamamoto, M. Shirakawa, H. Katayama
Several studies on the pharmacokinetic parameters of antidementia drugs have reported that plasma concentration is linked to the drugs’ efficacy and adverse effects. At present, there is no quantitation method that is highly sensitive and can be applied to simultaneous monitoring of the pharmacokinetics of rivastigmine and its metabolites (NAP 226-90) in rat plasma. No methods fulfilling the assay validation requirements of the US Food and Drug Administration and the European Medicines Agency was also established. Therefore, this study developed a quantitative method for measuring rivastigmine and NAP 226-90 concentrations using high-performance liquid chromatography and tandem mass spectrometry, examining plasma samples after rivastigmine administration. Rat plasma samples were prepared via the protein precipitation method. The methods for measuring rivastigmine and NAP 226-90 concentrations showed good fit over wide ranges of 1–100 ng mL−1 and 0.5–50 ng mL−1, with lower limits of quantification at 1 ng mL−1 and 0.5 ng mL−1, respectively. The plasma concentrations of rivastigmine and NAP 226-90 in six healthy rats were successfully determined, demonstrating the feasibility of applying the developed method. Thus, this research has successfully developed a sensitive, selective method, to simultaneously quantify rivastigmine and NAP 226-90 concentrations in rat plasma and be applicable to a pharmacokinetic study.
几项关于抗痴呆药物药代动力学参数的研究报告称，血浆浓度与药物的疗效和不良反应有关。目前，还没有一种高灵敏度的定量方法可以同时监测利伐他明及其代谢物（NAP 226-90）在大鼠血浆中的药代动力学。也没有建立符合美国食品药品监督管理局和欧洲药品管理局化验验证要求的方法。因此，本研究开发了一种使用高效液相色谱法和串联质谱法测定利伐他明和NAP 226-90浓度的定量方法，并检查了给药后的血浆样品。通过蛋白质沉淀法制备大鼠血浆样品。测定利瓦斯汀和NAP 226-90浓度的方法在1-100的宽范围内显示出良好的拟合性 ng mL−1和0.5–50 ng mL−1，定量下限为1 ng mL−1和0.5 ng mL−1。成功测定了6只健康大鼠的利瓦斯汀和NAP 226-90的血浆浓度，证明了应用该方法的可行性。因此，本研究成功地开发了一种灵敏、选择性的方法，可以同时定量大鼠血浆中的利瓦斯汀和NAP 226-90浓度，并适用于药代动力学研究。
{"title":"High performance liquid chromatography coupled with mass spectrometry for simultaneous determination of rivastigmine and its metabolite in rat plasma","authors":"Yuhki Sato, Ayana Michihara, K. Yamamoto, M. Shirakawa, H. Katayama","doi":"10.1556/1326.2021.00989","DOIUrl":"https://doi.org/10.1556/1326.2021.00989","url":null,"abstract":"\u0000 Several studies on the pharmacokinetic parameters of antidementia drugs have reported that plasma concentration is linked to the drugs’ efficacy and adverse effects. At present, there is no quantitation method that is highly sensitive and can be applied to simultaneous monitoring of the pharmacokinetics of rivastigmine and its metabolites (NAP 226-90) in rat plasma. No methods fulfilling the assay validation requirements of the US Food and Drug Administration and the European Medicines Agency was also established. Therefore, this study developed a quantitative method for measuring rivastigmine and NAP 226-90 concentrations using high-performance liquid chromatography and tandem mass spectrometry, examining plasma samples after rivastigmine administration. Rat plasma samples were prepared via the protein precipitation method. The methods for measuring rivastigmine and NAP 226-90 concentrations showed good fit over wide ranges of 1–100 ng mL−1 and 0.5–50 ng mL−1, with lower limits of quantification at 1 ng mL−1 and 0.5 ng mL−1, respectively. The plasma concentrations of rivastigmine and NAP 226-90 in six healthy rats were successfully determined, demonstrating the feasibility of applying the developed method. Thus, this research has successfully developed a sensitive, selective method, to simultaneously quantify rivastigmine and NAP 226-90 concentrations in rat plasma and be applicable to a pharmacokinetic study.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44305305","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Wenjing Shi, DI Haixiao, Bo Pang, Huixin Jin, Hongtao Liu, Bo Qiu, Bingnan Ren, Guoxun Pang
Bicalutamide (BCL) has been approved for treatment of advanced prostate cancer (Pca), and vitamin D is inevitably used in combination with BCL in Pca patients for skeletal or anti-tumor strategies. Therefore, it is necessary to study the effect of vitamin D application on the pharmacokinetics of BCL. We developed and validated a specific, sensitive and rapid UHPLC–MS/MS method to investigate the pharmacokinetic behaviours of BCL in rat plasma with and without the combined use of vitamin D. Plasma samples were extracted by protein precipitation with ether/dichloromethane (2:1 v/v), and the analytes were separated by a Kinetex Biphenyl 100A column (2.1 × 100 mm, 2.6 μm) with a mobile phase composed of 0.5 mM ammonium acetate (PH 6.5) in water (A) and acetonitrile (B) in a ratio of A:B = 35:65 (v/v). Analysis of the ions was run in the multiple reactions monitoring (MRM) mode. The linear range of BCL was 5–2000 ng mL−1. The intra- and inter-day precision were less than 14%, and the accuracy was in the range of 94.4–107.1%. The mean extraction recoveries, matrix effects and stabilities were acceptable for this method. The validated method was successfully applied to evaluate the pharmacokinetic behaviours of BCL in rat plasma. The results demonstrated that the pharmacokinetic property of BCL is significantly affected by combined use of vitamin D, which might help provide useful evidence for the clinical therapy and further pharmacokinetic study.
Bicalutamide（BCL）已被批准用于治疗晚期癌症（Pca），维生素D不可避免地与BCL联合用于Pca患者的骨骼或抗肿瘤策略。因此，有必要研究维生素D的应用对BCL药代动力学的影响。我们开发并验证了一种特异、灵敏、快速的UHPLC–MS/MS方法，以研究BCL在联合使用和不使用维生素D的大鼠血浆中的药代动力学行为。血浆样品用乙醚/二氯甲烷（2:1 v/v）通过蛋白质沉淀提取，分析物用Kinetex联苯100A柱（2.1 × 100 毫米，2.6 μm），流动相为0.5 mM乙酸铵（PH 6.5）在水（A）和乙腈（B）中的溶液，其比例为A∶B＝35:65（v/v）。离子的分析是在多重反应监测（MRM）模式下进行的。BCL的线性范围为5–2000 ng mL−1。日内和日间精密度均小于14%，准确度在94.4–107.1%之间。该方法的平均提取回收率、基质效应和稳定性均合格。经验证的方法已成功应用于评价BCL在大鼠血浆中的药代动力学行为。结果表明，维生素D的联合使用对BCL的药代动力学特性有显著影响，这可能有助于为临床治疗和进一步的药代学研究提供有用的证据。
{"title":"Comparative pharmacokinetic study of bicalutamide administration alone and in combination with vitamin D in rats","authors":"Wenjing Shi, DI Haixiao, Bo Pang, Huixin Jin, Hongtao Liu, Bo Qiu, Bingnan Ren, Guoxun Pang","doi":"10.1556/1326.2021.00995","DOIUrl":"https://doi.org/10.1556/1326.2021.00995","url":null,"abstract":"\u0000 Bicalutamide (BCL) has been approved for treatment of advanced prostate cancer (Pca), and vitamin D is inevitably used in combination with BCL in Pca patients for skeletal or anti-tumor strategies. Therefore, it is necessary to study the effect of vitamin D application on the pharmacokinetics of BCL.\u0000 We developed and validated a specific, sensitive and rapid UHPLC–MS/MS method to investigate the pharmacokinetic behaviours of BCL in rat plasma with and without the combined use of vitamin D. Plasma samples were extracted by protein precipitation with ether/dichloromethane (2:1 v/v), and the analytes were separated by a Kinetex Biphenyl 100A column (2.1 × 100 mm, 2.6 μm) with a mobile phase composed of 0.5 mM ammonium acetate (PH 6.5) in water (A) and acetonitrile (B) in a ratio of A:B = 35:65 (v/v). Analysis of the ions was run in the multiple reactions monitoring (MRM) mode. The linear range of BCL was 5–2000 ng mL−1. The intra- and inter-day precision were less than 14%, and the accuracy was in the range of 94.4–107.1%. The mean extraction recoveries, matrix effects and stabilities were acceptable for this method. The validated method was successfully applied to evaluate the pharmacokinetic behaviours of BCL in rat plasma. The results demonstrated that the pharmacokinetic property of BCL is significantly affected by combined use of vitamin D, which might help provide useful evidence for the clinical therapy and further pharmacokinetic study.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-12-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"48838630","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Zhibin Wang, Mingyu Zhang, Wenbo Zhu, Chunjuan Yang, H. Kuang
A rapid, simple and efficient ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was established to simultaneous determination of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle plasma and evaluated by using esculetin as internal standard. The electrospray ionization (ESI) source was operated in negative ionization mode. Multi-reaction monitoring (MRM) was used to quantitatively analyzed shikonin m/z 287.0 → 217.9, isobutyryl shikonin m/z 357.0 → 268.9, β, βʹ-dimethylacryl alkanin m/z 370.0 → 270.1 and esculetin m/z 177.0 → 89.0, respectively. The method was validated for selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, matrix effect and stability. All validation parameters met the acceptance criteria according to regulatory guidelines. This method was successfully applied for the pharmacokinetic study of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle dogs plasma after oral administration of A. euchroma extract.
{"title":"Simultaneous determination of three naphthoquinones from Arnebia euchroma (Royle) Johnst in beagle plasma by UPLC-MS/MS and application for pharmacokinetics study","authors":"Zhibin Wang, Mingyu Zhang, Wenbo Zhu, Chunjuan Yang, H. Kuang","doi":"10.1556/1326.2021.00982","DOIUrl":"https://doi.org/10.1556/1326.2021.00982","url":null,"abstract":"\u0000 A rapid, simple and efficient ultra-performance liquid chromatography-electrospray ionization-tandem mass spectrometry (UPLC-ESI-MS/MS) method was established to simultaneous determination of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle plasma and evaluated by using esculetin as internal standard. The electrospray ionization (ESI) source was operated in negative ionization mode. Multi-reaction monitoring (MRM) was used to quantitatively analyzed shikonin m/z 287.0 → 217.9, isobutyryl shikonin m/z 357.0 → 268.9, β, βʹ-dimethylacryl alkanin m/z 370.0 → 270.1 and esculetin m/z 177.0 → 89.0, respectively. The method was validated for selectivity, linearity, lower limit of quantification, precision, accuracy, recovery, matrix effect and stability. All validation parameters met the acceptance criteria according to regulatory guidelines. This method was successfully applied for the pharmacokinetic study of shikonin, isobutyryl shikonin, β, βʹ-dimethylacryl alkanin in beagle dogs plasma after oral administration of A. euchroma extract.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-12-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43984125","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
This study establishes a method for rapid detection of clonidine and cyproheptadine in foods of animal origin. In order to obtain the best detection method, capillary zone electrophoresis (CZE), large volume sample stacking (LVSS), and sweeping-micellar electrokinetic capillary chromatography (sweeping-MEKC) were used respectively. The limits of detection (LODs) of clonidine and cyproheptadine by LVSS-CZE were 0.028 μg mL−1 and 0.034 μg mL−1, and those by sweeping-MEKC were 0.023 μg mL−1 and 0.031 μg mL−1, respectively. Compared with the CZE method, the two online pre-concentration technologies have greatly improved the detection sensitivity and achieved good enrichment results. However, compared with the sweeping-MEKC system, the LVSS system consumed a longer time and was greatly affected by the actual sample matrix. The sweeping-MEKC method was proved to be suitable for real sample analysis. Under the best sweeping-MEKC conditions, clonidine and cyproheptadine could be well separated within 8 min and good linear relationships in the range of 0.1–1.0 μg mL−1 (r 2 > 0.99) were obtained. This method was successfully applied to the determination of clonidine and cyproheptadine in animal-derived foods with the recoveries of 82.3%–90.1% and the relative standard deviations (RSDs) less than 3.11%. The sweeping-MEKC method is simple to operate and has great potential in the rapid detection of clonidine and cyproheptadine in animal-derived foods.
建立了动物源性食品中可乐定和赛庚胺的快速检测方法。为获得最佳检测方法，分别采用毛细管区带电泳(CZE)、大体积样品堆积法(LVSS)和扫胶束电动毛细管色谱法(sweep - mekc)。LVSS-CZE法对可乐定和赛庚啶的检出限分别为0.028 μ mL - 1和0.034 μ mL - 1, sweep - mekc法对可乐定和赛庚啶的检出限分别为0.023 μ mL - 1和0.031 μ mL - 1。与CZE法相比，两种在线预富集技术均大大提高了检测灵敏度，富集效果良好。然而，与扫描- mekc系统相比，LVSS系统消耗的时间更长，并且受实际样品矩阵的影响较大。结果表明，扫描- mekc方法适用于实际样品的分析。在最佳扫描- mekc条件下，可乐定和赛庚啶可在8 min内分离，且在0.1 ~ 1.0 μg mL−1 (r 2 > 0.99)范围内具有良好的线性关系。该方法可用于动物性食品中可乐定和赛庚啶的含量测定，加样回收率为82.3% ~ 90.1%，相对标准偏差(rsd)小于3.11%。扫描- mekc方法操作简便，在动物源性食品中可乐定和赛庚胺的快速检测中具有较大的应用潜力。
{"title":"Comparison of clonidine and cyproheptadine determination in animal-derived foods by sweeping-micellar electrokinetic chromatography and large volume sample stacking-capillary zone electrophoresis","authors":"Zhihan Zheng, Li Xiaobin, Huitao Liu, Yuan Gao","doi":"10.1556/1326.2021.00970","DOIUrl":"https://doi.org/10.1556/1326.2021.00970","url":null,"abstract":"\u0000 This study establishes a method for rapid detection of clonidine and cyproheptadine in foods of animal origin. In order to obtain the best detection method, capillary zone electrophoresis (CZE), large volume sample stacking (LVSS), and sweeping-micellar electrokinetic capillary chromatography (sweeping-MEKC) were used respectively. The limits of detection (LODs) of clonidine and cyproheptadine by LVSS-CZE were 0.028 μg mL−1 and 0.034 μg mL−1, and those by sweeping-MEKC were 0.023 μg mL−1 and 0.031 μg mL−1, respectively. Compared with the CZE method, the two online pre-concentration technologies have greatly improved the detection sensitivity and achieved good enrichment results. However, compared with the sweeping-MEKC system, the LVSS system consumed a longer time and was greatly affected by the actual sample matrix. The sweeping-MEKC method was proved to be suitable for real sample analysis. Under the best sweeping-MEKC conditions, clonidine and cyproheptadine could be well separated within 8 min and good linear relationships in the range of 0.1–1.0 μg mL−1 (r\u0000 2 > 0.99) were obtained. This method was successfully applied to the determination of clonidine and cyproheptadine in animal-derived foods with the recoveries of 82.3%–90.1% and the relative standard deviations (RSDs) less than 3.11%. The sweeping-MEKC method is simple to operate and has great potential in the rapid detection of clonidine and cyproheptadine in animal-derived foods.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-11-29","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44568705","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.
{"title":"The RP-HPLC method development and validation for simultaneous determination of oryzalin and ethofumesate pesticides in soil and water","authors":"S. Tandon, S. Pal","doi":"10.1556/1326.2021.00953","DOIUrl":"https://doi.org/10.1556/1326.2021.00953","url":null,"abstract":"\u0000 A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-11-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44161265","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
N. El-Ragehy, Maha A. Hegazy, S. Tawfik, Ghada A. Sedik
Sulfacetamide sodium is a widely prescribed sulfonamide drug due to its topical antibacterial action on eye and skin. Four impurities are stated in the British Pharmacopoeia among which are sulfanilamide and dapsone. This work presents two specific, accurate and precise chromatographic methods for the simultaneous determination of a mixture of sulfacetamide sodium, sulfanilamide and dapsone. The first method is an isocratic RP-HPLC where the separation of components was achieved on C18 column. A green mobile phase was used consisting of methanol:water (60:40, v/v). The flow rate was 1.0 mL/min and effluent was monitored at 273 nm. The second method is a TLC-spectrodensitometric one where good separation was achieved by using silica plates and a mobile phase consisting of chloroform:dichloromethane:acetic acid (6:2.5:1.5, by volume). Determination was done by densitometry in the absorbance mode at 273 nm. Both methods were validated in compliance with ICH guidelines. They were also successfully applied for the determination of sulfacetamide sodium and its impurities in Ocusol® ophthalmic solutions. The obtained results were statistically compared to the results obtained by applying the official methods of analysis of each component where no significant difference was found with respect to accuracy and precision.
{"title":"Validated chromatographic methods for the simultaneous determination of a ternary mixture of sulfacetamide sodium and two of its official impurities; sulfanilamide and dapsone","authors":"N. El-Ragehy, Maha A. Hegazy, S. Tawfik, Ghada A. Sedik","doi":"10.1556/1326.2021.00921","DOIUrl":"https://doi.org/10.1556/1326.2021.00921","url":null,"abstract":"\u0000 Sulfacetamide sodium is a widely prescribed sulfonamide drug due to its topical antibacterial action on eye and skin. Four impurities are stated in the British Pharmacopoeia among which are sulfanilamide and dapsone. This work presents two specific, accurate and precise chromatographic methods for the simultaneous determination of a mixture of sulfacetamide sodium, sulfanilamide and dapsone. The first method is an isocratic RP-HPLC where the separation of components was achieved on C18 column. A green mobile phase was used consisting of methanol:water (60:40, v/v). The flow rate was 1.0 mL/min and effluent was monitored at 273 nm. The second method is a TLC-spectrodensitometric one where good separation was achieved by using silica plates and a mobile phase consisting of chloroform:dichloromethane:acetic acid (6:2.5:1.5, by volume). Determination was done by densitometry in the absorbance mode at 273 nm. Both methods were validated in compliance with ICH guidelines. They were also successfully applied for the determination of sulfacetamide sodium and its impurities in Ocusol® ophthalmic solutions. The obtained results were statistically compared to the results obtained by applying the official methods of analysis of each component where no significant difference was found with respect to accuracy and precision.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-11-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47269091","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
In this study, a UPLC-MS/MS method was developed to measure the concentrations of the flavonoids oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in the blank mouse blood, and the method was then used in the measurement of the pharmacokinetics of the compounds in mice. Oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin were administered intravenously at a dose of 5 mg kg−1, and the mouse blood (20 μL) was withdrawn from the caudal vein 0.08333, 0.25, 0.5, 1, 2, 4, 6, 8, and 10 h after administration. The mobile phase used for chromatographic separation by gradient elution was composed of acetonitrile and water (0.1% formic acid). The analytes were detected by operating in electrospray ionization (ESI) positive-ion mode using multiple reactions monitoring (MRM). The intra-day and inter-day accuracy ranged from 86.2 to 109.3%, the intra-day precision was less than 14%, and the inter-day precision was less than 15%. The matrix effect ranged from 85.3 to 111.3%, and the recovery of the analytes after protein precipitation were all above 78.2%. This method had the advantages of high sensitivity, accuracy, and recovery, and it had excellent selectivity, which enabled it to be applied to measuring the pharmacokinetics of the analytes in mice.
{"title":"Determination of oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in mouse blood by UPLC-MS/MS and its application to pharmacokinetics","authors":"Zheng Yu, Fan Chen, Yinan Jin, Minyue Zhou, Xianqin Wang, Xiuwei Shen","doi":"10.1556/1326.2021.00963","DOIUrl":"https://doi.org/10.1556/1326.2021.00963","url":null,"abstract":"\u0000 In this study, a UPLC-MS/MS method was developed to measure the concentrations of the flavonoids oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin in the blank mouse blood, and the method was then used in the measurement of the pharmacokinetics of the compounds in mice. Oroxin A, oroxin B, oroxylin A, oroxyloside, chrysin, chrysin 7-O-beta-gentiobioside, and guaijaverin were administered intravenously at a dose of 5 mg kg−1, and the mouse blood (20 μL) was withdrawn from the caudal vein 0.08333, 0.25, 0.5, 1, 2, 4, 6, 8, and 10 h after administration. The mobile phase used for chromatographic separation by gradient elution was composed of acetonitrile and water (0.1% formic acid). The analytes were detected by operating in electrospray ionization (ESI) positive-ion mode using multiple reactions monitoring (MRM). The intra-day and inter-day accuracy ranged from 86.2 to 109.3%, the intra-day precision was less than 14%, and the inter-day precision was less than 15%. The matrix effect ranged from 85.3 to 111.3%, and the recovery of the analytes after protein precipitation were all above 78.2%. This method had the advantages of high sensitivity, accuracy, and recovery, and it had excellent selectivity, which enabled it to be applied to measuring the pharmacokinetics of the analytes in mice.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":" ","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-11-09","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45149632","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Bingying Hu, Yingying Sun, Min Wang, Zhihui He, Shanshan Chen, D. Qi, Zhen Ge, L. Fan, Jingfang Chen, Yang Wei
A reliable LC-MS/MS method for the determination of five bioactive constituents (bilobalide, BLL; ginkgolide A, GLA; ginkgolide B, GLB; ginkgolide C, GLC; rutin) of Ginkgo biloba leaf extracts (GBE) in rat plasma was established, fully validated and applied to an intragastric pharmacokinetic study of a preparation of GBE in rat. Samples were extracted with ethyl acetate. C18 column was selected as analytical column in this method. Mobile phase was water with 0.01% formic acid and acetonitrile. Quantification was performed in negative multiple-reaction monitoring mode. Matrix instability of terpene lactones was noticed and hydrochloric acid was used as a stabilizer. This method showed good precision and accuracy, recovery was reproducible and matrix effect was negligible. Among four terpene lactones, BLL had the highest exposure and the shortest terminal half-life, GLA and GLB had lower exposure and longer terminal half-life, the exposure of GLC was lowest and its terminal half-life was the maximum, and all of them showed rapid absorption. This study provides a reference for determination of terpene lactones and flavonol glycoside prototypes in GBE and offers pharmacokinetic data of flavonol glycoside prototype in GBE.
{"title":"Simultaneous determination of ginkgolide A, B, C, bilobalide and rutin in rat plasma by LC-MS/MS and its application to a pharmacokinetic study","authors":"Bingying Hu, Yingying Sun, Min Wang, Zhihui He, Shanshan Chen, D. Qi, Zhen Ge, L. Fan, Jingfang Chen, Yang Wei","doi":"10.1556/1326.2021.00962","DOIUrl":"https://doi.org/10.1556/1326.2021.00962","url":null,"abstract":"\u0000 A reliable LC-MS/MS method for the determination of five bioactive constituents (bilobalide, BLL; ginkgolide A, GLA; ginkgolide B, GLB; ginkgolide C, GLC; rutin) of Ginkgo biloba leaf extracts (GBE) in rat plasma was established, fully validated and applied to an intragastric pharmacokinetic study of a preparation of GBE in rat. Samples were extracted with ethyl acetate. C18 column was selected as analytical column in this method. Mobile phase was water with 0.01% formic acid and acetonitrile. Quantification was performed in negative multiple-reaction monitoring mode. Matrix instability of terpene lactones was noticed and hydrochloric acid was used as a stabilizer. This method showed good precision and accuracy, recovery was reproducible and matrix effect was negligible. Among four terpene lactones, BLL had the highest exposure and the shortest terminal half-life, GLA and GLB had lower exposure and longer terminal half-life, the exposure of GLC was lowest and its terminal half-life was the maximum, and all of them showed rapid absorption. This study provides a reference for determination of terpene lactones and flavonol glycoside prototypes in GBE and offers pharmacokinetic data of flavonol glycoside prototype in GBE.","PeriodicalId":7130,"journal":{"name":"Acta Chromatographica","volume":"1 1","pages":""},"PeriodicalIF":1.9,"publicationDate":"2021-10-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"67652826","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":4,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
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