• 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>Journal of Chromatographic Science >Development and Validation of an LC-MS-MS Method for Determination of Simvastatin and Simvastatin Acid in Human Plasma: Application to a Pharmacokinetic Study
【24h】

Development and Validation of an LC-MS-MS Method for Determination of Simvastatin and Simvastatin Acid in Human Plasma: Application to a Pharmacokinetic Study

机译：LC-MS-MS法测定人血浆中的辛伐他汀和辛伐他汀酸的开发与验证：在药代动力学研究中的应用

获取原文
获取原文并翻译 | 示例
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

A liquid chromatography-tandem mass spectrometry method was developed and validated for the simultaneous determination of simvastatin (SV) and simvastatin acid (SVA) in human plasma. To improve assay sensitivity and achieve simultaneous analysis, SVA monitored in (-) ESI (electrospray ionization) mode within the first 4.5 min and SV thereafter in (+) ESI mode. The separation of all compounds was achieved in about 6.2 min using a C-18 reverse-phase fused-core (R) column (Ascentis (R) Express C-18) and a mobile phase, which was composed of 2.00 +/- 0.05 mMammonium acetate buffer titrated to pH 3.8 with glacial acetic acid-acetonitrile (25:75, v/v), in isocratic mode at a flow rate of 0.500 mL/min. Additionally, a solid-phase extraction step was performed to reduce any ion-suppression and/or enhancement effects. The developed method was linear in the concentration range of 0.100-74.626 ng/mL for SV, and 0.100-48.971 ng/mL for SVA, with correlation coefficient greater than 0.99 for both analytes. The method has shown tremendous reproducibility, with intra-and inter-day precision <7.6%, and intra-and interday accuracy within +/- 10.9% of nominal values, for the both analytes. The method was successfully applied to characterize the pharmacokinetic profiles of SV and SVA following an oral administration of 40 mg SV tablet to healthy human volunteers.
机译：建立了液相色谱-串联质谱法，并验证了该方法可同时测定人血浆中的辛伐他汀（SV）和辛伐他汀酸（SVA）。为了提高测定灵敏度并实现同时分析，在最初的4.5分钟内以（-）ESI（电喷雾电离）模式监测SVA，然后以（+）ESI模式监测SV。使用C-18反相熔核（R）色谱柱（Ascentis（R）Express C-18）和流动相（由2.00 +/- 0.05组成）在大约6.2分钟内完成了所有化合物的分离。 m冰醋酸缓冲液用冰醋酸-乙腈（25：75，v / v）在等度模式下以0.500 mL / min的流速滴定至pH 3.8。另外，进行固相萃取步骤以减少任何离子抑制和/或增强作用。所开发的方法在SV的浓度范围为0.100-74.626 ng / mL和对于SVA的浓度范围为0.100-48.971 ng / mL时呈线性，两种分析物的相关系数均大于0.99。该方法显示出极好的可重复性，两种分析物的日内和日间精度均<7.6％，日间和日间精度均在标称值的+/- 10.9％之内。在向健康人类志愿者口服40毫克SV片剂后，该方法已成功应用于表征SV和SVA的药代动力学。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号