...
  • 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >Development of a sensitive LC-MS/MS method for the determination of bilobalide in rat plasma with special consideration of ex vivo bilobalide stability: Application to a preclinical pharmacokinetic study
【24h】

Development of a sensitive LC-MS/MS method for the determination of bilobalide in rat plasma with special consideration of ex vivo bilobalide stability: Application to a preclinical pharmacokinetic study

机译：灵敏的LC-MS / MS方法用于测定大鼠血浆中的白果内酯，并特别考虑离体白果内酯的稳定性：在临床前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

The ex vivo instability of bilobalide containing three 7-lactone rings has been paid less attention by researchers who developed bioanalytical methods for bilobalide. In the present study, a sensitive LC-MS/MS method for the determination of bilobalide in rat plasma was developed with special consideration of ex vivo bilobalide stability. Several important factors affecting the stability of bilobalide in sampling and handling procedures were investigated. To prevent the ex vivo degradation of bilobalide, EDTA instead of heparin was used as an anticoagulant as well as an esterase inhibitor for blood collection and the separation of plasma was performed at 4degC. 20muL of plasma sample was acidified with 0.1 M hydrochloric acid, and then extracted with ethyl ether-methylene chloride (2:1, v/v). The extract was chromatographed on a Thermo Hypersil GOLD (100 mm x 2.1 mm, 5 mum) column using acetonitrile-10mM ammonium acetate-formic acid (90:10:0.4, v/v/v) as the mobile phase. The analyte and the internal standard (ginkgolide B) were detected by selected reaction monitoring mode via negative electrospray ionization. The method was fully validated and proved to be linear over a concentration range of 5.0-5000 ng/mL The intra- and inter-day precisions were less than 5.2% and the accuracy was within 92.5-101%. The extraction recoveries ranged from 80.7% to 86.7%. The proposed method was successfully applied to a preclinical pharmacokinetic study of bilobalide in rats after intragastric administration of a single dose of bilobalide at 7,14 and 28 mg/kg.
机译：开发出用于胆囊炎的生物分析方法的研究人员很少关注含有三个7-内酯环的胆囊炎的离体不稳定性。在本研究中，开发了一种灵敏的LC-MS / MS方法测定大鼠血浆中的白叶内酯，并特别考虑了离体白叶内酯的稳定性。研究了影响白果内酯稳定性的几个重要因素。为了防止白去内酯的离体降解，使用EDTA代替肝素作为抗凝剂以及酯酶抑制剂用于血液收集，并在4℃下进行血浆分离。用0.1M盐酸酸化20μl血浆样品，然后用乙醚-二氯甲烷（2∶1，v / v）萃取。萃取物在Thermo Hypersil GOLD（100 mm x 2.1 mm，5 mum）色谱柱上进行色谱分离，使用乙腈-10mM乙酸铵-甲酸（90：10：0.4，v / v / v）作为流动相。通过负电喷雾电离以选定的反应监测模式检测分析物和内标（银杏内酯B）。该方法得到了充分验证，并在5.0-5000 ng / mL的浓度范围内是线性的。日内和日间精度低于5.2％，精度在92.5-101％之内。提取回收率在80.7％至86.7％之间。所建议的方法已成功地应用于大鼠胃内给药7,14和28 mg / kg的单剂量比洛巴利特后大鼠中比洛巴利特的临床前药代动力学研究。

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