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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Development of two step liquid-liquid extraction tandem UHPLC-MS/MS method for the simultaneous determination of Ginkgo flavonoids, terpene lactones and nimodipine in rat plasma: Application to the pharmacokinetic study of the combination of Ginkgo biloba dispersible tablets and Nimodipine tablets
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Development of two step liquid-liquid extraction tandem UHPLC-MS/MS method for the simultaneous determination of Ginkgo flavonoids, terpene lactones and nimodipine in rat plasma: Application to the pharmacokinetic study of the combination of Ginkgo biloba dispersible tablets and Nimodipine tablets

机译：建立两步液-液萃取串联UHPLC-MS / MS方法同时测定大鼠血浆中的银杏黄酮，萜内酯和尼莫地平的方法：在银杏叶分散片和尼莫地平片组合的药代动力学研究中的应用

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摘要

A sensitive, reliable and accurate UHPLC-MS/MS method has been firstly established and validated for the simultaneous quantification of ginkgo flavonoids, terpene lactones and nimodipine in rat plasma after oral administration of Ginkgo biloba dispersible tablets, Nimodipine tablets and the combination of the both, respectively. The plasma samples were extracted by two step liquid-liquid extraction, nimodipine was extracted by hexane-ether (3:1, v/v) at the first step, after that ginkgo flavonoids and terpene lactones were extracted by ethyl acetate. Then the analytes were successfully separated by running gradient elution with the mobile phase consisting of 0.1% formic acid in water and methanol at a flow rate of 0.6 mL/min. The detection of the analytes was performed on a UHPLC-MS/MS system with turbo ion spray source in the negative ion and multiple reaction monitoring (MRM) mode. The calibration curves for the determination of all the analytes showed good linearity (R-2 > 0.99), and the lower limits of quantification were 0.50-4.00 ng/mL. Intra-day and inter-day precisions were in the range of 3.6%-9.2% and 3.2%-13.1% for all the analytes. The mean extraction recoveries of the analytes were within 69.82%-103.5% and the matrix were within 82.8%-110.0%. The validated method had been successfully applied to compare the pharmacokinetic parameters of ginkgo flavonoids, terpene lactones and nimodipine in rat plasma after oral administration of Ginkgo biloba dispersible tablets, Nimodipine tablets with the combination of the both. There were no statistically significant differences on the pharmacokinetic behaviors of all the analytes between the combined and single administration groups. Results showed that the combination of the two agents may avoid dosage adjustments in clinic and the combination is more convenient as well as efficient on different pathogenesis of cerebral ischemia. (C) 2016 Elsevier B.V. All rights reserved.
机译：首次建立了灵敏，可靠和准确的UHPLC-MS / MS方法，并已验证了口服银杏叶分散片，尼莫地平片和两者组合后可同时定量测定大鼠血浆中的银杏黄酮，萜内酯和尼莫地平， 分别。血浆样品采用两步液-液萃取，第一步用己烷-乙醚（3：1，v / v）萃取尼莫地平，然后用乙酸乙酯萃取银杏黄酮和萜烯内酯。然后，通过以流速为0.6 mL / min的流动相（由水和甲醇中的0.1％甲酸组成）进行梯度洗脱，成功分离出分析物。分析物的检测是在具有负离子和多反应监测（MRM）模式的涡轮离子喷雾源的UHPLC-MS / MS系统上进行的。用于测定所有分析物的校准曲线显示出良好的线性（R-2> 0.99），定量下限为0.50-4.00 ng / mL。所有分析物的日内和日间精度在3.6％-9.2％和3.2％-13.1％的范围内。分析物的平均提取回收率在69.82％-103.5％之内，基质在82.8％-110.0％之内。经验证的方法已成功地用于比较银杏黄酮分散剂，尼莫地平片与两者合用后大鼠血浆中银杏黄酮，萜烯内酯和尼莫地平的药代动力学参数。在联合和单次给药组之间，所有分析物的药代动力学行为在统计学上没有显着差异。结果表明，两种药物的联合使用可避免临床上的剂量调整，并且联合使用更方便，并且在不同的脑缺血发病机制中均有效。 （C）2016 Elsevier B.V.保留所有权利。

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