College of Pharmaceutical Sciences, Zhejiang University, 338 Yuhangtang Road, Hangzhou 310058, China.
J Pharm Biomed Anal. 2012 Jan 25;58:94-101. doi: 10.1016/j.jpba.2011.09.012. Epub 2011 Sep 22.
An ultra-high pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the quantification of three major ingredients in Chinese lantern preparations (CLP) in rat plasma. Following extraction by ethyl acetate, the analytes were separated on an Acquity UPLC BEH Shield RP C(18) column using a gradient mobile phase system of acetonitrile-water. Electrospray ionization (ESI) tandem interface was employed prior to mass spectrometric detection. The calibration curves were linear over the range of 5.0-500.0 ng/ml for physalin D, 2.3-230.0 ng/ml for physalin G and 0.71-71.0 ng/ml for 4,7-didehydroneophysalin B. The average extraction recoveries, examined at four concentration levels, carried from 57.1% to 76.9%, and the accuracies ranged from 94.0% to 113.3% with precision (RSD) <15%. The validated method was successfully applied to the determination of the three physalins in rat plasma after intragastric administration of CLP suspension.
建立了超高效液相色谱-串联质谱法(UPLC-MS/MS)测定大鼠血浆中三种中药灯笼制剂(CLP)主要成分的含量。采用乙酸乙酯提取后,在 Acquity UPLC BEH Shield RP C(18)柱上,以乙腈-水为梯度流动相系统进行分离。在质谱检测前采用电喷雾串联接口。在 5.0-500.0ng/ml 范围内, physalin D 的校准曲线呈线性,physalin G 的校准曲线在 2.3-230.0ng/ml 范围内,4,7-didehydroneophysalin B 的校准曲线在 0.71-71.0ng/ml 范围内。在四个浓度水平下测定的平均提取回收率为 57.1%-76.9%,准确度为 94.0%-113.3%,精密度(RSD)<15%。该方法已成功应用于大鼠胃内给予 CLP 混悬液后血浆中三种 physalins 的测定。