目的:建立用于测定对萼猕猴桃苷E血药浓度的液相色谱-串联质谱分析方法,并探讨对萼猕猴桃苷E在大鼠体内的药代动力学。方法:血浆样品经乙酸乙酯萃取后,用LC-MS/MS进行测定分析。内标为对萼猕猴桃苷F,色谱柱为ZorbaxSB-C18(100mm×2.1mm,3.5μm),流动相为甲醇-0.1%甲酸溶液(50:50,V/V),流速0.3mLmin1。结果:对萼猕猴桃苷E浓度在0.52500ngmL1之间线性关系良好,提取回收率在83.2%85.5%之间,日内和日间精密度RSD分别在1.7%7.5%和2.0%8.9%之间,准确度在95.7%108.6%之间,大鼠口服100mgkg1和静注5mgkg1对萼猕猴桃苷E后,该药绝对生物利用度约0.27%。结论:建立的LC-MS/MS联用方法简单准确,灵敏度高,适用于大鼠血浆中对萼猕猴桃苷E的药代动力学研究。
A highly sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for the determination of actinoside E in rat plasma. The analytes were extracted by ethyl acetate and an analogue of actinoside F was used as the internal standard. The mobile phase consisted of methanol-water (50 : 50, V/V) containing 0.1% formic acid was delivered at a flow rate of 0.3 mL.min^-1 to a Zorbax SB-CI8 column (100 mm × 2.1 mm, 3.5μm). The detection was performed by electrospray ionization mass spectrometry in the negative multiple reaction monitoring mode with a chromatograph run time of 3.0 min. Calibration curves of actinoside E were linear in the range of 0.5-2 500 ng'mL-1. In this range, intra- and inter-day precision ranged from 1.7% to 7.5% and 2.0% to 8.9%, respectively. The accuracy ranged from 95.7% to 108.6%, and extraction recovery from 83.2% to 85.5%. This method was successfully applied to a pharmacokinetic study of actinoside E in rats after intravenous (5 mg'kg-1) and oral (100 mg.kg^-1) administration, and the results showed that actinoside E was poorly absorbed with an absolute bioavailability being approximately 0.27%.