Li Guofei, Yang Fan, Liu Mei, Su Xianying, Zhao Mingming, Zhao Limei
Department of Pharmacy, Shengjing Hospital of China Medical University, Shenyang, China.
School of Pharmacy, Shenyang Pharmaceutical University, 103 Wenhua Road, Shenyang, 110016, China.
Biomed Chromatogr. 2016 Jul;30(7):1075-1082. doi: 10.1002/bmc.3652. Epub 2016 Jan 21.
With the purpose of carrying out pharmacokinetic interaction studies ofnberberine (BBR) and fenofibrate (FBT), an UPLC-MS/MS method has been developed and validated. The analytes, BBR and fenofibric acid (FBA, metabolite of FBT) and the internal standard, tetrahydropalmatine, were extracted with dichloromethane-diethyl ether (3:2, v/v) and separated on an Agilent Eclipse XDB C18 column using a mobile phase composed of acetonitrile and water. With positive ion electrospray ionization, the analytes were monitored on a triple quadrupole mass spectrometer in multiple reaction monitoring mode. Linear calibration curves were obtained over the concentration ranges of 0.1-100.0 ng/mL for BBR and 10.0-50,000.0 ng/mL for FBA. For BBR and FBA, the intra- and inter-day precisions were <11.5 and 11.9%, respectively. The accuracy was within 11.7% and 11.3%. The mean recoveries of BBR at three concentrations of 0.2, 20.0, 80.0 ng/mL were >85.6%, and those of FBA at three concentrations of 20.0, 2500.0, 40,000.0 ng/mL were >87.9%. Consequently, the proposed method was applied to the pharmacokinetic interaction study of FBT combined with BBR after oral administration in rats and was proved to be sensitive, specific and reliable to analyze BBR and FBA in biological samples simultaneously. Copyright © 2016 John Wiley & Sons, Ltd.
为了开展小檗碱(BBR)和非诺贝特(FBT)的药代动力学相互作用研究,已开发并验证了一种超高效液相色谱-串联质谱(UPLC-MS/MS)方法。分析物小檗碱、非诺贝特酸(FBA,FBT的代谢产物)以及内标四氢巴马汀,用二氯甲烷-乙醚(3:2,v/v)萃取,并在安捷伦Eclipse XDB C18柱上进行分离,流动相由乙腈和水组成。采用正离子电喷雾电离,在三重四极杆质谱仪上以多反应监测模式对分析物进行监测。在0.1 - 100.0 ng/mL浓度范围内获得了小檗碱的线性校准曲线,在10.0 - 50,000.0 ng/mL浓度范围内获得了非诺贝特酸的线性校准曲线。对于小檗碱和非诺贝特酸,日内和日间精密度分别<11.5%和11.9%。准确度在11.7%和11.3%以内。小檗碱在0.2、20.0、80.0 ng/mL三个浓度下的平均回收率>85.6%,非诺贝特酸在20.0、2500.0、40,000.0 ng/mL三个浓度下的平均回收率>87.9%。因此,所提出的方法应用于大鼠口服给药后FBT与BBR的药代动力学相互作用研究,被证明对同时分析生物样品中的BBR和FBA具有灵敏性、特异性和可靠性。版权所有© 2016约翰威立父子有限公司。