Huang Xiaochen, Su Shulan, Cui Wenxia, Liu Pei, Duan Jin-Ao, Guo Jianming, Li Zhenhao, Shang Erxin, Qian Dawei, Huang Zhijun
Jiangsu Key Laboratory for High Technology Research of TCM Formulae, Nanjing University of Chinese Medicine, Nanjing 210023, China; Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, Nanjing 210023, China; School of Chemical Engineering, Wuhan University of Technology, Wuhan 430070, China.
Jiangsu Key Laboratory for High Technology Research of TCM Formulae, Nanjing University of Chinese Medicine, Nanjing 210023, China; Jiangsu Collaborative Innovation Center of Chinese Medicinal Resources Industrialization, Nanjing University of Chinese Medicine, Nanjing 210023, China; School of Chemical Engineering, Wuhan University of Technology, Wuhan 430070, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jul 1;962:75-81. doi: 10.1016/j.jchromb.2014.05.032. Epub 2014 May 24.
In this present study, a sensitive and rapid UPLC-MS/MS method was developed for simultaneous quantification of paeoniflorin, albiflorin, ferulic acid, tetrahydropalmatine, protopine, typhaneoside and senkyunolide I in Beagle dog plasma after oral administration of the Shao-Fu-Zhu-Yu Decoction. Chloramphenicol and clarithromycin were used as internal standards. Plasma samples were processed by protein precipitation with methanol. The separation was performed on an Acquity BEH C18 column (100mm×2.1mm, 1.7μm) at a flow-rate of 0.4mL/min, using 0.1% formic acid-acetonitrile as mobile phase. Method validation was performed as per Food and Drug Administration guidelines and the results met the acceptance criteria. After validation, this method was successfully applied to a pharmacokinetic study. The results showed that the apparent plasma clearance of paeoniflorin, albiflorin, typhaneoside and senkyunolide I were significantly higher than others. Double peak was observed in plasma concentration curves of tetrahydropalmatine, the ferulic acid had a good absorption in Beagle dog plasma, and senkyunolide I was detected in plasma from the first blood sampling time (15min) and rapidly reached Tmax. The compound of typhaneoside has a low bioavailability according to the results.
在本研究中,建立了一种灵敏、快速的超高效液相色谱-串联质谱(UPLC-MS/MS)方法,用于同时定量比格犬口服少腹逐瘀汤后血浆中的芍药苷、白花芍药苷、阿魏酸、延胡索乙素、原阿片碱、知母皂苷元及藁本内酯。氯霉素和克拉霉素用作内标。血浆样品采用甲醇蛋白沉淀法处理。采用 Acquity BEH C18 柱(100mm×2.1mm,1.7μm),以 0.4mL/min 的流速进行分离,流动相为 0.1%甲酸-乙腈。按照美国食品药品监督管理局(FDA)指南进行方法验证,结果符合验收标准。验证后,该方法成功应用于药代动力学研究。结果表明,芍药苷、白花芍药苷、知母皂苷元及藁本内酯的表观血浆清除率显著高于其他成分。延胡索乙素的血浆浓度曲线出现双峰,阿魏酸在比格犬血浆中具有良好的吸收,藁本内酯在首次采血时间(15 分钟)的血浆中即可检测到,并迅速达到峰浓度(Tmax)。根据结果,知母皂苷元化合物的生物利用度较低。