Deng Yating, Liao Qiongfeng, Li Suhua, Bi Kaishun, Pan Biyan, Xie Zhiyong
Laboratory of Pharmaceutical Analysis & Quality Assessment, School of Pharmaceutical Sciences, Sun Yat-sen University, 74 Zhongshan Road II, Guangzhou 510080, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Mar 1;863(2):195-205. doi: 10.1016/j.jchromb.2007.12.028. Epub 2008 Jan 21.
A rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed to simultaneously determine berberine, palmatine and jatrorrhizine in rat plasma. After mixing with the internal standard (IS) tetrahydropalmatine, plasma samples were pretreated by protein precipitation with acetonitrile-methanol (1:2, v/v). Chromatographic separation was carried out on a C18 column using a mixture of water (containing 0.1% formic acid) and acetonitrile (30:70, v/v) as mobile phase. The detection was performed by selected reaction monitoring (SRM) mode via electrospray ionization (ESI) source operating in the positive ionization mode. The method was linear over the concentration range of 1.0-250.0 ng/mL for all components. The intra- and inter-day precision values were less than 14.6% and the deviations were within +/-4.0%. The fully validated LC-MS/MS method has been successfully applied to the pharmacokinetic study of berberine, palmatine and jatrorrhizine in rat plasma after oral administration of coptis-evodia herb couple. Three peaks were observed in both individual and mean plasma-concentration curves of berberine, palmatine and jatrorrhizine, which may be attributed to distribution re-absorption and enterohepatic circulation.
建立了一种快速灵敏的液相色谱-串联质谱（LC-MS/MS）法，用于同时测定大鼠血浆中的小檗碱、巴马汀和药根碱。血浆样品与内标（IS）四氢巴马汀混合后，用乙腈-甲醇（1:2，v/v）进行蛋白沉淀预处理。采用C18柱，以水（含0.1%甲酸）和乙腈（30:70，v/v）的混合物为流动相进行色谱分离。通过电喷雾电离（ESI）源在正离子模式下运行的选择反应监测（SRM）模式进行检测。该方法对所有组分在1.0-250.0 ng/mL浓度范围内呈线性。日内和日间精密度值均小于14.6%，偏差在±4.0%以内。经过充分验证的LC-MS/MS方法已成功应用于黄连-吴茱萸药对口服给药后大鼠血浆中小檗碱、巴马汀和药根碱的药代动力学研究。在小檗碱、巴马汀和药根碱的个体和平均血浆浓度曲线中均观察到三个峰，这可能归因于分布再吸收和肠肝循环。
