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目的:建立beagle犬血浆中氧化苦参碱的LCMS测定法,测定其灌胃后在beagle犬体内的药动学。方法:采用LichrospherC18柱(250mm×4.6mm,5μm),柱温:25℃。流动相为10mmol·L-1醋酸铵水溶液甲醇(25∶75),流速:1mL·min-1;电喷雾离子化(ESI)方式,采用选择性离子检测法,检测离子为正离子,氧化苦参碱的离子为[m/z+H]+265.1,内标非那雄胺的离子是[m/z+H]+373.3。结果:氧化苦参碱在2～5000μg·L-1的范围内呈良好的线性关系(r=0.9990),最低检出限达0.6μg·L-1,日内和日间误差均小于4.2%,萃取回收率大于90%;氧化苦参碱的药时数据符合二室模型,Cmax为(2418.3±970.8)μg·L-1,tmax为(1.0±0.3)h,t1/2β为(5.5±1.6)h,AUC0→∝为(6117.4±1080.2)μg·L-1·h。结论:该法灵敏、简单,专属性强,可用于犬血浆中氧化苦参碱的测定。
OBJECTIVE: To establish a LCMS method for the determination of oxymatrine in beagle dogs and determine its pharmacokinetics in beagle dogs after intragastric administration. Methods: Lichrospher C18 column (250mm × 4.6mm, 5μm) was used. The column temperature was 25 ℃. The mobile phase consisted of 10mmol·L-1 ammonium acetate aqueous solution (25:75), the flow rate was 1mL · min-1 and the electrospray ionization (ESI) The reference alkali ion is [m / z + H] +265.1, and the ion of the internal standard finasteride is [m / z + H] +373.3. Results: Oxymatrine showed a good linearity (r = 0.9990) in the range of 2 ~ 5000μg · L-1 and a minimum detection limit of 0.6μg · L-1 with an error of less than 4.2% The extraction recovery rate was more than 90%. The data of oxymatrine was in accordance with two-compartment model with C max of (2418.3 ± 970.8) μg · L -1, tmax of (1.0 ± 0.3) h and t1 / 2β of (5.5 ± 1.6 ) h, AUC0 → α was (6117.4 ± 1080.2) μg · L-1 · h. Conclusion: The method is sensitive, simple and specific and can be used for the determination of oxymatrine in dog plasma.