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目的:建立LC-MS/MS法测定大鼠血浆中丹参酮I、隐丹参酮及丹参酮IIA的浓度,并对大鼠口服丹参酮提取物后的3种丹参酮成分进行药代动学研究。方法 :血浆样品经甲醇沉淀蛋白后,以甲醇(含0.1%甲酸)-水(含0.1%甲酸)为流动相,梯度洗脱,采用Agilent Zorbax SB-C18(2.1 mm×150 mm,5μm)色谱柱分离,质谱以电喷雾离子源,选择反应监测(SRM)方式进行正离子检测。用于定量分析的离子反应分别为m/z 277.1→249.1(丹参酮I),m/z 297.1→251.2(隐丹参酮),m/z 295.1→277.1(丹参酮IIA)和m/z 360.9→233.0(内标,非诺贝特)。结果 :丹参酮I、隐丹参酮和丹参酮IIA的线性范围为2~100 ng.mL-1,日内、日间精密度(RSD)均小于12.0%,高、中、低3种浓度平均方法回收率均大于89.4%。结论 :本方法灵敏、简便,可用于丹参酮Ⅰ、隐丹参酮和丹参酮IIA的药代动力学研究。
OBJECTIVE: To establish a method for the determination of tanshinone I, cryptotanshinone and tanshinone IIA in rat plasma by LC-MS / MS and to study the pharmacokinetics of three tanshinones after oral administration of tanshinone in rats. METHODS: The plasma samples were precipitated with methanol and eluted with a mobile phase of methanol (containing 0.1% formic acid) -water (containing 0.1% formic acid) using an Agilent Zorbax SB-C18 (2.1 mm × 150 mm, 5 μm) Column separation, mass spectrometry electrospray ionization, selective reaction monitoring (SRM) positive ion detection mode. The ion reactions for quantitative analysis were m / z 277.1 → 249.1 (tanshinone I), m / z 297.1 → 251.2 (cryptotanshinone), m / z 295.1 → 277.1 (tanshinone IIA) and m / z 360.9 → 233.0 Standard, fenofibrate). Results: The linear range of tanshinone I, cryptotanshinone and tanshinone IIA was 2 ~ 100 ng.mL-1, the intra-day and inter-day precision was less than 12.0%, and the average recovery of high, medium and low concentration Greater than 89.4%. Conclusion: The method is sensitive and simple, and can be used to study the pharmacokinetics of tanshinone Ⅰ, cryptotanshinone and tanshinone IIA.