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机构地区:[1]天津中医药大学中医药研究院天津市现代中药重点实验室,天津300193 [2]天津中医药大学第一附属医院,天津300193
出 处:《辽宁中医药大学学报》2013年第6期32-34,共3页Journal of Liaoning University of Traditional Chinese Medicine
基 金:科技部国际科技合作项目(2009DFA31070)
摘 要: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O.1%甲酸)一水(含0.1%甲酸)为流动相,梯度洗脱,采用AgilentZorbaxSB-C18(2.11T11TI×150lrllrt,5斗m)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/z277.1→249.1(丹参酮I),m/z297.1→251.2(隐丹参酮),m/z295.1→277.1(丹参酮IIA)和m/z360.9→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2-100ng·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 develop a LC-MS/MS method for the determination of tanshinone I, cryptotanshinone and tanshinone IIA in rat plasma and to investigate the pharmacokinetics of the three tanshinones. Methods:The plasma samples were protein precipitated with methanol.After sample preparation, the samples were separated on an Agilent Zorbax SB-Cls ( 2.1 mm x 150 mm,5 p~ m ) column using methanol ( containing of 0.1% formic acid )and water ( containing of 0.1% formic acid )as mobile phase in gradient elution mode.The mass spectrometer was operated under the positive ion mode with the ESI source and the detection was performed by selected reaction monitoring ( SRM ) of the transition of m/z 277.1 →249.1 for tanshinone I, m/z 297.1→ 251.2 for cryptotanshinone, m/z 295.1→277.1 for tanshinone IIA and m/z 360.9→233.0 for fenofibrate. Results: The calibration curves for tanshinone I, cryptotanshinone and tanshinone IIA were all linear over the range of 2-100 ng · mL-1.The intra-day and inter-day precisions were within 12.0% and the average recovery was above 89.4%. Conclusion : The analysis method is sensitive, simple and suitable enough to be applied in the pharmacokinetic study of tanshinone I, cryptotanshinone and tanshinone IIA.
关 键 词:液相色谱-质谱联用法 丹参酮Ⅰ 隐丹参酮 丹参酮IIA 药动学
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