LC-MS-MS测定人血浆中贝前列素  

LC-MS-MS method determination of beraprost in human plasma

作　　者：陈秋华[1] 王亦男[2] 彭向东[1] 谭志荣[2] 

机构地区：[1]中南大学湘雅三医院药剂科,长沙410013 [2]中南大学临床药理研究所,长沙410078

出　　处：《中南药学》2008年第4期431-434,共4页Central South Pharmacy

摘　　要：目的建立液-质联用法测定人血浆中贝前列素的浓度。方法血浆样品用5mL乙醚-氯仿（3：1）提取，采用LC-MS-MS进行分析。色谱柱为Hypurity C18柱（2．10mm×150mm，5μm）；流动相为乙腈-0．02％甲酸水溶液-80：20；流速为0．20mL·min^-1；柱温为40℃，自动进样瓶温15℃。质谱采用ESI^-MRM方式进行监测；毛细管电压：3．0kV；源温度：100℃；去溶剂温度：250℃；锥孔气体流速：50L·h^-1；去溶剂气体流速：250L·h^-1。用于监测的离子为：m／z398→m／z269。结果线性回归方程为Y=0．41236X-6．1430，权重为1／x，决定系数（相关系数r的平方）为0．998，最小检出浓度为25．5pg·mL^-1绝对回收率均在70％以上，相对回收率在80％～120％，日内、日间RSD均％15％。结论本方法简便、灵敏、准确，可用于贝前列素血药浓度监测和药物动力学研究。Objective To establish an LC-MS-MS method for the determination of beraprost in human plasma. Methods Beraprost in plasma samples was extracted with 5 mL diethyl ether / chloroform （3 ： 1, v/v） . The analysis involved a Hypurity C18 （150 mm × 2.1 mm, 5 μm） column. The mobile phase consisted of acetonitrile., water （1 000 mL water added 2 mL formic acid） = （80 ： 20）, the flow rate was 0.2 mL ·min ^-1, and the column temperature was 40 ℃. Mass spectrum conditions： Caplillary voltage： 3.0 kV; Source Temp： 100 ℃ Desolvation temp： 250 ℃ Cone gas flow： 50 L·h^- 1 Desolvation flow; 250 L ·h ^-1. Monitor ion： m/z 398→ m/z 269. ESI^- was performed in the MRM mode using target ions at m/z 398→ m/z 269 （beraprost）. Results The peak area of beraprost in the plasma showed good linearity within 25.5 - 6 520 pg · mL^-1, r^2 = 0. 998. The limit lower outer quatrant （LLOQ） of beraprost in the plasma was 25.5 pg · mL^-1 , and the extracted recovery was 〉70%. The relative recovery was 80%-120%, while the intra- and inter-day RSD were 〈 15%. Conclusion The method is simple and sensitive with good recovery, and can be used in analyzing beraprost in biological samples.

关 键 词：液-质联用 贝前列素 血药浓度 

分 类 号：R917[医药卫生—药物分析学] R969.1[医药卫生—药学]