简单灵敏的LC-MS/MS方法检测人血浆中普伐他汀的浓度  

A simple and sensitive LC-MS/MS method for determination of pravastatin in human plasma

作　　者：谭志荣[1] 欧阳冬生[1] 周淦[1] 郭栋[1] 陈尧[1] 肖昌琼[1] 彭亮[1] 陈豪[1] 陈英[1] 张利[1] 韩仰[1] 周宏灏[1] 

机构地区：[1]中南大学临床药理研究所,长沙410078

出　　处：《中国新药杂志》2008年第13期1150-1153,共4页Chinese Journal of New Drugs

摘　　要：目的：建立液质联用法测定人血浆中普伐他汀的浓度。方法：空白血浆加普伐他汀和内标，用Bond Elut C18小柱进行固相提取，然后用LC-MS／MS进行分析。采用Thermo Hypurity C18柱（150mm×2．1mm，5μm），流动相为乙腈-0．2％甲酸水溶液（85：15），流速0．2mL·min^-1，柱温40℃，进样量为2μL。采用ESI正离子方式进行检测，用于定量分析的检测离子为m／z 447→327（普伐他汀钠）和m／z 482→272（瑞舒伐他汀）。结果：本方法线性范围是2．52～660μg·L^-1，r^2=0．994，最小检出浓度（LLOQ）为2．52μg·L^-1。绝对回收率均在70％以上，相对回收率在98％～102％之间，日内、日间RSD均〈15％。结论：本方法简便、灵敏、准确，可用于普伐他汀血药浓度检测和药动学研究。Objective：To establish a LC-MS/MS method for determination of pravastatin in human plasma. Methods：After addition of rosuvastatin （ internal standard）, pravastatin in plasma samples was extracted with SPE column. 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） （85：15 ）, the flow rate was 0.2 mL·min^-1, the column temperature was 40 ℃. ESI ＋ was performed in the MRM mode using target ions at m/z 447→327（pravastatin）and m/z 482→272（rosuvastatin）. Results：The peak area of pravastatin in plasma show good linearity within the range between 2.52 - 660 μg·L^-1,r^2 = 0. 994. The LLOQ of pravastatin in plasma was 2.52 μg·L^-1. The extracted recovery was 〉70% , and the relative recovery was 98% - 102%. The intra- and inter-day RSD were 〈 15%. Conclusion： The method is simple and sensitive with good recovery, and can be used in analyzing pravastatin in biological sample.

关 键 词：液质联用 普伐他汀 血药浓度 

分 类 号：R927.2[医药卫生—药学] R972.6