高效液相色谱-串联质谱法测定人血浆中伊托必利的浓度  

Determination of itopride concentration in human plasma by LC-MS/MS

作　　者：陈豪[1] 谭志荣[1] 郭栋[1] 陈尧[1] 杨智[1] 韩仰[1] 陈英[1] 张敏[1] 肖昌琼[1] 王亦男[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21期1869-1872,1876,共5页Chinese Journal of New Drugs

摘　　要：目的：建立HPLC-MS法测定人血浆中的伊托必利浓度。方法：以舒必利为内标,选用液液萃取法,然后进行LC-MS/MS分析。色谱柱为Phenomenex Luna C18柱（150 mm×2.0 mm,5μm）,流动相为乙腈-10 mmol.L-1甲酸胺水溶液（含0.1%甲酸）（60∶40）,流速为0.2 mL.min-1,柱温40℃,进样量为10μL,质谱采用ESI正离子方式进行扫描,MRM方式检测,用于定量分析的监测离子为m/z359.9→71.9（伊托必利）和m/z343.0→112.2（舒必利）。结果：本方法线性范围是0.336～688 ng.mL-1,r=0.999 3,最低定量限为0.336 ng.mL-1。绝对回收率均在80%以上,相对回收率在85%～115%之间,日内、日间RSD均〈5%。结论：本方法灵敏、快速和稳定,可用于伊托必利血药浓度检测和药动学研究。Objective：To develop a new sensitive LC-MS/MS method for the determination of itopride in human plasma.Methods：Sulpiride was selected as the internal standard,and the separation was performed on a Phenomenex Luna C18（150mm×2.0mm,5μm）column using acetonitrile-water（0.1% formic acid＋10mmol ammonium formate）（60∶40） at a flow rate of 0.2mL·min-1 as the mobile phase.The column temperature was 40℃.ESI＋ was performed in the MRM mode using target ions at m/z 359.9→71.9（itopride） and m/z 343.0→112.2（sulpiride）.Results：The calibration curve was linear within the range of 0.336～688ng·mL-1（r2=0.9993）.The lower limit of quantitation（LLOQ）of itopride in plasma was 0.336ng·mL-1.The extracted recovery of itopride from the plasma was more than 80%,the relative recovery was 85%～115%.The intra-and inter-day RSDs were all less than 5%.Conclusion：It can be used for the determination of itopride serum concentration and pharmacokinetic study as a sensitive,simple and accurate method.

关 键 词：高效液相色谱-串联质谱法 伊托必利 血药浓度 

分 类 号：R927.2[医药卫生—药学] R975.4