高效液相色谱－质谱联用测定人血浆中奥美拉唑的浓度

目的：建立高效液相色谱－质谱联用法测定人血浆中奥美拉唑的浓度。方法以泮托拉唑为内标，血浆样品经乙腈沉淀、取上清稀释后，进样，经HPLC－MS／MS分析。采用Ultimate XB－C18（2．1 mm ×150 mm，3μm），流动相甲醇（0．1％甲酸）∶水（0．1％甲酸）＝（70∶30，V／V）；流速：0．2mL? min －1，柱温：40℃，电喷雾离子源（ESI），以多离子反应监测方式（MRM）进行正离子监测，奥美拉唑和内标泮托拉唑的定量分析离子对分别为m／z 346．2→m／z 198．0和m／z 384．0→m／z 200．0。结果奥美拉唑的线性范围为5．00～2000．00μg? L－1，定量下限为5．00μg? L －1。方法回收率在96．4％～107．9％，日内和日间精密度（RSD）均小于15％。结论该方法操作简便、灵敏、准确、快速，适用于奥美拉唑的人体药代动力学研究。

Determination of Omeprazole in Human Plasma by HPLC-MS/MS

ABSTRACT:OBJECTIVE To establish a high performance liquid chromatography tandem mass spectrometry ( HPLC-MS/MS) method for the determination of Omeprazole in human plasma .METHODS Human plasma sam-ples were precipitated with acetonitrile and determined by HPLC-MS/MS using pantoprazole as the internal stand-ard.The separation was carried out on a Ultimate XB-C18(2.1mm ×150mm,3μm) with a mobile phase of methanol-water (including 0.1%formic acid) (70∶30) and the flow rate was 0.2mL? min-1.ESI was performed in the MRM positive mode with using target ions at m/z 346.2→m/z 198.0 ( Omeprazole ) and m/z 384.0→m/z 200.0 ( panto-prazole).RESULTS The calibration curve of Omeprazole was obtained in the range of 5.00~2000.00μg? L-1 with good linearity ( r>0.99 ) .The LLOQ of Omeprazole was 5μg? L-1 .The method recovery was between 96.4%and 107.9%,and the intra and inter day RSD were less than 15%.CONCLUSION This method is convenient , sensitive ,accurate and fast ,which is suitable for human pharmacokinetic studies of Omeprazole .