HPLC-MS/MS法测定人血浆中乌苯美司浓度

目的建立高效液相色谱-串联质谱(HPLC-MS/MS)法测定人血浆中乌苯美司浓度。方法采用API3000型HPLC-MS/MS液质联用系统,Ultimate C18分析柱(50mm×4.6mm,5μm),流动相为甲醇-水-甲酸(70∶30∶0.05,V/V/V),流速为0.2mL/min,格拉司琼作为内标。样品经过固相萃取后浓缩进样,多反应离子检测模式,正离子扫描,离子源为ESI源。结果检测乌苯美司的线性范围为0.4～4000ng/mL,最低定量限为0.4ng/mL。批内精密度和批间精密度均小于6%。结论本法具有快速简便、灵敏准确的特点,可满足乌苯美司临床药物浓度测定的需要。

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

Objective To establish a liquid chromatography tandem mass spectrometry method for the determination of ubenimex in human plasma.Methods The essay was conducted with an API 3000 HPLC-MS/MS system consisted of a Ultimate C18 column(50 mm×4.6 mm,5 μm).The mobile phase consisted of methanol-water-formic acid(70∶30∶0.05,V/V/V) at a flow rate of 0.2 mL/min.Granisetron was used as the internal standard.The sample was extracted by solid phase extraction column and was operated under the multiple reaction monitoring mode using the electrospray ionization technique in positive mode.Results The linear range of ubenimex was 0.4-4000 ng/mL.The limit of quantity was set at 0.4 ng/mL.The within-day and between-day variations were less than 6%.Conclusion This method for the quantitative determination of ubenimex was proved to be accurate,sensitive,selective and convenient and can be applied in the determination of ubenimex in human plasma.