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目的建立一种快速、灵敏的液相色谱-串联质谱法(LC-MS/MS)测定微量人血浆中伏立康唑。方法氟康唑为内标(IS),25μL血浆样品经乙醚-二氯甲烷(3∶2,V∶V)萃取,在ZorbaxSB-C18色谱柱(150mm×4.6mmI.D.,5μm,USA)上分离,以乙腈-水-甲酸(80∶20∶0.15,V∶V∶V)为流动相。采用电喷雾电离源(ESI源),在正离子检测方式下,以选择反应监测模式进行定量分析,监测的离子反应分别为m/z350→m/z(127+281)(伏立康唑)和m/z307→m/z(220+238)(氟康唑)。结果本法伏立康唑的线性范围为5.00～5000μg·L-1,定量下限为5.00μg·L-1,提取回收率大于90%(RSD小于6.2%),日内、日间RSD均小于6.6%,RE在(-1.1～1.8)%之间,每一个样品色谱分析时间小于4.5min。结论本方法操作简便、快速、灵敏,成功应用于伏立康唑的药动学研究。
Objective To establish a rapid and sensitive liquid chromatography-tandem mass spectrometry (LC-MS / MS) for the determination of voriconazole in human plasma. Methods Fluconazole was used as internal standard (IS). 25μL plasma samples were extracted with diethyl ether-dichloromethane (3: 2, V:V) and analyzed on a Zorbax SB-C18 column (150mm × 4.6mmI.D., 5μm, USA) With acetonitrile-water-formic acid (80: 20: 0.15, V: V: V) as the mobile phase. The electrospray ionization source (ESI source) was used in the positive ion detection mode to conduct the quantitative analysis by selective reaction monitoring mode. The ion reactions monitored were m / z 350 → m / z 127 + 281 (voriconazole) and m / z307 → m / z (220 + 238) (fluconazole). Results The results showed that the linear range of voriconazole in this method was 5.00-5000μg · L-1, the lower limit of quantification was 5.00μg · L-1, the recovery was more than 90% (RSD less than 6.2%). The intra- and inter-day RSD were less than 6.6% Between (-1.1 and 1.8)%, the chromatographic time for each sample was less than 4.5 min. Conclusion The method is simple, rapid, sensitive and successfully applied to voriconazole pharmacokinetic studies.