摘要
建立HPLC-MS/MS方法定量测定人血浆中氢可酮浓度。以地西泮为内标,采用甲醇-0.05%甲酸水溶液为流动相进行梯度洗脱,以Agilent-C18(2.1×50 mm×3.5μm)色谱柱为分析柱,通过电喷雾离子源(ESI),以正离子多反应监测(MRM)方式进行检测。用于定量分析的离子对分别为m/z300.2→199.1(氢可酮)和m/z285.0→193.0(地西泮,内标)。氢可酮线性范围为0.5~50μg/L,定量下限为0.5μg/L(n=6),日内、日间精密度的RSD均小于15%,平均回收率大于75%。本方法专属性强、样品处理简便、灵敏度高,适用于氢可酮临床药动学研究。
HPLC-MS/MS method was established for the determination of hydrocodone in human plasma.Diazepam was used as internal standard,methanol-0.5% formic acid water was used as the mobile phase for gradient elution,Agilent-C18 column(2.1×50 mm×3.5 μm) was used as analytical column.Electrospray ionization(ESI) source was applied,and multiple reaction monitoring(MRM) mode was operated in the positive mode with the monitor ions at m/z 300.2→199.1 for hydrocodone and m/z 285.0→193.0 for the internal standard,respectively.The linear calibration curve is obtained over the concentration range of 0.5—50 μg/L.The limit of quantitation is 0.5 μg/L(n=6).The inter and intra-day precision(RSD) is less than 15%.The average recoveries are above 75%.The method is proved to be specific,convenient,sensitive and suitable for pharmacokinetics of hydrocodone.
出处
《质谱学报》
EI
CAS
CSCD
2011年第4期252-256,共5页
Journal of Chinese Mass Spectrometry Society