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目的建立同时测定人血浆中氯苯那敏和咖啡因含量的液相色谱-大气压化学电离-串联质谱(LC-APCI-MS-MS)法。方法血浆样品经乙酸乙酯提取后,采用Diamonsil C18柱分离,流动相为甲醇-水-甲酸(体积比80∶20∶0.5),采用大气压化学电离(APCI)源,以选择反应监测(SRM)方式进行检测,用于定量分析的离子反应分别为m/z275→m/z230(氯苯那敏)、m/z195→m/z138(咖啡因)、m/z256→m/z167(内标,苯海拉明)。结果血浆中氯苯那敏和咖啡因的线性范围分别为0.2~40.0μg.L-1和20.0~4 000μg.L-1;日内和日间精密度均小于13.4%,相对误差在±8.2%以内。结论该法适用于人血浆中氯苯那敏和咖啡因的同时测定。
Objective To establish a liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry (LC-APCI-MS-MS) method for simultaneous determination of chlorphenamine and caffeine in human plasma. Methods The plasma samples were extracted with ethyl acetate and separated on a Diamonsil C18 column. The mobile phase consisted of methanol - water - formic acid (80:20:0.5 by volume) and the source of atmospheric pressure chemical ionization (APCI) , And the ion reactions used for quantitative analysis were m / z 275 → m / z 230 (chlorpheniramine), m / z 195 → m / z 138 (caffeine), m / z 256 → m / z 167 Diphenhydramine). Results The linear ranges of chlorpheniramine and caffeine were 0.2-40.0μg.L-1 and 20.0-4000μg.L-1, respectively. The intra-and inter-day precision was less than 13.4% and the relative error was within ± 8.2% . Conclusion This method is suitable for simultaneous determination of chlorphenamine and caffeine in human plasma.