用液相色谱-离子阱质谱联用法检测兔体液中阿普唑仑及其主要代谢产物

Identification of Alprazolam and Its Major Metabolites in Body Fluids by Liquid Chromatography electrospray Ion Trap Mass Spectrometry

建立鉴别体液中阿普唑仑及其主要代谢物的高效液相色谱 电喷雾离子阱质谱联用(LC/MSn)法 .采用LC/MSn联用技术 ,检测家兔灌胃给药后血样和尿样中阿普唑仑原形药及其羟基化代谢物、葡萄糖苷酸型结合物 ,得到了它们的色谱、质谱以及特征碎片离子信息 .阿普唑仑的最低检测限小于 1ng .本法专属性强 ,可推广至其他生物检材的测定 。

A method was described for the characterization of alprazolam and its major metabolites by liquid chromatography electrospray ion trap mass spectrometry, involving α hydroxyalprazolam, 4 hydroxyalprazolam and their glucuronide conjugates. After a single 40 mg/kg dose to a rabbit, blood and urine samples were extracted and then injected into an ODS column with a mobile phase of 70% methanol and 30% water for LC/MS n analysis. The structures of alprazolam in blood and urine were identified by direct comparison of the observed mass spectra and the chromatographic retention time with those of the reference substance. Its metabolites were deduced by the characteristic ions in the selected-ion monitoring as well as full scan MS 2 mode. It was demonstrated that the method could be applied to the toxicological detection in forensic medicine due to its advantage of high specificity and sensitivity(the detection limit of alprazolam was below 1 ng ).