液相色谱-质谱联用法检测体液中三唑仑及其代谢产物Identification of triazolam and its metabolites in body fluids by liquid chromatography mass spectrometry
李雪庆,钟大放,宋明,阎立志
LI Xue qing 1; ZHONG Da fang 1; SONG Ming 2; YAN Li zhi 2 (1.Laboratory of Drug Metabolism and Pharmacokinetics;
摘要(Abstract):
建立了鉴别体液中三唑仑及其主要代谢物的液相色谱 质谱联用法。采用液相色谱 电喷雾离子阱质谱法 ,得到三唑仑和羟基化代谢物及其葡萄糖苷酸型结合物的色谱、质谱信息以及特征碎片离子。三唑仑的最低检测限小于 0 1ng。用本法分析了一例怀疑服用过量三唑仑的麻醉抢劫案例所取证的血样及尿样 ,并与健康受试者服药后尿样及家兔灌胃三唑仑后所取的血样及尿样比较 ,得到了当事人服用三唑仑的可靠数据。该方法可靠、快速、简便 ,尤其适用于需快速响应的法医学和毒理学分析
A highly sensitive method was described for the detection of triazolam and its major metabolites, α hydroxytriazolam and 4 hydroxytriazolam, in the plasma and urine with liquid chromatography mass spectrometry system which incorporated an electrospray ionization interface. After oral administration of a single 0 25 mg dose of triazolam to a healthy volunteer as well as a single 40 mg/kg dose to a rabbit,the plasma and urine samples were extracted and then injected into an ODS column with a mobile phase of 80% methanol and 20% water for LC/MS analysis. The structures of triazolam and its metabolites were identified either by direct comparison of the observed mass spectra and the chromatographic retention time with reference spectra or by the characteristic ions in the selected ion monitoring as well as full scan MS 2 (or MS 3) mode. The detection limit was below 0 1 ng of triazolam. By this method, we demonstrated the presence of triazolam in the unknown plasma and urine samples from a human being. It is proved that this method is especially suitable for the detection in body fluids of forensical and clinical toxicological relevant triazolam.
关键词(KeyWords):
三唑仑;代谢物;血浆;尿样;液相色谱质谱联用法
triazolam; metabolites; plasma; urine; LC/x
基金项目(Foundation): 国家自然科学基金资助项目!(39930 180 )
作者(Authors):
李雪庆,钟大放,宋明,阎立志
LI Xue qing 1; ZHONG Da fang 1; SONG Ming 2; YAN Li zhi 2 (1.Laboratory of Drug Metabolism and Pharmacokinetics;
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