Senda N, Kohta K, Takahashi T, Shizukuishi K, Mimura T, Fujita T, Nakayama M
Techno Research Laboratory, Hitachi Instruments Engineering, Co., Ltd., Ibaraki Prefecture, Japan.
Biomed Chromatogr. 1995 Jan-Feb;9(1):48-51. doi: 10.1002/bmc.1130090110.
We established a highly sensitive method to determine triazolam and its major metabolites, alpha-hydroxytriazolam and 4-hydroxytriazolam, in human plasma and urine with a liquid chromatography-mass spectrometry system which incorporates an atmospheric chemical ionization interface. A plasma sample and a urine sample after solvent extraction were injected into an ODS column of reversed phase with a mobile phase in a linear solvent gradient of initially 50 mM ammonium acetate (pH 4.0) 50%:methanol 50% and 15 min later methanol 100%; quantification limits of as low as 20 pg/mL at an SNR of 3 were obtained for each compound. With diazepam as an internal standard, recovery yields of 84, 81, and 77% were obtained for triazolam, alpha-hydroxytriazolam and 4-hydroxytriazolam, respectively.
我们建立了一种高灵敏度方法，使用配备大气化学电离接口的液相色谱-质谱系统来测定人血浆和尿液中的三唑仑及其主要代谢物α-羟基三唑仑和4-羟基三唑仑。将溶剂萃取后的血浆样品和尿液样品注入反相ODS柱，流动相采用线性溶剂梯度，初始为50 mM醋酸铵（pH 4.0）50%:甲醇50%，15分钟后为甲醇100%；每种化合物在信噪比为3时的定量限低至20 pg/mL。以地西泮为内标，三唑仑、α-羟基三唑仑和4-羟基三唑仑的回收率分别为84%、8l%和77%。
