Chang Qing, Ma Hongying, Wang Fangjie, Ou Honglian, Zou Ming
Xiangya Hospital, Central South University, Changsha 410008, China.
Se Pu. 2011 Nov;29(11):1082-6.
A simple, precise and sensitive gas chromatography-mass spectrometry (GC-MS) method coupled with pulse splitless injection technique was developed for the determination of 10 sedative-hypnotics (barbital, amobarbital, phenobarbital, oxazepam, diazepam, nitrazepam, clonazepam, estazolam, alprazolam, triazolam) in human plasma. The drugs spiked in plasma were extracted with ethyl acetate after alkalization with 0.1 mol/L NaOH solution. The organic solvent was evaporated under nitrogen stream, and the residues were redissolved by ethyl acetate. The separation was performed on an HP-5MS column (30 m x 250 microm x 0.25 microm). The analytes were determined and identified using selected ion monitoring (SIM) mode and scan mode, respectively. The internal standard method was used for the determination. The target analytes were well separated from each other on their SIM chromatograms and also on the total ion current (TIC) chromatograms. The blank extract from human plasma gave no peaks that interfered with all the analytes on the chromatogram. The calibration curves for 10 sedative-hypnotics showed excellent linearity. The correlation coefficients of all the drugs were higher than 0.9954. The recoveries of the drugs spiked in human plasma ranged from 92.28% to 111.7%, and the relative standard deviations (RSDs) of intra-day and inter-day determinations were from 4.09% to 14.26%. The detection limits ranged from 2 to 20 microg/L. The method is simple, reliable, rapid and sensitive for the determination and the quantification of 10 sedative-hypnotics in human plasma and seems to be useful in the practice of clinical toxicological cases.
建立了一种简单、精确且灵敏的气相色谱 - 质谱联用（GC - MS）方法，并结合脉冲不分流进样技术，用于测定人血浆中的10种镇静催眠药（巴比妥、异戊巴比妥、苯巴比妥、奥沙西泮、地西泮、硝西泮、氯硝西泮、艾司唑仑、阿普唑仑、三唑仑）。血浆中添加的药物经0.1 mol/L氢氧化钠溶液碱化后，用乙酸乙酯萃取。有机溶剂在氮气流下蒸发，残留物用乙酸乙酯重新溶解。分离在HP - 5MS柱（30 m×250μm×0.25μm）上进行。分别采用选择离子监测（SIM）模式和扫描模式测定和鉴定分析物。采用内标法进行测定。目标分析物在其SIM色谱图和总离子流（TIC）色谱图上均能很好地相互分离。人血浆的空白提取物在色谱图上没有出现干扰所有分析物的峰。10种镇静催眠药的校准曲线显示出良好的线性。所有药物的相关系数均高于0.9954。人血浆中添加药物的回收率在92.28%至111.7%之间，日内和日间测定的相对标准偏差（RSD）为4.09%至14.26%。检测限为2至20μg/L。该方法对于测定和定量人血浆中的10种镇静催眠药简单、可靠、快速且灵敏，在临床毒理学病例实践中似乎很有用。
