色谱

色谱

• 研究论文 • 上一篇    下一篇

脉冲不分流进样气相色谱-质谱法分析血浆中的10种镇静催眠药

常青1, 马虹英1*, 王方杰1,2, 欧红莲3, 邹明1,2   

  1. 1. 中南大学湘雅医院, 湖南 长沙 410008; 2. 中南大学药学院, 湖南 长沙 410078; 3. 桂林医学院, 广西 桂林 541004
  • 收稿日期:2011-06-13 修回日期:2011-08-01 出版日期:2011-11-28 发布日期:2011-12-25
  • 通讯作者: 马虹英,副主任药师,硕士生导师,主要研究方向为临床药学和体内药物分析. Tel: (0731)84327460,

Determination of 10 sedative-hypnotics in human plasma using pulse splitless injection technique and gas chromatography-mass spectrometry

CHANG Qing1, MA Hongying1*, WANG Fangjie1,2, OU Honglian3, ZOU Ming1,2   

  1. 1. Xiangya Hospital, Central South University, Changsha 410008, China; 2. School of Pharmaceutical Sciences, Central South University, Changsha 410078, China; 3. Guilin Medical College, Guilin 541004, China
  • Received:2011-06-13 Revised:2011-08-01 Online:2011-11-28 Published:2011-12-25

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摘要： 采用脉冲不分流进样技术建立了血浆中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)的气相色谱-质谱(GC-MS)快速定性定量分析方法。血浆样品经0.1 mol/L氢氧化钠溶液碱化后,用乙酸乙酯萃取;萃取液经氮气吹干,用乙酸乙酯溶解后进行GC-MS分析,所用的色谱柱为HP-5MS毛细管柱(30 m×250 μm×0.25 μm),采用全扫描(SCAN)模式定性,选择离子监测(SIM)模式下采用内标法定量。所测样品色谱分离良好,线性关系良好,10种药物的回收率均在92.28%～111.7%之间,日内、日间精密度在4.09%～14.26%范围内,样品检出限为2～20 μg/L。该方法简便、快速、准确可靠,可作为血浆中镇静催眠类药物的快速筛查及定量的方法。

关键词: 脉冲不分流进样, 气相色谱-质谱法, 血浆, 镇静催眠药

Abstract: 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×250 μm×0.25 μm). 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 μg/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.

Key words: plasma, plasma qualitative and quantitative analysis, pulse splitless, pulse splitless injection, sedative-hypnotics, gas chromatography-mass spectrometry (GC-MS)