固相萃取-气相色谱-质谱法测定利多卡因代谢物单乙基甘氨酰二甲苯胺的血药浓度  

Determination of monoethylglycinexylidide concentration in serum using solid phase extraction and capillary gas chromatography-mass spectrometry

作　　者：王震侠[1] 张瑞明[1] 曹伟[2] 欧阳晓晖[1] 赵海平[1] 董培德[1] 孟兴凯[1] 

机构地区：[1]内蒙古医学院第一附属医院普外科,内蒙古呼和浩特010050 [2]四川大学华西医院麻醉与危重病研究室,四川成都610041

出　　处：《色谱》2008年第3期310-313,共4页Chinese Journal of Chromatography

基　　金：国家自然科学基金资助项目(No30460131)

摘　　要：建立了固相萃取-气相色谱-质谱（GC-MS）测定利多卡因代谢物单乙基甘氨酰二甲苯胺（MEGX）血药浓度的方法。血清中的MEGX采用固相萃取小柱萃取、GC-MS测定。色谱条件为：HP-5MS毛细管柱（15m×0.25mm×0.1μm）,初始柱温100℃,保持1min后以40℃/min速率升温至200℃,保持0.5min;进样口温度250℃;分流进样,分流比1∶1,进样量2μL;载气为氦气,流量为1.0mL/min。质谱条件为：离子源温度230℃,电子轰击电离,电子能量70eV,选择离子检测（m/z58（MEGX）、m/z86（普鲁卡因,内标））。结果表明,MEGX在血清中的浓度在1.562～25ng/mL范围内的线性关系良好,相关系数0.9981,最低检测限为0.5ng/mL,不同浓度MEGX的萃取回收率在80.1%～85.7%之间。实验证明该方法快速、准确,选择性好,灵敏度高,适合用于血清中微量MEGX的测定。A novel method for the determination of monoethylglycinexylidide （MEGX） （lidocaine metabolin） in serum using solid phase extraction （SPE） and capillary gas chromatography-mass spectrometry （GC-MS） was established. The serum sample was extracted with a CN-SPE column. An HP-5MS capillary column （15 m×0.25 mm×0.1 μm） was used. The initial temperature of the column was set at 100 ℃, held for 1 min, then raised to 200 ℃ at 40 ℃/min, and held at 200 ℃ for 0.5 min. The sample size was 2 μL, and the split ratio was set at 1∶1. The carrier gas was high purity helium with a flow rate of 1.0 mL/min. The monitoring ions for the determination were m/z 58 for MEGX and m/z 86 for procaine （internal standard）. The calibration curve of MEGX had good linear relationship in the range of 1.562-25 ng/mL （r=0.998 1）. The limit of detection was 0.5 ng/mL. The extraction recovery ranged from 80.1% to 85.7%. The method advanced the quantitative analysis of MEGX in serum by combining rapid and efficient SPE with specific and sensitive quantitation by GC-MS.

关 键 词：气相色谱-质谱联用法 固相萃取 单乙基甘氨酰二甲苯胺 利多卡因 代谢物 血清 

分 类 号：O658[理学—分析化学]