色谱

色谱 ›› 2008, Vol. 26 ›› Issue (3): 310-313.

• 研究论文 • 上一篇    下一篇

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

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   

  1. 1.General Surgery Department, the First Affiliated Hospital of Inner Mongolia Medical College,
    Hohhot 010050, China; 2.Laboratory of Anesthesia and Critical Care Medicine, West China Hospital,
    Sichuan University, Chengdu 610041, China
  • 收稿日期:2007-09-04 修回日期:2007-11-14 出版日期:2008-05-30 发布日期:1984-03-25
  • 通讯作者: 张瑞明

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

WANG Zhenxia1, ZHANG Ruiming1, CAO Wei2, OUYANG Xiaohui1, ZHAO Haiping1, DONG Peide1, MENG Xingkai1   

  1. 1.General Surgery Department, the First Affiliated Hospital of Inner Mongolia Medical College,
    Hohhot 010050, China; 2.Laboratory of Anesthesia and Critical Care Medicine, West China Hospital,
    Sichuan University, Chengdu 610041, China
  • Received:2007-09-04 Revised:2007-11-14 Online:2008-05-30 Published:1984-03-25
  • Contact: ZHANG Ruiming

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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(15 m×0.25 mm×0.1 μm),初始柱温100 ℃,保持1 min后以40 ℃/min速率升温至200 ℃，保持0.5 min；进样口温度250 ℃；分流进样,分流比1∶1,进样量2 μL；载气为氦气，流量为1.0 mL/min。质谱条件为:离子源温度230 ℃,电子轰击电离,电子能量70 eV,选择离子检测（m/z 58(MEGX)、 m/z 86(普鲁卡因，内标)）。结果表明,MEGX在血清中的浓度在1.562～25 ng/mL范围内的线性关系良好,相关系数0.9981,最低检测限为0.5 ng/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。

关键词: 代谢物；血清, 单乙基甘氨酰二甲苯胺, 利多卡因, 气相色谱-质谱联用法；固相萃取

Abstract: 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=0.9981). 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.

Key words: gas chromatography-mass spectrometry (GC-MS), lidocaine, metabolin, monoethylglycinexylidide, serum, solid phase extraction (SPE)