色谱

色谱 ›› 2018, Vol. 36 ›› Issue (8): 803-808.DOI: 10.3724/SP.J.1123.2018.03021

• 研究论文 • 上一篇    下一篇

电场促进下的单滴微萃取-气相色谱法测定尿中6种苯丙胺类兴奋剂

宋爱英, 杨晶   

  1. 甘肃政法学院公安技术学院, 甘肃 兰州 730070
  • 收稿日期:2018-03-23 出版日期:2018-08-08 发布日期:2014-06-28
  • 通讯作者: 宋爱英,E-mail:say6982@gsli.edu.cn
  • 基金资助:

    国家自然科学基金（21565005）；甘肃省高等学校科学研究项目（2018A-069）；兰州市科技计划项目（2016-3-36）；甘肃政法学院校级重点项目（2017XZDLW02）.

Determination of six amphetamine-type stimulants in urine samples using electro-enhanced single drop microextraction-gas chromatography

SONG Aiying, YANG Jing   

  1. School of Public Security & Technology, Gansu Institute of Political Science and Law, Lanzhou 730070, China
  • Received:2018-03-23 Online:2018-08-08 Published:2014-06-28
  • Supported by:

    National Natural Science Foundation of China (No.21565005);Scientific Research Project of College and University in Gansu Province (No.2018A-069);Project of Science and Technology of Lanzhou City (No.2016-3-36);Key Project of Gansu Institute of Political Science and Law (No.2017XZDLW02).

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摘要：

建立了电场促进下的单滴微萃取结合气相色谱技术测定尿中6种苯丙胺类兴奋剂（ATSs）的分析方法。通过对影响萃取效率因素的优化，确定了最佳萃取条件：二氯甲烷萃取溶剂2 μL、萃取时间3 min、样品溶液pH 7和电压-2.5 V。采用HP-5毛细管色谱柱（30 m×0.32 mm×0.25 μm）进行分离，用氢火焰离子化检测器进行检测。6种ATSs在20~1000 μg/L范围内呈良好的线性关系，相关系数（r）为0.989~0.997，检出限（S/N=3）为3.2~7.6 μg/L；对尿样进行加标回收试验（50、100和500 μg/L），6种ATSs的回收率为91.6%~111.2%，相对标准偏差为2.9%~6.2%（n=3）。该法具有快速简便、灵敏度高、重复性好、线性范围宽、对环境友好的特点，可用于尿样中6种ATSs的分析测定。

关键词: 苯丙胺类兴奋剂, 单滴微萃取, 电场促进, 尿, 气相色谱

Abstract:

A method for the simultaneous determination of six amphetamine-type stimulants (ATSs) in urine by electro-enhanced single drop microextraction-gas chromatography (EE-SDME-GC) with a flame ionization detector (FID) was developed. The influences of the EE-SDME parameters on the extraction efficiencies were investigated. The 5 mL-samples at pH 7 were extracted with 2 μL dichloromethane for 3 min under an applied potential of -2.5 V. The analysis was performed on a HP-5 capillary column (30 m×0.32 mm×0.25 μm) using a flame ionization detector. The six ATSs were linear in the range of 20-1000 μg/L with correlation coefficients (r) between 0.989 and 0.997. The limits of detection (S⁄N=3) of the six ATSs ranged from 3.2 to 7.6 μg/L. The recoveries of the six ATSs in the spiked urine samples were 91.6%-111.2%, and the relative standard deviations were 2.9%-6.2% (n=3) at three spiked levels of 50, 100 and 500 μg/L. This method was rapid, sensitive, reliable, easily-operated and environment-friendly for the determination of the ATSs in urine samples.

Key words: amphetamine-type stimulants (ATSs), electro-enhancement (EE), gas chromatography (GC), single drop microextraction (SDME), urine

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