色谱

色谱 ›› 2015, Vol. 33 ›› Issue (3): 304-308.DOI: 10.3724/SP.J.1123.2014.12001

• 研究论文 • 上一篇    下一篇

超声辅助低密度溶剂分散液液微萃取-气相色谱-三重四极杆质谱法检测生物样品中的8种毒品

孟梁1, 朱彬玲1, 郑可芳1, 张文文2, 孟品佳3   

  1. 1. 福建警察学院刑事科学技术系, 福建 福州 350007;
    2. 北京市公安局公安交通管理局, 北京 100037;
    3. 中国人民公安大学刑事科学技术学院, 北京 100038
  • 收稿日期:2014-12-01 修回日期:2015-01-04 出版日期:2015-03-08 发布日期:2015-02-12
  • 通讯作者: 孟梁
  • 基金资助:

    福建省教育厅中青年教师教育科研项目(JA14336).

Ultrasound-assisted low-density solvent dispersive liquid- liquid microextraction for the determination of eight drugs in biological samples by gas chromatography- triple quadrupole mass spectrometry

MENG Liang1, ZHU Binling1, ZHENG Kefang1, ZHANG Wenwen2, MENG Pinjia3   

  1. 1. Department of Forensic Science, Fujian Police College, Fuzhou 350007, China;
    2. Traffic Management Bureau, Beijing Municipal Public Security Bureau, Beijing 100037, China;
    3. College of Forensic Science, People's Public Security University of China, Beijing 100038, China
  • Received:2014-12-01 Revised:2015-01-04 Online:2015-03-08 Published:2015-02-12

PDF

262

被引次数

7

摘要：

建立了生物样品中8种毒品的超声辅助分散液液微萃取-气相色谱-三重四极杆串联质谱检测方法,采用密度比水低的有机溶剂甲苯作为萃取溶剂,萃取过程中不需要任何分散剂。对影响萃取富集效率的因素进行优化:将100 μL甲苯萃取剂加入到1 mL样品溶液中,超声波剧烈振荡使甲苯充分分散到样品溶液中进行萃取,离心分层后,抽取上层萃取剂供气相色谱-三重四极杆串联质谱分析检测。在优化条件下,分析物在各自的线性范围内具有良好的线性关系,线性相关系数在0.9984~0.9994之间;检出限为0.05~0.40 μg/L (S/N=3);样品加标回收率在79.3%~100.3%之间,RSD<5.7%。本方法具有操作简单、灵敏度高和重现性好等优点,可应用于生物样品中多种毒品的分析检测。

关键词: 超声, 毒品, 分散液液微萃取, 气相色谱-三重四极杆质谱, 生物样品

Abstract:

A novel microextraction technique based on ultrasound-assisted low-density solvent dispersive liquid-liquid microextraction (UA-LDS-DLLME) has been developed for the determination of multiple drugs of abuse in biological samples by gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS). A total of 100 μL of toluene as extraction solvent was dropped into the sample solution. Then the mixture was sonicated drastically in an ultrasonic bath for 3 min with occasional manual shaking to form a cloudy suspension. After centrifugation at 10000 r/min for 3 min, the upper layer of low-density extractant was withdrawn and injected into the GC-QQQ-MS for analysis. The parameters affecting extraction efficiency have been investigated and optimized. Under the optimum conditions, good linearities were observed for all analytes with the correlation coefficients ranging from 0.9984 to 0.9994. The recoveries of 79.3%-100.3% with RSDs<5.7% were obtained. The LODs (S/N=3) were in the range from 0.05 to 0.40 μg/L. UA-LDS-DLLME technique has the advantages of less extraction time, suitable for batches of sample pretreatment simultaneously, and higher extraction efficiency. It was successfully applied to the analysis of amphetamines in real human urine samples.

Key words: biological samples, dispersive liquid-liquid microextraction (DLLME), drugs of abuse, gas chromatography-triple quadrupole mass spectrometry (GC-QQQ-MS), ultrasonication

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