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超声辅助分散液液微萃取结合气相色谱-质谱法测定人全血中的七种娱乐性药物

Ultrasound-assisted dispersive liquid-liquid microextraction for the determination of seven recreational drugs in human whole blood using gas chromatography-mass spectrometry.

作者信息

Lin Zebin, Li Jiaolun, Zhang Xinyu, Qiu Meihong, Huang Zhibin, Rao Yulan

机构信息

Department of Forensic Medicine (Center of Forensic Science), School of Basic Medical Sciences, Fudan University, Shanghai 200032, China.

Department of Forensic Medicine (Center of Forensic Science), School of Basic Medical Sciences, Fudan University, Shanghai 200032, China; Department of Pharmaceutical Analysis, China Pharmaceutical University, 24 Tongjiaxiang, Nanjing 210009, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2017 Mar 1;1046:177-184. doi: 10.1016/j.jchromb.2017.01.024. Epub 2017 Jan 22.

Abstract

Recreational drugs have large impact on public health and security, and to monitor them is of urgent demand. In the present study, ultrasound-assisted dispersive liquid-liquid microextraction combined with the detection of gas chromatography-mass spectrometry was applied to the determination of seven common recreational drugs, including amphetamine, methamphetamine, 3,4-methylenedioxyamphetamine, 3,4-methylenedioxymethamphetamine, meperidine, methadone and ketamine in 200μL of human whole blood. A series of factors which would affect the extraction efficiency were systematically investigated, including the nature and the volume of extraction and dispersing solvents, ultrasonication time, salting-out effect and pH value. The method consumed small amount of sample. The limits of detection and limits of quantification for each analyte were 10 and 40ng/mL, respectively, and the linearity was in the range of 0.04-25μg/mL (R higher than 0.99). Good specificity, precision (1.5-8.2% for the intra-day study and 2.6-12.8% for the inter-day study), satisfactory accuracy (85.0-117.1%) and extraction recovery (77.0-92.4%) were obtained, which makes it a high performance method for the determination of recreational drugs in human whole blood samples.

摘要

消遣性药物对公众健康和安全有重大影响,因此对其进行监测迫在眉睫。在本研究中,超声辅助分散液液微萃取结合气相色谱-质谱检测法被应用于测定200μL人全血中的七种常见消遣性药物,包括苯丙胺、甲基苯丙胺、3,4-亚甲基二氧基苯丙胺、3,4-亚甲基二氧基甲基苯丙胺、哌替啶、美沙酮和氯胺酮。系统研究了一系列会影响萃取效率的因素,包括萃取溶剂和分散溶剂的性质及体积、超声时间、盐析效应和pH值。该方法样品用量少。各分析物的检测限和定量限分别为10和40ng/mL,线性范围为0.04-25μg/mL(R高于0.99)。该方法具有良好的特异性、精密度(日内研究为1.5-8.2%,日间研究为2.6-12.8%)、令人满意的准确度(85.0-117.1%)和萃取回收率(77.0-92.4%),使其成为测定人全血样品中消遣性药物的高效方法。

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