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分散液液微萃取和 GC-MS/MS 在饮料和头发中测定 GHB 的应用。

Application of dispersive liquid-liquid microextraction and GC-MS/MS for the determination of GHB in beverages and hair.

机构信息

Department of Forensic Science, Fujian Police College, Fuzhou 350007, PR China; Engineering Research Center, Fujian Police College, Fuzhou 350007, PR China.

Department of Forensic Science, Fujian Police College, Fuzhou 350007, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2020 May 1;1144:122058. doi: 10.1016/j.jchromb.2020.122058. Epub 2020 Mar 11.

DOI:10.1016/j.jchromb.2020.122058
PMID:32224437
Abstract

Recently, gamma-hydroxybutyrate (GHB) was determined in "Kawa Trendy Drink" which was labeled as a functional beverage containing gamma-aminobutyric acid and quickly became popular in various club in China. GHB has a strong sedative effect and is often used as a date rape drug and euphoriant in drug-facilitated sexual assaults. However, it is believed that same beverages themselves contain natural GHB. Whether GHB contained in seized beverages was added or exists in themselves resulted in complicated interpretation of the nature of cases. The detection window of GHB in blood (5 h) and urine (<12 h) was narrow, make documentation of GHB exposure difficult, while hair can extend the detection time of GHB from several hours to several days/months. Thus, a sensitive detection method based on dispersive liquid-liquid microextraction (DLLME) and GC-MS/MS for GHB in beverages and hair had been established. Under the optimum extraction conditions, acceptable linear relationship was achieved in the range of 1.5-500 ng/mL with the correlation coefficient (r) of 0.9986 for spiked water samples and in the range of 0.03-10 ng/mg with the correlation coefficient (r) of 0.9979 for spiked melanin samples. The LOD (S/N = 3) was estimated to be 0.5 ng/mL and 0.01 ng/mg, respectively. A recovery of 70.6-88.5% were obtained for spiked samples. The mean relative error (MRE) was within ±6.5% and the relative standard error (RSD) was less than 4.9%. The combination of DLLME with GC-MS/MS offers an alternative analytical approach for the sensitive detection of GHB in real beverages sold in Chinese markets and in hair of Chinese population for forensic purposes. The proposed methods had the advantages of shorter extraction time and were suitable for simultaneous pretreatment of samples in batches. To our knowledge, this is the first report to present GHB in beverages and human hair using DLLME.

摘要

最近,一种名为“Kawa Trendy Drink”的功能性饮料中被检测出含有伽马-羟基丁酸(GHB),该饮料迅速在中国的各种夜店中流行起来。GHB 具有很强的镇静作用,常被用作约会强奸药物和毒品促进的性侵犯中的快感增强剂。然而,人们认为这些饮料本身就含有天然的 GHB。被扣押的饮料中所含的 GHB 是被添加的还是本身存在的,这导致了案件性质的解释变得复杂。GHB 在血液中的检测窗口(5 小时)和尿液中的检测窗口(<12 小时)很窄,使得 GHB 暴露情况的记录变得困难,而头发可以将 GHB 的检测时间从数小时延长至数天/数月。因此,建立了一种基于分散液液微萃取(DLLME)和 GC-MS/MS 的用于检测饮料和头发中 GHB 的灵敏检测方法。在最佳萃取条件下,对于加标水样,在 1.5-500ng/mL 范围内可获得可接受的线性关系,相关系数(r)为 0.9986;对于加标黑素样本,在 0.03-10ng/mg 范围内可获得可接受的线性关系,相关系数(r)为 0.9979。检测限(S/N=3)分别估计为 0.5ng/mL 和 0.01ng/mg。加标样品的回收率为 70.6-88.5%。平均相对误差(MRE)在±6.5%范围内,相对标准偏差(RSD)小于 4.9%。DLLME 与 GC-MS/MS 的结合为在实际销售的中国市场饮料和中国人的头发中对 GHB 进行灵敏检测提供了一种替代分析方法。该方法具有萃取时间短的优点,适合批量同时处理样品。据我们所知,这是首次使用 DLLME 报告饮料和人发中的 GHB。

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