微萃取柱进样结合气相色谱-串联质谱法用于污水中4种常见毒品的测定

引用本文: 黄晴, 胡胜华, 杨道兵, 王晓如, 邢钧. 微萃取柱进样结合气相色谱-串联质谱法用于污水中4种常见毒品的测定[J]. 分析化学, 2022, 50(1): 153-161. doi: 10.19756/j.issn.0253-3820.210687 shu

Citation: HUANG Qing, HU Sheng-Hua, YANG Dao-Bing, WANG Xiao-Ru, XING Jun. Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(1): 153-161. doi: 10.19756/j.issn.0253-3820.210687 shu

微萃取柱进样结合气相色谱-串联质谱法用于污水中4种常见毒品的测定

黄晴 ^1, ,
胡胜华 ^2, ,
杨道兵 ^2, ,
王晓如 ^1, ,
邢钧 ^{1,
,}

1.
武汉大学化学与分子科学学院, 武汉 430072;
2.
武汉市公安毒品司法鉴定中心, 武汉 430010

通讯作者: 邢钧,E-mail:gc-ms@263.net

摘要: 采用一种适用于气相色谱的针式微萃取技术，即微萃取柱进样（METI）技术，此技术以一段毛细管整体柱（5 cm）作为萃取柱兼进样针，通过将柱内静态解吸和萃取柱直接进样相结合，可实现1 mL水样中ng/L水平分析物的富集。以N-乙烯基吡咯烷酮和二乙烯基苯为单体制备了毛细管整体柱，以4种常见毒品甲基苯丙胺、氯胺酮、去甲氯胺酮和可卡因为目标物，优化了METI的操作条件，结合气相色谱-串联质谱（GC-MS/MS）技术，建立了污水中4种毒品的分析方法。检测甲基苯丙胺、氯胺酮和去甲氯胺酮的线性范围为0.05~50 μg/L，检测可卡因的线性范围为0.10~50 μg/L，相关系数（R²）均大于0.9985，检出限（S/N=3）为0.32~10.00 ng/L，定量限（S/N=10）为1.07~33.00 ng/L。对于湖水水样和污水处理站进水口处水样，在0.3、3和30 μg/L加标水平下的回收率为74.65%~114.36%；除在湖水中加标浓度为0.3 μg/L时，可卡因测试结果的相对标准偏差（RSD）为15.0%外，其它加标回收实验测试结果的RSD均小于10.6%。本研究结果表明，METI集分离、富集和进样功能于一体，具有操作简便和富集效率高等优点，适用于少量样品中痕量组分的快速前处理。

关键词:

English

Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry

1.
College of Chemistry and Molecular Sciences, Wuhan University, Wuhan 430072, China;
2.
Judicial Drug Identification Center, Wuhan City Public Security, Wuhan 430010, China

Corresponding author: XING Jun, gc-ms@263.net

Received Date: 18 August 2021
Revised Date: 22 November 2021

Abstract: Micro-extraction tube injection (METI), a needle-typed micro-extraction technology, has been proposed for gas chromatography (GC). In METI, a section of monolithic capillary tube (5 cm in length) works as an extraction tube and also as an injection needle. Based on the strategy of static desorption in tube and direct injection with tube, METI is able to enrich analytes at ng/L level in water for GC analysis when 1 mL of sample is consumed. In this work, the monolithic capillary tube was prepared with N-vinylpyrrolidone (NVP) and divinylbenzene (DVB), and four kinds of illicit drugs including methamphetamine, ketamine, norketamine and cocaine were tested. After the conditions of METI were optimized, a method of METI coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS) was established for determination of illicit drugs in wastewater. The linear ranges were 0.05-50 μg/L for methamphetamine, ketamine and norketamine, and 0.10-50 μg/L for cocaine with the correlation coefficients (R²) greater than 0.9985. The limits of detection (S/N=3) of the analytes varied from 0.32 to 10.00 ng/L, and the limits of quantification (S/N=10) were in the range of 1.07-33.00 ng/L. The spiking recoveries ranged from 74.65% to 114.36% at spiking levels of 0.3, 3.0 and 30.0 μg/L in water samples from East Lake and intake of wastewater treatment plant, and relative standard deviations (RSDs) were less than 10.6%, except for cocaine which was 15.0% at low concentration in East Lake water. METI integrated separation, enrichment and injection, with the advantages including simple operation and high enrichment efficiency, and could be used for rapid pretreatment of trace components in small amounts of samples.

Key words:

Sample pretreatment
/ Micro-extraction tube injection
/ Illicit drugs
/ Wastewater
/ Gas chromatography-tandem mass spectrometry

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

微萃取柱进样结合气相色谱-串联质谱法用于污水中4种常见毒品的测定

通讯作者: 邢钧,E-mail:gc-ms@263.net

English

Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry

Corresponding author: XING Jun, gc-ms@263.net

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

微萃取柱进样结合气相色谱-串联质谱法用于污水中4种常见毒品的测定

通讯作者: 邢钧,E-mail:gc-ms@263.net

English

Determination of Four Kinds of Illicit Drugs in Wastewater by Micro-extraction Tube Injection Coupled with Gas Chromatography-Tandem Mass Spectrometry

Corresponding author: XING Jun, gc-ms@263.net

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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