在线固相萃取-超高效液相色谱/串联质谱法测定水中的11种精神活性物质

殷行行; 郭昌胜; 邓洋慧; 王玮敏; 袁汉成; 孙文军; 徐建

环境化学

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殷行行, 郭昌胜, 邓洋慧, 王玮敏, 袁汉成, 孙文军, 徐建. 在线固相萃取-超高效液相色谱/串联质谱法测定水中的11种精神活性物质[J]. 环境化学, 2019, (12): 2883-2888.

引用本文:

YIN Xingxing, GUO Chansgheng, DENG Yanghui, WANG Weimin, YUAN Hancheng, SUN Wenjun, XU Jian. Determination of 11 psychoactive substances in water by ultra performance liquid chromatography-tandem mass spectrometry coupled with online solid phase extraction[J]. Environmental Chemistry, 2019, (12): 2883-2888.

Citation:

在线固相萃取-超高效液相色谱/串联质谱法测定水中的11种精神活性物质

1. 中国环境科学研究院环境健康风险评估与研究中心, 北京, 100012;
2. 北京师范大学水科学研究院, 北京, 100875;
3. 环境基准与风险评估国家重点实验室, 北京, 100012;
4. 国家环境保护化学品生态效应与风险评估重点实验室, 北京, 100012;
5. 沃特世科技(上海)有限公司, 北京, 100026

通讯作者: 徐建, E-mail: xujian@craes.org.cn

基金项目:
国家水体污染控制与治理科技重大专项（2017ZX07301005-003，2017ZX07302001）和国家自然科学基金（41673120）资助．

Determination of 11 psychoactive substances in water by ultra performance liquid chromatography-tandem mass spectrometry coupled with online solid phase extraction

1. Center for Environmental Health Risk Assessment and Research, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
2. College of Water Sciences, Beijing Normal University, Beijing, 100875, China;
3. State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
4. State Environmental Protection Key Laboratory of Ecological Effect and Risk Assessment of Chemicals, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
5. Waters Technologies(Shanghai) Limited, Beijing, 100026, China

Corresponding author: XU Jian, xujian@craes.org.cn

Fund Project: Supported by the National Water Pollution Control and Management Science and Technology Major Project (2017ZX07301005-003, 2017ZX07302001) and the National Natural Science Foundation of China (41673120).

摘要: 采用在线固相萃取-超高效液相色谱/串联质谱技术，建立了地表水中广泛存在的11种精神活性物质的检测方法.样品经微孔滤膜过滤后，用甲酸调节至pH=3.0，直接进入在线固相萃取-超高效液相色谱/串联质谱仪进行分析.样品以Oasis HLB萃取柱净化富集，被流动相反冲出萃取柱后进入UPLC系统，采用Waters ACQUITY BEH C18色谱柱分离.上样泵（四元泵）的流动相为纯水和体积分数为0.5%的甲酸乙腈溶液，分析泵（二元泵）的流动相为乙腈和体积分数为0.1%的甲酸水溶液.以电喷雾正离子（ESI+）多反应监测模式（MRM）进行定性定量分析.该方法分析时长13.0 min，11种精神活性物质在0-10 ng·L^-1范围内线性关系良好，线性相关系数R²≥ 0.9877，检出限≤0.1 ng·L^-1，6次平行测定峰面积RSD≤10.80%.该方法前处理简单、快速、重现性好，可用于环境水体和饮用水中痕量精神活性物质的测定.将建立的方法应用于北京市城市地表水及污水处理厂采集的水样分析，地表水中未检测到苯丙胺，污水处理厂水样中检测出11种精神活性物质，其中浓度最高的为可替宁，在进水中最高可达到2035.28 ng·L^-1.
- 精神活性物质 /
- 地表水 /
- 在线固相萃取 /
- 超高效液相色谱/串联质谱法
Abstract: An on-line solid phase extraction (SPE)-high performance liquid chromatography-tandem mass spectrometry system was used for the simple and sensitive determination of 11 psychoactive substances in water. These psychoactive substances are widespread in the aquatic environment and encompass multiple categories. After filtered through a microporous membrane, water samples were adjusted to pH=3.0 with formic acid and directly injected to the on-line SPE- high performance liquid chromatography-tandem mass spectrometry system. The samples were adsorbed to the online SPE Oasis^® HLB column, back-flushed into UPLC system with the mobile phase and separated on a Waters ACQUITY C18 column. The target compounds were separated on a Waters ACQUITY C18 column. The mobile phase used for on-line SPE (Quaternary Solvent Manager, QSM) was water and 5‰ formic acid in acetonitrile, and that used for separation (Binary Solvent Manager, BSM) was acetonitrile and 1‰ formic acid in water. Electrospray ionization source was used under positive electrospray ionization (ESI+) and multiple-reaction monitoring (MRM) mode. The complete analysis only requires 13 min. The relative standard deviation (RSD) of 11 psychoactive substances were all less than 10. 80% for peak area (n=6). Good linearity was obtained from 0 to 10 μg·L^-1 with the correlation coefficients of above 0.9877 for all the 11 target compounds; and the method detection limits (MDL) were all less than 0.1 ng·L^-1 for the 11 target compounds.
- psychoactive substances /
- surface water /
- on-line SPE /
- ultra performance liquid chromatography-tandem mass spectrometry

[1]	胡鹏, 张艳, 郭昌胜, 等. 水环境中滥用药物的环境学研究进展[J]. 环境化学, 2017, 36(8):1711-1723. HU P, ZHANG Y, GUO C S, et al. Environmental studies on drugs of abuse in the aquatic environment[J]. Environmental Chemistry, 2017, 36(8):1711-1723(in Chinese).
[2]	FELIX L M, ANTUNES L M, COIMBRA A M. Ketamine NMDA receptor-independent toxicity during zebrafish (Danio rerio) embryonic development[J]. Neurotoxicology and Teratology, 2014, 41:27-34.
[3]	GUO R, LIU G, DU M, et al. Early ketamine exposure results in cardiac enlargement and heart dysfunction in Xenopus embryos[J]. BMC Anesthesiology, 2016, 16:23.
[4]	PAROLINI M, MAGNI S, CASTIGLIONI S, et al. Realistic mixture of illicit drugs impaired the oxidative status of the zebra mussel (Dreissena polymorpha)[J]. Chemosphere, 2015, 128:96-102.
[5]	LIAO P H, HWANG C C, Chen T H, et al. Developmental exposures to waterborne abused drugs alter physiological function and larval locomotion in early life stages of medaka fish[J]. Aquatic Toxicology, 2015, 165:84-92.
[6]	张艳, 张婷婷, 郭昌胜, 等. 北京市城市河流中精神活性物质的污染水平及环境风险[J]. 环境科学研究, 2016, 29(6):845-853. ZHANG Y, ZHANG T T, GUO C S, et al. Pollution status and environmental risks of illicit drugs in the urban rivers of Beijing[J]. Research of Environmental Sciences, 2016, 29(6):845-853(in Chinese).
[7]	GUO C, ZHANG T, HOU S, et al. Investigation and application of a new passive sampling technique for in situ monitoring of illicit drugs in waste waters and rivers[J]. Environmental Science &Technology, 2017, 51:9101-9108.
[8]	ZHANG Y, ZHANG T, GUO C, et al. Drugs of abuse and their metabolites in the urban rivers of Beijing, China:Occurrence, distribution, and potential environmental risk[J]. Science of the Total Environment, 2017, 579:305-313.
[9]	FONTANALS N, MARCÉ R M, BORRULL F. On-line solid-phase extraction coupled to hydrophilic interaction chromatography - mass spectrometry for the determination of polar drugs[J]. Journal of Chromatography A, 2011, 1218:5975-5980.
[10]	YAO B, LIAN L, PANG W, et al. Determination of illicit drugs in aqueous environmental samples by online solid-phase extraction coupled to liquid chromatography-tandem mass spectrometry[J]. Chemosphere, 2016, 160:208-215.
[11]	李明昕, 王倩, 朱婧, 等. 亲水作用色谱-串联质谱测定尿液中尼古丁和可替宁[J]. 色谱, 2017, 35(8):826-831. LI M X, WANG Q, ZHU Q, et al。Determination of nicotine and cotinine in urine by hydrophilic interaction chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatagraphy, 2017, 35(8):826-831(in Chinese).
[12]	中国禁毒委员会. 2018年中国毒品形势报告[R]. 北京:中国禁毒委员会, 2019.

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在线固相萃取-超高效液相色谱/串联质谱法测定水中的11种精神活性物质

通讯作者: 徐建, E-mail: xujian@craes.org.cn

1. 中国环境科学研究院环境健康风险评估与研究中心, 北京, 100012;
2. 北京师范大学水科学研究院, 北京, 100875;
3. 环境基准与风险评估国家重点实验室, 北京, 100012;
4. 国家环境保护化学品生态效应与风险评估重点实验室, 北京, 100012;
5. 沃特世科技(上海)有限公司, 北京, 100026

基金项目:

国家水体污染控制与治理科技重大专项（2017ZX07301005-003，2017ZX07302001）和国家自然科学基金（41673120）资助．

关键词:

摘要: 采用在线固相萃取-超高效液相色谱/串联质谱技术，建立了地表水中广泛存在的11种精神活性物质的检测方法.样品经微孔滤膜过滤后，用甲酸调节至pH=3.0，直接进入在线固相萃取-超高效液相色谱/串联质谱仪进行分析.样品以Oasis HLB萃取柱净化富集，被流动相反冲出萃取柱后进入UPLC系统，采用Waters ACQUITY BEH C18色谱柱分离.上样泵（四元泵）的流动相为纯水和体积分数为0.5%的甲酸乙腈溶液，分析泵（二元泵）的流动相为乙腈和体积分数为0.1%的甲酸水溶液.以电喷雾正离子（ESI+）多反应监测模式（MRM）进行定性定量分析.该方法分析时长13.0 min，11种精神活性物质在0-10 ng·L^-1范围内线性关系良好，线性相关系数R²≥ 0.9877，检出限≤0.1 ng·L^-1，6次平行测定峰面积RSD≤10.80%.该方法前处理简单、快速、重现性好，可用于环境水体和饮用水中痕量精神活性物质的测定.将建立的方法应用于北京市城市地表水及污水处理厂采集的水样分析，地表水中未检测到苯丙胺，污水处理厂水样中检测出11种精神活性物质，其中浓度最高的为可替宁，在进水中最高可达到2035.28 ng·L^-1.

English Abstract

Determination of 11 psychoactive substances in water by ultra performance liquid chromatography-tandem mass spectrometry coupled with online solid phase extraction

Corresponding author: XU Jian, xujian@craes.org.cn

1. Center for Environmental Health Risk Assessment and Research, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
2. College of Water Sciences, Beijing Normal University, Beijing, 100875, China;
3. State Key Laboratory of Environmental Criteria and Risk Assessment, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
4. State Environmental Protection Key Laboratory of Ecological Effect and Risk Assessment of Chemicals, Chinese Research Academy of Environmental Sciences, Beijing, 100012, China;
5. Waters Technologies(Shanghai) Limited, Beijing, 100026, China

Fund Project: Supported by the National Water Pollution Control and Management Science and Technology Major Project (2017ZX07301005-003, 2017ZX07302001) and the National Natural Science Foundation of China (41673120).

Keywords:

psychoactive substances /
surface water /
on-line SPE /
ultra performance liquid chromatography-tandem mass spectrometry

Abstract: An on-line solid phase extraction (SPE)-high performance liquid chromatography-tandem mass spectrometry system was used for the simple and sensitive determination of 11 psychoactive substances in water. These psychoactive substances are widespread in the aquatic environment and encompass multiple categories. After filtered through a microporous membrane, water samples were adjusted to pH=3.0 with formic acid and directly injected to the on-line SPE- high performance liquid chromatography-tandem mass spectrometry system. The samples were adsorbed to the online SPE Oasis^® HLB column, back-flushed into UPLC system with the mobile phase and separated on a Waters ACQUITY C18 column. The target compounds were separated on a Waters ACQUITY C18 column. The mobile phase used for on-line SPE (Quaternary Solvent Manager, QSM) was water and 5‰ formic acid in acetonitrile, and that used for separation (Binary Solvent Manager, BSM) was acetonitrile and 1‰ formic acid in water. Electrospray ionization source was used under positive electrospray ionization (ESI+) and multiple-reaction monitoring (MRM) mode. The complete analysis only requires 13 min. The relative standard deviation (RSD) of 11 psychoactive substances were all less than 10. 80% for peak area (n=6). Good linearity was obtained from 0 to 10 μg·L^-1 with the correlation coefficients of above 0.9877 for all the 11 target compounds; and the method detection limits (MDL) were all less than 0.1 ng·L^-1 for the 11 target compounds.