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环境样品中苯二氮类镇静催眠药物的分析方法

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雷浩俊, 杨滨, 叶璞, 赵建亮, 黄月明. 环境样品中苯二氮类镇静催眠药物的分析方法[J]. 环境化学, 2020, (8): 2296-2306. doi: 10.7524/j.issn.0254-6108.2019061203
引用本文: 雷浩俊, 杨滨, 叶璞, 赵建亮, 黄月明. 环境样品中苯二氮类镇静催眠药物的分析方法[J]. 环境化学, 2020, (8): 2296-2306. doi: 10.7524/j.issn.0254-6108.2019061203
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LEI Haojun, YANG Bin, YE Pu, ZHAO Jianliang, HUANG Yueming. Analytical method of benzodiazepines in environmental samples[J]. Environmental Chemistry, 2020, (8): 2296-2306. doi: 10.7524/j.issn.0254-6108.2019061203
Citation: LEI Haojun, YANG Bin, YE Pu, ZHAO Jianliang, HUANG Yueming. Analytical method of benzodiazepines in environmental samples[J]. Environmental Chemistry, 2020, (8): 2296-2306. doi: 10.7524/j.issn.0254-6108.2019061203
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环境样品中苯二氮类镇静催眠药物的分析方法

  • 华南师范大学环境研究院, 广东省化学品污染与环境安全重点实验室, 广州, 510006

    • 通讯作者: 杨滨, E-mail: bin.yang@m.scnu.edu.cn ; 
  • 基金项目:

    国家自然科学基金（41877358，21806043）和广州市科技创新发展专项资金（201804010108）资助.

Analytical method of benzodiazepines in environmental samples

  • Guangdong Provincial Key Laboratory of Chemical Pollution and Environmental Safety, SCNU Environmental Research Institute, South China Normal University, Guangzhou, 510006, China

    • Corresponding author: YANG Bin, bin.yang@m.scnu.edu.cn ; 
  • Fund Project: Supported by the National Natural Science Foundation of China (41877358, 21806043) and Science and Technology Innovation Development Program of Guangzhou, China (201804010108).

  • 摘要: 近年有关药物及其转化产物的环境污染问题引起了人们的广泛关注.苯二氮类药物是一类作用于中枢神经系统的药物，其母体化合物和代谢产物均具有镇静、催眠及抗焦虑等作用.本文建立了17种苯二氮类药物及其3种中间产物，在环境水相和固相样品中的分析检测方法.水样采用HLB柱进行固相萃取，固体样以柠檬酸缓冲液和乙腈混合液进行超声提取，采用同位素稀释法进行定量，超高效液相色谱-串联四极杆质谱法（UPLC-MS/MS）分析.分析检测方法对地表水样、污水厂进水、污水厂出水的基质加标平均回收率分别为84.1%-130.6%、57.5%-127.6%和60.3%-141.8%；对沉积物和污泥加标平均回收率为57.9%-131.3%和52.2%-150.5%.地表水、污水厂进水、出水的方法检出限分别为0.008-0.166、0.006-0.114、0.005-0.124 ng·L-1；沉积物和污泥的方法检出限为0.002-0.110 ng·g-1和0.003-0.041 ng·g-1.应用所建立的分析检测方法，对深圳市茅洲河（水样及沉积物）和广州市某城市污水处理厂（进出水及脱水污泥）进行分析测试.结果表明，茅洲河水样及沉积物中目标物浓度范围分别在0.11-4.83 ng·L-1和0.04-3.31 ng·g-1之间，广州市某城市污水处理厂进出水及污泥中目标物浓度范围分别在0.22-24.21、0.04-2.74、0.09-10.80 ng·g-1之间.
    Abstract: In recent years pharmaceuticals and their transformation products have received increasing attentions in general public and scientific community due to their environmental contamination issue. Benzodiazepines are a class of psychiatric pharmaceuticals which can affect mammalian central nervous system functions. Benzodiazepines and their metabolites have sedative, muscle relaxant, anxiolytic, anticonvulsive and antiepileptic properties. In this study, the analytical methods for the determination of 17 benzodiazepines and their 3 intermediates in environmental aqueous and solid samples were developed and optimized by combining solid phase extraction or ultrasonic extraction and ultra-pressure liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) with isotopic dilution method. Under the optimized conditions, the average spiked recoveries of the analytes in environmental surface water samples, wastewater treatment plant (WWTP) influents, WWTP effluents ranged from 84.1% to 130.6%, 57.5% to 127.6% and 60.3% to 141.8%, and in the sediment and sludge ranged from 57.9% to 131.3% and 52.2% to 150.5%, respectively. The method detection limits for the surface water, influents and effluents ranged from 0.008 ng·L-1 to 0.166 ng·L-1, 0.006 ng·L-1 to 0.114 ng·L-1 and 0.005 ng·L-1 to 0.124 ng·L-1, and for the sediment and sludge from 0.002 ng·g-1 to 0.110 ng·g-1 and 0.002 ng·g-1 to 0.041 ng·g-1, respectively. The occurrence of the benzodiazepines in Maozhou River (Shenzhen) and a WWTP (Guangzhou) were investigated and analyzed by using the established method. The concentration range of benzodiazepines in water samples and sediments of Maozhou River was from 0.11 ng·g-1 to 4.83 ng·g-1 and 0.04 ng·g-1 to 3.31 ng·g-1, respectively. While the concentrations of benzodiazepines in the WWTP influent, effluent and sludge ranged from 0.22 ng·g-1 to 24.21 ng·g-1, 0.04 ng·g-1 to 2.74 ng·g-1 and 0.09 ng·g-1 to 10.80 ng·g-1, respectively.
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  • 收稿日期:  2019-06-12

环境样品中苯二氮类镇静催眠药物的分析方法

    通讯作者: 杨滨, E-mail: bin.yang@m.scnu.edu.cn ; 
  • 华南师范大学环境研究院, 广东省化学品污染与环境安全重点实验室, 广州, 510006
  • 收稿日期:  2019-06-12
基金项目:

国家自然科学基金（41877358，21806043）和广州市科技创新发展专项资金（201804010108）资助.

摘要: 近年有关药物及其转化产物的环境污染问题引起了人们的广泛关注.苯二氮类药物是一类作用于中枢神经系统的药物，其母体化合物和代谢产物均具有镇静、催眠及抗焦虑等作用.本文建立了17种苯二氮类药物及其3种中间产物，在环境水相和固相样品中的分析检测方法.水样采用HLB柱进行固相萃取，固体样以柠檬酸缓冲液和乙腈混合液进行超声提取，采用同位素稀释法进行定量，超高效液相色谱-串联四极杆质谱法（UPLC-MS/MS）分析.分析检测方法对地表水样、污水厂进水、污水厂出水的基质加标平均回收率分别为84.1%-130.6%、57.5%-127.6%和60.3%-141.8%；对沉积物和污泥加标平均回收率为57.9%-131.3%和52.2%-150.5%.地表水、污水厂进水、出水的方法检出限分别为0.008-0.166、0.006-0.114、0.005-0.124 ng·L-1；沉积物和污泥的方法检出限为0.002-0.110 ng·g-1和0.003-0.041 ng·g-1.应用所建立的分析检测方法，对深圳市茅洲河（水样及沉积物）和广州市某城市污水处理厂（进出水及脱水污泥）进行分析测试.结果表明，茅洲河水样及沉积物中目标物浓度范围分别在0.11-4.83 ng·L-1和0.04-3.31 ng·g-1之间，广州市某城市污水处理厂进出水及污泥中目标物浓度范围分别在0.22-24.21、0.04-2.74、0.09-10.80 ng·g-1之间.

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