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气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留

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王正全, 崔云云, 陈力, 陈健康, 俞骏, 刘源, 汪立平, 赵勇, 谢晶. 气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留[J]. 环境化学, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
引用本文: 王正全, 崔云云, 陈力, 陈健康, 俞骏, 刘源, 汪立平, 赵勇, 谢晶. 气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留[J]. 环境化学, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
shu
WANG Zhengquan, CUI Yunyun, CHEN Li, CHEN Jiankang, YU Jun, LIU Yuan, WANG Liping, ZHAO Yong, XIE Jing. Determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
Citation: WANG Zhengquan, CUI Yunyun, CHEN Li, CHEN Jiankang, YU Jun, LIU Yuan, WANG Liping, ZHAO Yong, XIE Jing. Determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
shu

气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留

  • 1.

    上海海洋大学食品学院, 上海, 201306;

  • 2.

    农业部水产品贮藏保鲜质量安全风险评估实验室(上海), 上海, 201306;

  • 3.

    上海水产品加工及贮藏工程技术研究中心, 上海, 201306

  • 基金项目:

    国家自然科学基金（31401486），上海市教育委员会科研（创新）项目（ZZHY13018）和上海海洋大学博士启动基金（A-0209-13-0105345）资助.

Determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry

  • 1.

    College of Food Science and Technology, Shanghai Ocean University, Shanghai, 201306, China;

  • 2.

    Laboratory of Quality and Safety Risk Assessment for Aquatic Products on Storage and Preservation(Shanghai), Ministry of Agriculture, Shanghai, 201306, China;

  • 3.

    Shanghai Engineering Research Center of Aquatic-Product Processing & Preservation, Shanghai, 201306, China

  • Fund Project: Supported by the National Natural Science Foundation of China (31401486), Innovation Program of Shanghai Municipal Education Commission (ZZHY13018) and Shanghai Ocean University Scientific Research Foundation for Doctor Project (A-0209-13-0105345).

  • 摘要: 本文建立了环境水和饮用水中37种农药和环境激素残留的大体积进样气相色谱质谱检测方法.环境水和饮用水样经简单净化处理后用两种不同极性有机溶剂萃取，混合有机相直接浓缩至干并定容检测，使用内标法定量.基质方法开发过程中优化了萃取溶剂、大体积进样量、磁力搅拌超声萃取时间、样品量和离心时间等参数，最终优化的方法确定使用正己烷和二氯甲烷做萃取溶剂、20 mL大体积进样量、5 min磁力搅拌超声萃取时间、20 mL水样品量、2 min超高速离心，且在基质提取液浑浊情况下加NaCl和无水硫酸镁辅助萃取时效果最佳.该方法的最低定量浓度（LOQs）为0.012—0.141 μg·L-1，在5.0—25000.0 μg·L-1线性范围内线性相关系数r2范围在0.9955—1.0000.本方法可用于6种上海市和北京市地区的环境水和饮用水样基质的检测，6种基质加标的平均回收率范围维持在80%—117%，6次平行测定结果相对标准偏差（RSDs）小于20%.在针对2014年的沪浙闽地区的16个及2015年的230个养殖水样的检测结果显示均为阴性未检出，该方法是一种简单易操作、低消耗、低污染、快速的检测方法.
    Abstract: A method for the determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry (LVI-GC-MS) was established. Samples were purified with simple operation, extracted with two different polar organic solvents, and then directly concentrated and dried for determination. The parameters such as the extraction solvent, extraction time, ultrasonic extraction time, sample amount and centrifugal time were optimized. As a result, dichloromethane and n-hexane, 20 mL injection volume, 5 min extraction time by using ultrasonic with stir bar, 20 mL water sample amount, 2 min ultra-high speed centrifugation, and NaCl-plus MgSO4-assisted extraction in case turbid happens were selected, and the internal standard method was used. The limit of quantifications (LOQs) ranged from 0.012 to 0.141 μg·L-1, and the correlation coefficients r2 were 0.9955 to 1.0000 with a linear range of 5.0 to 25000 μg·L-1. This method was successfully applied to the analysis of six different matrices of environmental water and drinking water obtained from Shanghai and Beijing, and the spiked recoveries of 37 pesticides and environmental hormones were maintained at 80% to 117%, while the relative standard deviations (RSDs) of 6 parallel measurements were less than 20%. Furthermore, the aquaculture practice water samples obtained from Shanghai, Zhejiang and Fujian province during 2014 (16)-2015 (230) were also investigated, which showed negative results. The established method is simple, rapid, convenient, efficient and accurate with high sensitivity and low-cost, and is also considered environmental friendly.
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  • 收稿日期:  2017-09-21
  • 刊出日期:  2018-06-15
王正全, 崔云云, 陈力, 陈健康, 俞骏, 刘源, 汪立平, 赵勇, 谢晶. 气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留[J]. 环境化学, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
引用本文: 王正全, 崔云云, 陈力, 陈健康, 俞骏, 刘源, 汪立平, 赵勇, 谢晶. 气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留[J]. 环境化学, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
shu
WANG Zhengquan, CUI Yunyun, CHEN Li, CHEN Jiankang, YU Jun, LIU Yuan, WANG Liping, ZHAO Yong, XIE Jing. Determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
Citation: WANG Zhengquan, CUI Yunyun, CHEN Li, CHEN Jiankang, YU Jun, LIU Yuan, WANG Liping, ZHAO Yong, XIE Jing. Determination of 37 pesticides and environmental hormones residues in environmental water and drinking water by large volume injection-gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1362-1375. doi: 10.7524/j.issn.0254-6108.2017092403
shu

气相色谱质谱大体积进样法检测环境水和饮用水中37种农药和环境激素的残留

  • 1.  上海海洋大学食品学院, 上海, 201306;
  • 2.  农业部水产品贮藏保鲜质量安全风险评估实验室(上海), 上海, 201306;
  • 3.  上海水产品加工及贮藏工程技术研究中心, 上海, 201306
  • 收稿日期:  2017-09-21
基金项目:

国家自然科学基金（31401486），上海市教育委员会科研（创新）项目（ZZHY13018）和上海海洋大学博士启动基金（A-0209-13-0105345）资助.

摘要: 本文建立了环境水和饮用水中37种农药和环境激素残留的大体积进样气相色谱质谱检测方法.环境水和饮用水样经简单净化处理后用两种不同极性有机溶剂萃取，混合有机相直接浓缩至干并定容检测，使用内标法定量.基质方法开发过程中优化了萃取溶剂、大体积进样量、磁力搅拌超声萃取时间、样品量和离心时间等参数，最终优化的方法确定使用正己烷和二氯甲烷做萃取溶剂、20 mL大体积进样量、5 min磁力搅拌超声萃取时间、20 mL水样品量、2 min超高速离心，且在基质提取液浑浊情况下加NaCl和无水硫酸镁辅助萃取时效果最佳.该方法的最低定量浓度（LOQs）为0.012—0.141 μg·L-1，在5.0—25000.0 μg·L-1线性范围内线性相关系数r2范围在0.9955—1.0000.本方法可用于6种上海市和北京市地区的环境水和饮用水样基质的检测，6种基质加标的平均回收率范围维持在80%—117%，6次平行测定结果相对标准偏差（RSDs）小于20%.在针对2014年的沪浙闽地区的16个及2015年的230个养殖水样的检测结果显示均为阴性未检出，该方法是一种简单易操作、低消耗、低污染、快速的检测方法.

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