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水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法

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覃东立, 高磊, 黄晓丽, 陈中祥, 王鹏, 郝其睿, 吴松, 汤施展, 白淑艳, 黄丽. 水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法[J]. 环境化学, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
引用本文: 覃东立, 高磊, 黄晓丽, 陈中祥, 王鹏, 郝其睿, 吴松, 汤施展, 白淑艳, 黄丽. 水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法[J]. 环境化学, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
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QIN Dongli, GAO Lei, HUANG Xiaoli, CHEN Zhongxiang, WANG Peng, HAO Qirui, WU Song, TANG Shizhan, BAI Shuyan, HUANG Li. Simultaneous determination of organochlorine pesticides and herbicides residues in water and sediment by gas chromatography tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
Citation: QIN Dongli, GAO Lei, HUANG Xiaoli, CHEN Zhongxiang, WANG Peng, HAO Qirui, WU Song, TANG Shizhan, BAI Shuyan, HUANG Li. Simultaneous determination of organochlorine pesticides and herbicides residues in water and sediment by gas chromatography tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
shu

水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法

  • 1.

    中国水产科学研究院黑龙江水产研究所, 哈尔滨, 150070;

  • 2.

    农业部水产品质量安全控制重点实验室, 北京, 100141

  • 基金项目:

    公益性行业（农业）科研专项（201503108）和中央级公益性科研院所基本科研业务费专项（HSY2016008）资助.

Simultaneous determination of organochlorine pesticides and herbicides residues in water and sediment by gas chromatography tandem mass spectrometry

  • 1.

    Heilongjiang River Fishery Research Institute Chinese Academy of Fishery Sciences, Harbin, 150070, China;

  • 2.

    Key Labrotary of Control of Quality and Safety for Aquatic Products, Ministry of Agriculture, Beijing, 100141, China

  • Fund Project: Supported by the Special Fund for Agro-scientific Research in the Public Interest (201503108) and the Central-Level Non-profit Scientific Research Institutes Special Funds (HSY2016008).

  • 摘要: 本研究建立了水体和底泥中8种有机氯农药和5种除草剂的气相色谱-串联质谱（GC-MS/MS）同步测定分析方法.水样以甲醇作为基体改进剂，利用官能化聚苯乙烯/二乙烯苯（PEP）固相萃取柱富集和净化；底泥样品加乙腈用超声波辅助提取，二氯甲烷反萃取，使用氟罗里硅土固相萃取柱净化.采用DB-5MS（30 m×0.25 mm×0.25 μm）色谱柱对待测物进行分离，多反应监测模式（MRM）测定.方法的线性相关性均大于0.999.空白水样在低、中、高等3个加标水平下的平均回收率为71%—115%，相对标准偏差（RSD）为4.0%—12.6%，检出限（LOD）0.12—2.0 ng·L-1.底泥样品在低、中、高等3个加标水平下，平均回收率为73%—120%，RSD为4.1%—11.0%，检出限（LOD）0.011—0.20 μg·kg-1.该方法选择性好、灵敏度高且准确可靠，适合于水体和底泥中常见有机氯农药和除草剂类农药的检测.应用该方法测定了东北地区养殖池塘及松花江的水体和底泥样品.结果表明，莠去津检出率最高（100%），水体中残留量在11.2—1671 ng·L-1之间，底泥中残留量在0.35—21.8 μg·kg-1之间.有机氯β-六六六检出率 > 80%，水体中残留量在ND—6.76 ng·L-1之间，底泥中残留量在ND—4.74 μg·kg-1之间.底泥样品中滴滴涕农药的残留量未超过我国淡水养殖产地环境限量标准.
    Abstract: A gas chromatography tandem mass spectrometry (GC-MS/MS) method was developed for the simultaneous determination of eight organochlorine pesticides (OCPs) and five herbicides residues in water and sediment samples. Water samples were mixed with methanol which was a matrix modifier, then extracted and cleaned up by Polar Enhanced Polymer solid-phase extraction cartridge (PEP). Sediment samples were extracted with acetonitrile by ultrasonic wave, back-extracted with dichloromethane, and then cleaned up with Florisil solid-phase extraction cartridge. DB-5MS column (30 m×0.25 mm×0.25 μm) was used for compounds separation. Mass spectrometric determination was carried out under multiple reactions monitoring (MRM) mode. For all the calibration curves of 13 analytes, the correlation coefficients were all higher than 0.999. Average recoveries of 13 analytes in blank water samples which spiked at three concentration levels were between 71% and 115%, with RSDs of 4.0%-12.6%. The limit of detection (LOD) was 0.12-2.0 ng·L-1. The average recoveries of 13 analytes in sediment samples at three spiked levels ranged from 73% to 120% with RSDs of 4.1%-11.0%. The LOD was 0.011-0.20 μg·kg-1. This method was suitable for the determination of eight OCPs and five herbicides residues in aquatic environmental water and sediment with high sensitivity and selectivity. The method was used for testing the samples collected from aquaculture pond and Songhua River in northeastern China. The results showed that the detection rate of atrazine was 100%, and the residual amount in water and sediment samples were in the range of 11.2-1671 ng·L-1 and 0.35-21.8 μg·kg-1, respectively. Detection rate of β-HCH was more than 80%, and the residue in water and sediment samples were in the range of nd-6.76 ng·L-1 and nd-4.74 μg·kg-1, respectively. The DDT residues in sediment samples were all less than the maximum residue limits in freshwater aquaculture environment.
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  • 收稿日期:  2017-04-06
  • 刊出日期:  2017-11-15
覃东立, 高磊, 黄晓丽, 陈中祥, 王鹏, 郝其睿, 吴松, 汤施展, 白淑艳, 黄丽. 水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法[J]. 环境化学, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
引用本文: 覃东立, 高磊, 黄晓丽, 陈中祥, 王鹏, 郝其睿, 吴松, 汤施展, 白淑艳, 黄丽. 水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法[J]. 环境化学, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
shu
QIN Dongli, GAO Lei, HUANG Xiaoli, CHEN Zhongxiang, WANG Peng, HAO Qirui, WU Song, TANG Shizhan, BAI Shuyan, HUANG Li. Simultaneous determination of organochlorine pesticides and herbicides residues in water and sediment by gas chromatography tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
Citation: QIN Dongli, GAO Lei, HUANG Xiaoli, CHEN Zhongxiang, WANG Peng, HAO Qirui, WU Song, TANG Shizhan, BAI Shuyan, HUANG Li. Simultaneous determination of organochlorine pesticides and herbicides residues in water and sediment by gas chromatography tandem mass spectrometry[J]. Environmental Chemistry, 2017, 36(11): 2366-2374. doi: 10.7524/j.issn.0254-6108.2017040601
shu

水体与底泥中有机氯和除草剂农药残留的气相色谱串联质谱同步测定方法

  • 1.  中国水产科学研究院黑龙江水产研究所, 哈尔滨, 150070;
  • 2.  农业部水产品质量安全控制重点实验室, 北京, 100141
  • 收稿日期:  2017-04-06
基金项目:

公益性行业（农业）科研专项（201503108）和中央级公益性科研院所基本科研业务费专项（HSY2016008）资助.

摘要: 本研究建立了水体和底泥中8种有机氯农药和5种除草剂的气相色谱-串联质谱（GC-MS/MS）同步测定分析方法.水样以甲醇作为基体改进剂，利用官能化聚苯乙烯/二乙烯苯（PEP）固相萃取柱富集和净化；底泥样品加乙腈用超声波辅助提取，二氯甲烷反萃取，使用氟罗里硅土固相萃取柱净化.采用DB-5MS（30 m×0.25 mm×0.25 μm）色谱柱对待测物进行分离，多反应监测模式（MRM）测定.方法的线性相关性均大于0.999.空白水样在低、中、高等3个加标水平下的平均回收率为71%—115%，相对标准偏差（RSD）为4.0%—12.6%，检出限（LOD）0.12—2.0 ng·L-1.底泥样品在低、中、高等3个加标水平下，平均回收率为73%—120%，RSD为4.1%—11.0%，检出限（LOD）0.011—0.20 μg·kg-1.该方法选择性好、灵敏度高且准确可靠，适合于水体和底泥中常见有机氯农药和除草剂类农药的检测.应用该方法测定了东北地区养殖池塘及松花江的水体和底泥样品.结果表明，莠去津检出率最高（100%），水体中残留量在11.2—1671 ng·L-1之间，底泥中残留量在0.35—21.8 μg·kg-1之间.有机氯β-六六六检出率 > 80%，水体中残留量在ND—6.76 ng·L-1之间，底泥中残留量在ND—4.74 μg·kg-1之间.底泥样品中滴滴涕农药的残留量未超过我国淡水养殖产地环境限量标准.

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