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高冉, 饶竹, 郭晓辰. 地下水中91种农药多残留气相色谱-质谱分析方法研究及应用[J]. 岩矿测试, 2021, 40(6): 973-986. DOI: 10.15898/j.cnki.11-2131/td.202011170148
引用本文: 高冉, 饶竹, 郭晓辰. 地下水中91种农药多残留气相色谱-质谱分析方法研究及应用[J]. 岩矿测试, 2021, 40(6): 973-986. DOI: 10.15898/j.cnki.11-2131/td.202011170148
GAO Ran, RAO Zhu, GUO Xiao-chen. Analysis of 91 Pesticide Residues in Groundwater by Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2021, 40(6): 973-986. DOI: 10.15898/j.cnki.11-2131/td.202011170148
Citation: GAO Ran, RAO Zhu, GUO Xiao-chen. Analysis of 91 Pesticide Residues in Groundwater by Gas Chromatography-Mass Spectrometry[J]. Rock and Mineral Analysis, 2021, 40(6): 973-986. DOI: 10.15898/j.cnki.11-2131/td.202011170148

地下水中91种农药多残留气相色谱-质谱分析方法研究及应用

Analysis of 91 Pesticide Residues in Groundwater by Gas Chromatography-Mass Spectrometry

  • 摘要: 地下水中多种农药快速检测是全面表征地下水水质、确保地下水安全的重要技术支撑。本文结合现有检测标准和文献中农药需分类分别前处理和测试的问题,采用气相色谱-质谱仪,通过对水样前处理方法和气相色谱-质谱分析条件进行选择和优化,建立了地下水中91种农药气相色谱-质谱同时测定的快速分析方法。经优化,目标物采用脉冲不分流进样,Zebron Multiresidue-2色谱柱分离,分段选择离子扫描,内标法定量,多数农药在1.0~1000μg/L浓度范围内线性良好,相关系数在0.9901~0.9997之间。水样经二氯甲烷液液萃取浓缩后上机测试,各农药方法检出限为3.1~12.5ng/L,平均加标回收率在54.3%~129%之间,相对标准偏差(RSD)为1.2%~20%。本方法快速、简单,准确度高,不仅显著提高了地下水中多种类农药残留分析效率,降低了分析成本;而且方法更适合大批量地下水样品的快速筛查,从而保证了样品分析的时效性。该方法已成功应用于全国地下水污染调查专项。

     

    Abstract:
    BACKGROUNDFast screening of multiple pesticides in groundwater is an important technical support for comprehensively characterizing groundwater quality and ensuring groundwater safety.
    OBJECTIVESTo establish a rapid, easy and highly efficient method for the determination of 91 pesticides in groundwater.
    METHODSBy selecting and optimizing the water sample pretreatment method and gas chromatography-mass spectrometry analysis conditions, a rapid analysis method for the simultaneous determination of 91 pesticides in groundwater by gas chromatography-mass spectrometry (GC-MS) was established. The targets were determined by GC-MS and quantified by an internal standard. After optimization, the target substance adopts pulsed splitless injection, separated by Zebron Multiresidue-2 chromatographic column, and segmented selective ion scanning.
    RESULTSUnder the optimized conditions, pesticides showed good linearity with the correlation coefficient between 0.9901 and 0.9997 in the concentration range of 1.0-1000μg/L. The water sample was subjected to liquid-liquid extraction and concentration of dichloromethane and then tested on the machine, yielding method detection limits (MDLs) of 3.1-12.5ng/L, the average recoveries of 54.3%-129%, and the relative standard deviation (RSD) of 1.2% to 20%.
    CONCLUSIONSCompared to previous studies, the method not only greatly improves the efficiency, reduces the cost of analysis, ensures the effectiveness of sample analysis, but also has wide applicability, high accuracy and high sensitivity. The method is more suitable for analysis of large batches of samples, which ensures the timeliness of sample analysis. The method has been successfully applied to the national groundwater pollution survey.

     

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