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基于全二维气相色谱-四极杆飞行时间质谱法同时检测土壤中 24种有机磷与20种有机氯农药残留
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余 磊,赵志燊,赵 杰,向章敏 1. 贵阳学院 贵州生态环境中优势农产品残留农药降解关键技术研究重点实验室贵州 贵阳 550005 2. 广东省科学院测试分析研究所 广东省化学危害应急检测技术重点实验室广东 广州 510070 
基金项目:贵阳市科技局贵阳学院专项资金资助[GYU-KY-(2021)];贵州生态环境中优势农产品残留农药降解关键技术研究重点 实验室项目[黔教合KY字(2018)005]
中文摘要:基于全二维气相色谱-四极杆飞行时间质谱(GC × GC-Q-TOF MS)建立了土壤样品中24种有机磷 和20种有机氯农药残留的快速同时检测方法,样品经索氏提取后直接采用全二维气相色谱进行分离,有效实 现了杂质与目标物的完全族分离效果。以24种有机磷和20种有机氯农药的高分辨精确质量特征离子进行定 量分析,结果表明,44 种农药均在 20~3 000 μg/L 质量浓度范围内呈线性关系,相关系数(r 2 )为 0. 990 3~ 0. 999 9,检出限(LOD)为 0. 3~7. 9 μg/L;方法的平均回收率为 93. 0%,平均相对标准偏差(RSD,n = 5)为 6. 9%。该文可为土壤中农药残留的高通量快速筛查提供方法参考。
中文关键词:全二维气相色谱-四极杆飞行时间质谱  有机磷  有机氯  土壤
 
Simultaneous Determination of 24 Organo? phosphorus and 20 Organochlorine Pesti? cides in Soil by GC × GC-Q-TOF MS
Abstract:A comprehensive two-dimensional gas chromatography quadrupole time-of-flight mass spectrometry(GC × GC-Q-TOF MS)was developed for the rapid and simultaneous determination of 24 organophosphorus and 20 organochlorine pesticides in soil. The impurities and analytes in samples were perfectly intragroup-separated by two-dimensional gas chromatography after soxhlet extraction. 24 organophosphorus and 20 organochlorine pesticides were determined by using the high resolution molecular mass characteristic ions. Results showed that there existed linear relationships for 44 pesticides in the concentration range of 20-3 000 μg/L,with their correlation coefficients(r 2 )of 0. 990 3-0. 999 9 and limits of detection(LOD)of 0. 3-7. 9 μg/L. The average value for fortified recovery was 93. 0%,and accordingly the relative standard deviation(RSD,n = 5)was 6. 9%. The method could provide a reference for the high-throughput rapid screening of pesticide residues in soil.
Key Words:comprehensive two-dimensional gas chromatography quadrupole time-of-flight mass spectrometry  organophosphorus pesticides  organochlorine pesticides  soil
引用本文:余 磊,赵志燊,赵 杰,向章敏.基于全二维气相色谱-四极杆飞行时间质谱法同时检测土壤中 24种有机磷与20种有机氯农药残留[J].分析测试学报,2021,40(8):1184-1189.
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