作者：邱世婷1,2, 王艳1,2, 韩梅1,2, 李莹1,2, 向冰1,2, 郑维3, 侯雪1,2
作者单位：1. 四川省农业科学院分析测试中心, 四川 成都 610066;
2. 农业部农产品质量安全风险评估实验室(成都), 四川 成都 610066;
3. 西华师范大学化学化工学院, 四川 南充 637002
关键词：QuEChERS;酰胺类除草剂;超高效液相色谱-串联质谱;土壤;农药残留
摘要：
采用QuEChERS方法结合超高效液相色谱-串联质谱法测定土壤中10种酰胺类除草剂残留量。土壤样品经水和乙腈提取，4 g无水硫酸镁和1 g氯化钠盐析，100 mg PSA净化后用UPLC-MS/MS测定。质谱采用正离子电离和多反应监测模式（MRM），基质匹配标准溶液外标法定量。10种酰胺类除草剂在各自的浓度范围内线性关系良好（r2>0.99）。10种酰胺类除草剂在高、中、低3个添加水平下，回收率为82.7%~114.2%，RSD为1.1%~8.5%，方法的定量限为0.5~100 μg/kg。该方法操作简单、快速、灵敏度和准确度高，适合土壤样品中10种酰胺类除草剂多残留的检测分析。
Determination of ten amide herbicide residues in soil by QuEChERs-ultra high performance liquid chromatography-tandem mass spectrometry
QIU Shiting1,2, WANG Yan1,2, HAN Mei1,2, LI Ying1,2, XIANG Bing1,2, ZHENG Wei3, HOU Xue1,2
1. Analytical and Testing Centre, Sichuan Academy of Agricultural Sciences, Chengdu 610066, China;
2. Laboratory of Risk Assessment for Agricultural Product (Chengdu), Ministry of Agriculture, Chengdu 610066, China;
3. College of Chemistry and Chemical Engineering, China West Normal University, Nanchong 637002, China
Abstract: A new method was adopted for the simultaneous determining of 10 amide herbicide residues in soil by UPLC-MS/MS. The soil samples were extracted by water and acetonitrile, and salted out with 4 g magnesium sulfate and 1 g sodium chloride, then cleaned up by 100 mg primary secondary amine (PSA), the purified extracts were detected by UPLC-MS/MS with positive mode and multiple reactions monitoring (MRM) mode and quantified by matrix-matched external standard calibration curves. The calibration curves of 10 amide herbicide residues showed good linearity. The correlation coefficients were higher than 0.99 and the recoveries of the 10 amide herbicide residues at three spiked levels ranging from 82.7% to 114.2% with the relative standard deviations (RSDs) from 1.1% to 8.5%.The limits of quantification were in the range of 0.5-100 μg/kg. The method is simple, time-saving, sensitive and accurate, and suitable for qualitative and quantitative analysis of the 10 amide herbicide residues in soil.
Keywords: QuEChERS;amide herbicide;ultra liquid chromatography-tandem mass spectrometry;soil;pesticide residues
2019, 45(4):63-67 收稿日期: 2018-11-06;收到修改稿日期: 2018-12-23
基金项目:
作者简介: 邱世婷(1986-),女,四川简阳市人,助理研究员,硕士,主要从事农产品风险评估
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