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中国农学通报

中国农学通报 ›› 2022, Vol. 38 ›› Issue (36): 126-131.doi: 10.11924/j.issn.1000-6850.casb2022-0282

• 植物保护·农药 • 上一篇    下一篇

QuEChERS-高效液相色谱-串联质谱法测定水稻中氯虫苯甲酰胺和噻虫胺的残留

孙悦萍1,2(), 周芹1,3,4(), 徐利剑1(), 任红波2, 马文琼2, 张晓波2, 金海涛2, 陈国峰2, 刘峰2, 董见南2   

  1. 1黑龙江大学现代农业与生态环境学院，哈尔滨 150080
    2黑龙江省农业科学院农产品质量安全研究所，哈尔滨 150086
    3农业农村部甜菜品质监督检验测试中心，哈尔滨 150080
    4农业农村部糖料产品质量安全风险评估实验室，哈尔滨 150080
  • 收稿日期:2022-04-13 修回日期:2022-07-27 出版日期:2022-12-25 发布日期:2023-01-17
  • 作者简介:

    孙悦萍，女，1986年出生，黑龙江齐齐哈尔人，主要从事食品质量安全及环境检验工作。通信地址：150086 哈尔滨市南岗区学府路368号农科创新大厦1011室，Tel：0451-86617148，E-mail：。

  • 基金资助:
    《农药产品中有效成分测定通用分析方法-液相色谱法》体系建设“啶磺草胺等10个农药品种液相色谱分析方法建立”(14192195); 现代农业产业技术体系建设项目“质量安全与营养品质评价”(CARS-170503)

Chlorantraniliprole and Clothianidin Residues in Rice: Determined by QuEChERS-High Performance Liquid Chromatography-Tandem Mass Spectrometry

SUN Yueping1,2(), ZHOU Qin1,3,4(), XU Lijian1(), REN Hongbo2, MA Wenqiong2, ZHANG Xiaobo2, JIN Haitao2, CHEN Guofeng2, LIU Feng2, DONG Jiannan2   

  1. 1College of Modern Agricultural Ecology and Environment of Heilongjiang University, Harbin 150080
    2Safety and Quality Institute of Agricultural Products, Heilongjiang Academy of Agricultural Sciences, Harbin 150086
    3Beet Quality Supervision, Inspection and Test Center, Ministry of Agriculture and Rural Affairs, Harbin 150080
    4Laboratory of Quality Safety Risk Assessment for Sugar Crops Products, Ministry of Agriculture and Rural Affairs, Harbin 150080
  • Received:2022-04-13 Revised:2022-07-27 Online:2022-12-25 Published:2023-01-17

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摘要：

为了监测水稻中氯虫苯甲酰胺和噻虫胺的残留量，本文建立了分散固相萃取的QuEChERS法结合超高效液相色谱串联质(UPLC-MS/MS)同时测定糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺残留量的测定方法。样品经乙腈水振荡提取，PSA或C18净化，UPLC-MS/MS多反应离子监测模式(MRM)下检测，外标法定量。结果表明：氯虫苯甲酰胺和噻虫胺最佳提取溶剂为50%乙腈水，提取方式为振荡提取，选择C18作为糙米提取液的净化剂，PSA作为稻壳和秸秆提取溶剂的净化剂。氯虫苯甲酰胺在0.1~100 μg/L、噻虫胺胺在0.1~500 μg/L范围内线性关系良好，相关系数R2均大于0.99；两种农药在糙米、稻壳和秸秆中的平均添加回收率在83.2%~105.4%之间，相对标准偏差为1.2%~10.1%；氯虫苯甲酰胺和噻虫胺在糙米中定量限为0.005 mg/kg，在稻壳和秸秆中均为0.025 mg/kg。该方法前处理过程操作简单快速，灵敏度高，适用于同时检测糙米、稻壳、秸秆中氯虫苯甲酰胺和噻虫胺的残留量。

关键词: 氯虫苯甲酰胺, 噻虫胺, 分散固相萃取, 高效液相色谱-串联质谱, 水稻

Abstract:

To monitor chlorantraniliprole and clothianidin residues in rice, a QuEChERS method based on dispersive solid-phase extraction combined with ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was established for the simultaneous determination of chlorantraniliprole and clothianidin residues in brown rice, rice husk and straw. The samples were extracted by shaking with acetonitrile water solution, purified by PSA or C18, detected under UPLC-MS/MS multiple-reaction monitoring mode, and quantified by external standard method. The results showed that the best extraction solvent for chlorantraniliprole and clothianidin was 50% acetonitrile water solution, and the extraction method was shaking extraction. C18 was selected as the purifying agent for the brown rice extract, and PSA was used as the purifying agent for the extraction solvent of rice husk and straw. Good linear relations were obtained in the range of 0.1-100 μg/L for chlorantraniliprole and in the range of 0.1-500 μg/L for clothianidin, and the correlation coefficient R2 was greater than 0.99. The average recovery of the two pesticides in brown rice, rice husk and straw were between 83.2% and 105.4%, and the relative standard deviations were between 1.2% and 10.1%. The limit of quantitation of chlorantraniliprole and clothianidin in brown rice was 0.005 mg/kg, and the limit of quantitation in rice husk and straw were 0.025 mg/kg. The pretreatment process of the method is simple, rapid and highly sensitive. The method is suitable for the simultaneous detection of chlorantraniliprole and clothianidin residues in brown rice, rice husk, and straw.

Key words: chlorantraniliprole, clothianidin, dispersive solid-phase extraction, high performance liquid chromatography-tandem mass spectrometry, rice