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中国农学通报

中国农学通报 ›› 2024, Vol. 40 ›› Issue (13): 129-139.doi: 10.11924/j.issn.1000-6850.casb2023-0421

• 植物保护·农药 • 上一篇    下一篇

荔枝中20种登记农药残留分析方法研究

王思威1(), 刘艳萍1, 张树飞2(), 张惠云3, 何强4(), 王潇楠1, 常虹1   

  1. 1 广东省农业科学院植物保护研究所/农业农村部华南果蔬绿色防控重点实验室/广东省植物保护新技术重点实验室，广州 510640
    2 深圳职业技术大学食品药品学院，深圳 518000
    3 云南省农业科学院热带亚热带经济作物研究所，云南保山 678000
    4 广东省农产品质量安全中心，广州 525000
  • 收稿日期:2023-05-31 修回日期:2023-12-27 出版日期:2024-04-28 发布日期:2024-04-28
  • 通讯作者:
    张树飞，女，1981年出生，江苏连云港人，高级农艺师，硕士，主要从事农药应用与示范推广工作。通信地址：518000 广东省深圳市南山区留仙大道7098号 深圳职业技术大学，Tel：0755-26019091，E-mail：。
    何强，男，1975年出生，广东河源人，正高级农艺师，硕士，主要从事农产品质量安全研究工作。通信地址：510500 广东省广州市天河区先烈东路135号 广东省农产品质量安全中心，Tel：020-37288071，E-mail：。
  • 作者简介:

    王思威，女，1984年出生，黑龙江望奎人，副研究员，博士，主要从事农药残留研究。通信地址：510640 广东省广州市天河区金颖路7号 广东省农业科学院植物保护研究所，Tel：020-87597590，E-mail：。

  • 基金资助:
    国家现代农业产业技术体系项目“荔枝龙眼产业技术体系”(CARS-32); 乡村振兴战略专项资金(农业科技能力提升); 乡村振兴战略专项资金(2023TS-2-3); 广州市科技计划项目“植保无人机旋翼分场下纳米农药雾滴与荔枝叶片交互作用机理与调控研究”(202201010479); 广州市科技计划项目“性信息素受体调控荔枝蒂蛀虫识别性信息素的分子机制”(2023A04J0805); 广东省基础和应用基础研究基金“气味综合蛋白在荔枝蒂蛀虫识别性信息素行为中的功能研究”(2022A1515110473)

Determination of Residues of Twenty Registered Pesticides in Lychee

WANG Siwei1(), LIU Yanping1, ZHANG Shufei2(), ZHANG Huiyun3, HE Qiang4(), WANG Xiaonan1, CHANG Hong1   

  1. 1 Plant Protection Research Institute, Guangdong Academy of Agricultural Sciences/Key Laboratory of Green Prevention and Control on Fruits and Vegetables in South China, Ministry of Agriculture and Rural Affairs/Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Guangzhou 510640
    2 School of Food and Drug, Shenzhen Polytechnic University, Shenzhen 518000
    3 Institute of Tropical and Subtropical Cash Crops, Yunnan Academy of Agricultural Sciences, Baoshan, Yunnan 678000
    4 Guangdong Quality Safety Center of Agricultural Products, Guangzhou 510500
  • Received:2023-05-31 Revised:2023-12-27 Published:2024-04-28 Online:2024-04-28

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摘要：

为解决荔枝中20种登记农药多残留的同时快速检测问题，建立并优化基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测荔枝中7种杀虫剂和13种杀菌剂的分析方法。荔枝全果样品经80%乙腈水溶液提取后，用石墨化碳黑(GCB)净化，流动相为乙腈和水，梯度洗脱，采用Extend C18色谱柱进行分离。电喷雾正负离子交替模式采集，多反应监测(MRM)，外标法定量。20种供试农药的质量浓度与其对应的峰面积之间呈现良好线性关系，相关系数均大于0.9990；20种农药在荔枝基质中的平均回收率为71%~106%，相对标准偏差(RSD)在0.9%~9.8%之间，满足残留分析的要求。该方法简便、高效，可用于荔枝样品中20种农药残留的快速检测。

关键词: 超高效液相色谱-串联质谱, 荔枝, 杀虫剂, 杀菌剂, 残留

Abstract:

The paper aims to solve the problem of simultaneous and rapid detection of 20 registered pesticide residues in lychee. An analytical method based on ultra-high performance liquid chromatography-tandem mass spectrometry was established and optimized for simultaneous determination of 7 insecticides and 13 fungicides in lychee. The whole lychee fruit were extracted with 80% acetonitrile aqueous solution and cleaned up with graphitized carbon black (GCB). Extend C18 chromatographic column was used for separation and the mobile phase was acetonitrile and water by gradient elution. Electrospray ionization in positive and negative ion mode was selected, the detection mode was multi-reaction monitoring, and external standard method was used for quantification. The results showed that a good linear relationship was presented between the mass concentration and peak area of the twenty tested pesticides, and the determination coefficient was greater than 0.9990. The average recoveries of the twenty pesticides in lychee were in range of 71%-106% with the relative standard deviations (RSD) of 0.9%-9.8%, which met the requirements of residue analysis. The results demonstrated that the proposed method was convenient and effective for the quick determination of these twenty pesticides residues in lychee.

Key words: ultra-high performance liquid chromatography-tandem mass spectrometry, lychee, insecticide, fungicide, residue