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中国农学通报

中国农学通报 ›› 2022, Vol. 38 ›› Issue (36): 146-151.doi: 10.11924/j.issn.1000-6850.casb2022-0147

• 食品·营养·检测·安全 • 上一篇    下一篇

LC-MS/MS测定3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留

叶倩1,2,3(), 朱富伟1,2,3, 万凯1,2,3, 黄聪灵1,2,3, 唐雪妹1,2,3()   

  1. 1广东省农业科学院农业质量标准与监测技术研究所，广州 510640
    2广东省农产品质量安全风险评估重点实验室，广州 510640
    3农业农村部农产品质量安全检测与评价重点实验室，广州 510640
  • 收稿日期:2022-03-30 修回日期:2022-06-15 出版日期:2022-12-25 发布日期:2023-01-17
  • 作者简介:

    叶倩，女，1984年出生，内蒙古人，高级实验师，硕士，研究方向：农产品质量安全。通信地址：510640 广东省广州市天河区五山金颖路20号 农业质量标准与监测技术研究所，E-mail：。

  • 基金资助:
    国家重点研发计划“食品中农药残留标准再评估研究”(2019YFC1605204); 广东省基础与应用基础研究基金项目“基于代谢组学的农药-重金属联合毒性及分子机制研究”(2020A1515010620); 公益研究与能力建设项目“广东省农产品质量安全风险评估重点实验室建设”（2019年度）(2019B121203009)

Pyraclostrobin, Acetamiprid and Pyridaben Residues in Three Composite Fruit and Vegetable Juice: Determination by LC-MS/MS

YE Qian1,2,3(), ZHU Fuwei1,2,3, WAN Kai1,2,3, HUANG Congling1,2,3, TANG Xuemei1,2,3()   

  1. 1Institute of Quality Standard and Monitoring Technology for Agro-products of Guangdong Academy of Agricultural Sciences, Guangzhou 510640
    2Laboratory of Quality and Safety Risk Assessment of Agro-product, Guangdong Province, Guangzhou 510640
    3Key Laboratory of Testing and Evaluation for Agro-product Safety and Quality, Ministry of Agriculture and Rural Affairs, Guangzhou 510640
  • Received:2022-03-30 Revised:2022-06-15 Online:2022-12-25 Published:2023-01-17

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摘要：

为了探究目前蔬果生产中常用杀菌剂、杀虫剂、杀螨剂在复合蔬果汁中的残留情况，本研究建立了3种复合蔬果汁中吡唑醚菌酯、啶虫脒和哒螨灵残留的LC-MS/MS分析方法。选取以不同蔬果进行调和的3种复合蔬果汁为材料，采用含1%(v%)乙酸的乙腈溶液提取，以SPE-NH2柱进行净化，以C18色谱柱分离待测物，采用电喷雾离子化，正离子扫描和多反应监测模式(MRM)检测，基质匹配标准溶液外标法定量。试验结果表明：啶虫脒在5~1000 μg/L，吡唑醚菌酯和哒螨灵在1~500 μg/L范围内均有良好的线性关系，相关系数(R2)在0.9984以上。添加浓度为0.010、0.10和0.50 mg/kg时，3种复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵回收率为80.6%~113.4%；相对标准偏差(RSD)介于0.5%~9.3%之间；以最低添加浓度0.010 mg/kg为方法定量限(LOQ)。该方法快捷、简便、准确，满足复合蔬果汁中吡唑醚菌酯、啶虫脒及哒螨灵残留分析的要求。

关键词: 蔬果汁, 吡唑醚菌酯, 啶虫脒, 哒螨灵, 残留

Abstract:

In order to explore the residues of fungicides, insecticides and acaricides, which are commonly used in fruit and vegetable planting, in composite fruit and vegetable juice, a method for the simultaneous detection of pyraclostrobin, acetamiprid and pyridaben in 3 kinds of composite fruit and vegetable juice by LC-MS/MS was developed. Three composite fruit and vegetable juice made by mixed vegetables and fruits were selected as the materials. The samples were initially extracted by acetonitrile containing 1% (v%) acetic acid, and cleaned up by SPE-NH2 column. The targets were separated on a C18 column, and detected by LC-MS/MS with ESI positive polarity multiple reactions monitoring (MRM) mode. The matrix-matched external standard calibration curves were used for quantitative analysis. The results showed that: good linear relationship appeared in 5-1000 μg/L of acetamiprid and 1-500 μg/L of pyraclostrobin and pyridaben. The correlation coefficients (R2) were higher than 0.9984. Under three spiked levels of 0.010, 0.10 and 0.50 mg/kg, the recovery rates ranged from 80.6% to 113.4%, and the relative standard deviations (RSD) were 0.5%-9.3%. Limit of quantification (LOQ) of pyraclostrobin, acetamiprid and pyridaben were 0.010 mg/kg, which was the lowest spiked concentration. The method can meet the requirements for the determination of pyraclostrobin, acetamiprid and pyridaben residues in composite fruit and vegetable juice simultaneously, and it is quick, efficient and accurate.

Key words: fruit and vegetable juice, pyraclostrobin, acetamiprid, pyridaben, residue