QuEChERS-HPLC-MS/MS法同时测定水果中38 种农药的残留量

doi:10.7506/spkx1002-6630-20191018-199

食品科学 ›› 2020, Vol. 41 ›› Issue (8): 288-296.doi: 10.7506/spkx1002-6630-20191018-199

QuEChERS-HPLC-MS/MS法同时测定水果中38 种农药的残留量

梁秀美，张维一，张微，谢拾冰，何如意，徐静，苏来金，孙博伦，张井

（1.温州市农业科学研究院，农业农村部农产品质量安全风险评估实验站，温州市特色食品资源工程技术研究中心，浙江温州 325006；2.舟山市食品药品检验检测研究院，浙江舟山 316000；3.宁波大学食品与药学学院，浙江宁波 315000）

出版日期:2020-04-25 发布日期:2020-04-20
基金资助:
浙江省科技厅公益性项目（2017C37087）

Simultaneous Determination of Residues of 38 Pesticides in Fruits by QuEChERS Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

LIANG Xiumei, ZHANG Weiyi, ZHANG Wei, XIE Shibing, HE Ruyi, XU Jing, SU Laijin, SUN Bolun, ZHANG Jing

(1. Experimental Station of Agricultural Products Quality Safety Risk Assessment, Ministry of Agriculture and Rural Affairs, Wenzhou Research Center of Characteristic Food Resources Engineering and Technology, Wenzhou Academy of Agricultural Sciences, Wenzhou 325006, China; 2. Zhoushan Institute for Food and Drug Control, Zhoushan 316000, China;3. College of Food and Pharmaceutical Sciences, Ningbo University, Ningbo 315000, China)

Online:2020-04-25 Published:2020-04-20

摘要/Abstract

摘要： 建立水果中38 种农药残留量的测定方法。样品经粉碎后，用1%甲酸-乙腈溶液快速提取，无水硫酸镁除水后，经C18、N-丙基乙二胺和硅藻土填料净化，用高效液相色谱-串联质谱仪分析。采用Accucore aQ柱进行分离，电喷雾正离子多反应监测模式检测，外标法定量。经方法验证，38 种农药的方法检出限在0.3～26.2 μg/kg之间，定量限在0.6～52.4 μg/kg之间，线性相关系数（R）在0.999 5～0.999 9之间；本方法选择3 个浓度水平进行添加回收实验（n=6），平均加标回收率在70.1%～119.3%之间，相对标准偏差在2.7%～12.4%之间。该方法前处理快速、灵敏、准确，可为水果中农药的监管提供技术支持。

关键词: 水果, QuEChERS, 高效液相色谱-串联质谱, 农药残留

Abstract: A method for the determination of the residues of 38 pesticides in fruits was established. After being ground, the pesticide residues in samples were extracted with 1% acetic acid-acetonitril and dehydrated with anhydrous magnesium sulfate. Then, the pesticide residues in the supernatant were cleaned up with octadecylsilane (C18), primary secondary amine (PSA) and diatomite before being subjected to high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) analysis. The separation was performed on an Accucore aQ column. The electrospray ionization mass spectrometry was operated in the positive mode using multiple reaction monitoring (MRM) and the analytes were quantified by the external standard method. The results indicated that the limits of detection (LODs) for all the pesticides were in the range of 0.3–26.2 μg/kg, and the limits of quantitation (LOQs) ranged from 0.6 to 52.4 μg/kg. The correlation coefficients (R) of the calibration curves were in the range of 0.999 5–0.999 9. The average recoveries at three spiked levels ranged from 70.1% to 119.3% (n = 6) with relative standard deviations (RSDs) of 2.7%–12.4%. The method was rapid, sensitive and precise, and could provide technical support for the determination of pesticide residues in fruits.

Key words: fruits, QuEChERS, high performance liquid chromatography-mass spectrometry, pesticide residues

中图分类号:

TS255

梁秀美，张维一，张微，谢拾冰，何如意，徐静，苏来金，孙博伦，张井. QuEChERS-HPLC-MS/MS法同时测定水果中38 种农药的残留量[J]. 食品科学, 2020, 41(8): 288-296.

LIANG Xiumei, ZHANG Weiyi, ZHANG Wei, XIE Shibing, HE Ruyi, XU Jing, SU Laijin, SUN Bolun, ZHANG Jing. Simultaneous Determination of Residues of 38 Pesticides in Fruits by QuEChERS Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. FOOD SCIENCE, 2020, 41(8): 288-296.

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QuEChERS-HPLC-MS/MS法同时测定水果中38 种农药的残留量

Simultaneous Determination of Residues of 38 Pesticides in Fruits by QuEChERS Combined with High Performance Liquid Chromatography-Tandem Mass Spectrometry

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