QuEChERS-高效液相色谱-串联四极杆/静电场轨道阱高分辨质谱法同时测定水产品中62种农药残留  

Simultaneous determination of 62 kinds of pesticides in aquatic products by QuEChERS-high-performance liquid chromatography coupled with quadrupole/orbitrap high resolution mass spectrometry

作　　者：张梅超 王秀丽 周宏霞 ZHANG Mei-Chao;WANG Xiu-Li;ZHOU Hong-Xia(Weihai Institute for Food and Drug Control,Weihai 264200,China;Weihai Key Laboratory of Food and Drug Quality Evaluation and Technical Research,Weihai 264200,China)

机构地区：[1]威海市食品药品检验检测研究院,威海264200 [2]威海市食品药品质量评价与技术研究重点实验室,威海264200

出　　处：《食品安全质量检测学报》2024年第17期83-91,共9页Journal of Food Safety and Quality

摘　　要：目的建立QuEChERS结合高效液相色谱-串联四极杆/静电场轨道阱高分辨质谱法(high performance liquid chromatography coupled with quadrupole/orbitrap high-resolution mass spectrometry,HPLC/Q-Orbitrap HRMS)快速测定水产品中甲胺磷、毒死蜱、三唑酮、西马津和溴氰菊酯等62种农药残留量的方法。方法样品采用1%甲酸乙腈/水溶液提取,300 mg N-丙基乙二胺(primary secondary amine,PSA)和C18分散吸附剂进行净化,上清液氮吹浓缩后结合HPLC/Q-Orbitrap HRMS进行定性定量测定。结果62种农药在一定质量浓度范围内呈良好的线性关系,相关系数r^(2)均大于0.99(甲基毒死蜱除外),方法定量限(limit of quantification,LOQ)为2~10μg/kg之间。在大菱鲆、南美白对虾、扇贝3种基质中,分别进行1倍LOQ、2倍LOQ和10倍LOQ3个水平的加标试验,62种农药化合物3种添加水平回收率分别为61.4%~112.4%、63.7%~119.6%、66.2%~113.5%,相对标准偏差分别为2.1%~16.5%、2.6%~13.4%以及2.7%~15.2%。基质效应评价实验中,大菱鲆相对于南美白对虾和扇贝有更强的基质效应,其中51.2%化合物表现出弱基质效应,46.8%化合物为基质抑制效应。利用该方法对当地市场中30批样品进行农药残留的检测,结果发现共有5批大菱鲆样品和2批南美白对虾中检测出农药残留化合物。主要是除草剂和杀虫杀菌剂等,例如西马津、扑草净、毒死蜱、溴氰菊酯和毒草胺等。通过定量分析,各化合物浓度均低于国内外相关标准限量。结论该研究可以快速、准确地检测鱼肉产品中的农药残留化合物,为食品安全监测提供了有力的技术支持。Objective To establish a method for rapid determination of 62 kinds of pesticide residues such as methamidophos,chlorpyrifos,triazolone,simazine and deltamethrin in aquatic products by QuEChERS high performance liquid chromatography coupled with quadrupole/orbitrap method high resolution mass spectrometry,HPLC/Q-Orbitrap HRMS).Methods The samples were extracted by 1%acidified acetonitrile/water,cleaned-up by 300 mg primary secondary amine(PSA)and C18.The supernatant was concentrated using nitrogen and qualitatively and quantitatively determined by HPLC/Q-Orbitrap HRMS.Results The 62 kinds of pesticides showed a good linear relationship in a certain concentration range from 1 to 200.0μg/L.Except for chlorpyrifos-methyl,the correlation coefficient r^(2) was greater than 0.99.The limit of quantification(LOQ)ranged from 2 to 10μg/kg.In the turbot,shrimp and scallop,spiking experiments were performed at 3 levels:1 LOQ,2 LOQ,and 10 LOQ.The recovery rates ranged from 61.4%-112.4%,63.7%-119.6%,66.2%-113.5%,respectively,while the relative standard deviation values ranging from 2.1%-16.5%,2.6%-13.4%and 2.7%-15.2%,respectively.In the matrix effect evaluation experiment,51.2%of the compounds in turbot showed weak matrix effects,while 46.8%exhibited matrix suppression effects.Compared to shrimp and scallop,turbot exhibited a stronger matrix effect.The method was used to determine 30 samples from local market.The results showed that there were 5 turbots and 2 scallops that had pesticide residue compounds detected,mainly herbicides,insecticides,fungicides,etc.,such as simazine,prometryn,chlorpyrifos,deltamethrin and propachlor.Through quantitative analysis,the concentration of each compound was lower than the relevant standard limits both domestically and internationally.Conclusions This study provides an effective method for rapid and accurate detection of pesticide residues in fish products,offering strong technical support for food safety monitoring.

关 键 词：高效液相色谱-串联四极杆/静电场轨道阱高分辨质谱法 QUECHERS 农药 水产品 

分 类 号：O657.63[理学—分析化学] TS254.7[理学—化学]