固相萃取-液相色谱串联质谱法测定蔬果中54种农药残留  

Determination of 54 pesticide residues in vegetables and fruits by solid phased extraction-liquid chromatography tandem mass spectrometry

作　　者：康超 刘凤听 龚民君 李莉莉 周昕仪 潘东进 覃弘毅 KANG Chao;LIU Fengting;GONG Minjun;LI Lili;ZHOU Xinyi;PAN Dongjin;QIN Hongyi(College of Food and Quality Engineering,Nanning University,Nanning 530200,Guangxi,China;Ninning Institute of Food and Drug Control,Nanning 530000,Guangxi,China)

机构地区：[1]南宁学院食品与质量工程学院,广西南宁530200 [2]南宁市食品药品检验所,广西南宁530000

出　　处：《粮食与油脂》2025年第4期155-162,共8页Cereals & Oils

基　　金：广西科技计划项目(2020GXNSFAA297006、2024AB33074);南宁市科技开发项目(2023001)。

摘　　要：建立了新型固相萃取法结合超高效液相色谱串联质谱法测定蔬果中54种农药残留的方法。样品采用纯乙腈提取,使用QPet-Tea小柱对样品进行净化,净化液经离心过膜后上机检测。以体积分数0.1%甲酸乙腈和体积分数0.1%甲酸水溶液为流动相,在0.3 mL/min流速下梯度洗脱,采用Agilent Eclipse plus色谱柱进行液相分离,电喷雾正离子电离(ESI^(+)),多重反应监测模式(MRM)检测,外标法定量。结果表明:54种农药残留在质量浓度1~200 ng/mL范围内线性关系良好(R^(2)>0.995),定量限为0.01 mg/kg。当以姜作为样本时,在1、5、10倍定量限水平下的回收率在61.7%~123.5%,相对标准偏差(RSD)在2.1%~9.8%。建立的方法准确、灵敏、快捷,适用于蔬果中54种农药残留的快速确证和定量分析。A new solid phase extraction method combined with ultra-high performance liquid chromatography tandem mass spectrometry was established for the determination of 54 pesticide residues in vegetables and fruits.The samples were extracted with pure acetonitrile,and purified with QPet-Tea column.After centrifugation and membrane filtration,the purified solutions were subjected to instrumental detection.The mobile phase consisted of acetonitrile with volume fraction 0.1%formic acid and aqueous solution with volume fraction 0.1%formic acid.Gradient elution was performed at a flow rate of 0.3 mL/min.Liquid phase separation was carried out using an Agilent Eclipse plus chromatographic column.Detection was performed in the positive electrospray ionization(ESI^(+))mode and multiple reaction monitoring(MRM)mode,and quantification was carried out by the external standard method.The results showed that there was a good linear relationship(R^(2)>0.995)between 54 pesticide residues in the mass concentration range of 1-200 ng/mL,with a quantification limit of 0.01 mg/kg.When using ginger as a sample,the recovery rate ranged from 61.7%to 123.5%at 1,5,and 10 times the quantification limit level,and the relative standard deviation(RSD)ranged from 2.1%to 9.8%.The method was accurate,sensitive,and rapid,and was suitable for the rapid confirmation and quantitative analysis of 54 pesticide residues in vegetables and fruits.

关 键 词：液相色谱-串联质谱法 蔬果 新型固相萃取法 农药残留 

分 类 号：TS207.53[轻工技术与工程—食品科学]