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食品研究与开发:2017,38(20):130-134
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UPLC-MS/MS测定动物源食品中4种农药残留
韩丙军1,黄海珠1,何燕1,林冰1,陈丽霞2,*
(1.中国热带农业科学院分析测试中心,海南省热带果蔬产品质量安全重点实验室,海南海口571101;2.琼台师范学院数理系,海南海口571100)
Determination of Four Pesticides Residues in Food Products of Animal Origin Using Ultra-high Performance Liquid Chromatography Tandem Mass Spectrometry
HAN Bing-jun1,HUANG Hai-zhu1,HE Yan1,LIN Bing1,CHEN Li-xia2,*
(1.Analysis&Testing Center,Chinese Academy of Tropical Agricultural Sciences,Hainan Provincial Key Laboratory of Quality and Safety for Tropical Fruits and Vegetables,Haikou 571101,Hainan,China;2.Mathematical Department,Qiongtai Teachers College,Haikou 571100,Hainan,China)
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投稿时间:2017-03-02    
中文摘要: 建立一种超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定动物源食品中的4种新型农药氯虫苯甲酰胺、螺螨酯、联苯三唑醇和噻菌灵残留的方法。样品通过乙腈提取,采用改进的QuEChERS方法进行净化,经C18超高效液相柱分离后,使用电喷雾正离子(ESI+)模式电离,多反应离子监测模式定性分析,基质匹配标准曲线外标法定量。结果表明,氯虫苯甲酰胺、螺螨酯、联苯三唑醇和噻菌灵的定量限(10倍信噪比)分别为0.30、3.00、0.50、0.10 μg/kg;在0.005 mg/L~0.200 mg/L浓度范围内,4种农药的线性相关系数均大于0.999;在0.005、0.050、0.200 mg/kg添加水平范围内,牛奶、猪肉、猪肝和鸡蛋样品的平均添加回收率在82%~109%之间,相对标准偏差在2.1%~8.5%之间(n=5)。该方法简单、快速,灵敏度及准确度高,能够满足动物源食品中4种农药残留量的检测要求。
Abstract:To determine the residues of chlorantraniliprole,spirodiclofen,bitertanol and thiabendazole in food products of animal origin,a method was established by using ultra-high performance liquid chromatographytandem mass spectrometry.With acetonitrile as the extraction solvent,a modified QuEChERS method was chosen to purified the analytes from the food sample.The target compounds were separated by a C18 UPLC column,then detected by electro-spray ionization(ESI+)and multiple reaction monitoring(MRM)mode.Quantification was performed by peak area external standard methods using matrix-matched calibration curves,which were linear in the range of 0.005 mg/L-0.200 mg/L with good linear relationships.The correlation coefficients were better than 0.999.The limit of quantification (LOQ)of chlorantraniliprole,spirodiclofen,bitertanol and thiabendazole was 0.30,3.00,0.50,0.10 μg/kg respectively.At 0.005,0.050 ,0.200 mg/kg spiked levels for milk,pork,liver and egg samples,the recoveries were between 82%and 109%,and the relative standard deviations(RSD)were in range of 2.1%to 8.5%(n=5).This method was simple,quick,accurate,and could be applied to the determination of the four pesticides residues in food products of animal origin.
文章编号:201720027     中图分类号:    文献标志码:
基金项目:海南省应用技术研发与示范推广专项(ZDXM2015044);海南自然科学基金面上项目(20163078);海南省高等学校科学研究项目(Hnky2016ZD-14);中国热带农业科学院基本科研业务费专项资金(1630082017005)
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