基于N-丙基乙二胺键合硅胶和十八烷基键合锆胶的QuEChERS-气相色谱-质谱法检测酥油中的8种有机磷农药残留  

Determination of 8 kinds of organophosphorus pesticide residues in butter by QuEChERS-gas chromatography-mass spectrometry based on primary secondary amine and C18-bonded zirconium rubber

作　　者：王军 扎西次旦 黄利英 白军平 张飞龙 代艳娜 WANG Jun;ZHAXI Ci-Dan;HUANG Li-Ying;BAI Jun-Ping;ZHANG Fei-Long;DAI Yan-Na(Institute ofAgricultural Product Quality Standard and Testing Research,Tibet Academy of Agricultural and Animal Husbandry Sciences,Lhasa 850032,China)

机构地区：[1]西藏自治区农牧科学院农业质量标准与检测研究所

出　　处：《食品安全质量检测学报》2019年第21期7360-7364,共5页Journal of Food Safety and Quality

基　　金：西藏自治区科技厅重点研发与转化项目(XZ201801NB07);西藏自治区财政预算内项目(XZNKY-2019-C-029)~~

摘　　要：目的 建立一种基于N-丙基乙二胺键合硅胶(primary secondary amine,PSA)和十八烷基键合锆胶(C18-bonded zirconium rubber,Z-sep+)为净化材料的QuEChERS-气相色谱-质谱法检测酥油中的8种有机磷农药残留的分析方法 .方法使用乙腈对样品中的农药残留进行提取,以PSA和Z-sep+为QuEChERS净化材料,对提取液中的干扰物质进行去除,净化后的样品进气相色谱-质谱联用仪检测.结果 在线性范围10~500μg/kg内,目标定量离子峰面积与相应浓度呈良好的线性关系,相关系数r>0.99,检出限(limit of detection,LODs)为1.08~7.16μg/kg,定量限(limit of quantitation,LOQs)为3.59~23.86μg/kg,以25、100和500μg/kg浓度水平添加回收率为73.6~113.1%,相对标准偏差(relative standard deviation,RSD)位于5.1~17.2%,日内精密度和日间精密度满足实验要求.结论 该方法快速、准确、灵敏,适合测定酥油中有机磷农药残留.Objective To establish a method for the determination of 8 organophosphorus pesticide residues in butter by Qu ECh ERS-gas chromatography-mass spectrometry based on PSA(primary secondary amine) and Z-sep+(C18-bonded zirconium rubber) as clean-up materials. Methods After the pesticide residues were extracted by acetonitrile, PSA and Z-sep+ were used as QuEChERS clean-up agents to remove the interfering substances in the extract, and the purified samples were detected by GC-MS. Results In the linear range of 10~500 μg/kg, the peak area of the target quantitative ion had good linear relationship with the corresponding concentration r>0.99, LODs(limit of detection) were 1.08-7.16 μg/kg, LOQs(limit of quantitation) were 3.59-23.8 μg/kg, the recoveries were 73.6-11.31% at the concentration of 25, 100 and 500 μg/kg, and the RSDs were 5.1-17.2%. The intra-day precision and inter-day precision met the experimental requirements. Conclusion This method is rapid, accurate, sensitive and suitable for the determination of organophosphorus pesticide residues in butter.

关 键 词：酥油 净化剂 气相色谱-质谱法 有机磷农药 

分 类 号：R28[医药卫生—中药学]