摘要
[目的]建立同时检测鲜食辣椒中啶虫脒、吡虫啉、乙草胺、噻虫嗪、毒死蜱和氯虫苯甲酰胺6种农药的QuEChERS-超高效液相色谱-串联质谱法分析方法。[方法]采用QuEChERS前处理方法,样品经2.0%乙酸乙腈提取,50 mg C_(18)和20 mg GCB净化,采用UHPLC-MS/MS检测,基质外标法定量。[结果]6种农药在质量浓度为0.01~1.00 mg/L范围内峰面积与对应的质量浓度间呈现出良好线性关系,相关系数均大于0.99;6种农药在0.01、0.1、1.0 mg/kg添加水平下的平均回收率为71%~107%,相对标准偏差为1.46%~7.79%(n=5),方法定量限均为0.01 mg/kg。[结论]该方法样品前处理简单快速,方法的精密度、准确度和灵敏度均满足农药残留在农作物中检测分析要求,适用于6种农药在鲜食辣椒中的多残留同时检测、准确定性和定量分析以及市场监督抽查等。实际样品检测显示6种农药在贵州辣椒上的使用是安全的,不会产生相关的膳食风险和危害。
[Aims]This study aims to establish a method for the simultaneous determination of acetamiprid,imidacloprid, acetochlor, thiamethoxam, chlorpyrifos and chlorantraniliprole in fresh pepper by ultra high performance liquid chromatography tandem mass spectrometry(UHPLC-MS/MS). [Methods]Based on the QuEChERS extraction technique, the samples were extracted with a mixture of 2% acetonitrile acetate, purified by dispersive solid phase extraction with 50 mg octadecylsilane(C;) and 20 mg graphitized carbon black(GCB), and detected by UHPLC-MS/MS using the external matrix standard method for quantitative analysis. [Results]In the mass concentration range of 0.01-1.00 mg/L, there was a good correlation between concentrations and peak areas of6 pesticides in the pepper with correlation coefficients higher than 0.99. In the pepper samples spiked with 0.01, 0.1 and1.0 mg/kg of 6 pesticides, their recoveries and relative standard deviations were 71 to 107% and 1.46 to 7.79%(n=5),respectively. The limits of quantification(LOQs) of all those pesticides were 0.01 mg/kg. [Conclusions]This method is simple and rapid. Its sensitivity, accuracy and precision can meet the requirements of the pesticide residue analysis.Therefore, this method can be applied to the simultaneously accurate qualitative and quantitative analysis of acetamiprid, imidacloprid, acetochlor, thiamethoxam, chlorpyrifos and chlorantraniliprole in pepper as well as market supervision and spot check. It was safety for application of the six pesticides on peppers from Guizhou when testing the real samples. It would not pose the related dietary risk and hazard.
作者
张盈
魏进
龙家寰
高迪
段婷婷
陈才俊
ZHANG Ying;WEI Jin;LONG Jia-huan;GAO Di;DUAN Ting-ting;CHEN Cai-jun(Guizhou Academy of Agricultural Sciences,Institute of Plant Protection,Guiyang 550006,China)
出处
《农药》
CAS
CSCD
北大核心
2022年第3期198-202,共5页
Agrochemicals
基金
贵州省科技支撑计划项目([2018]2353)
贵州省科研机构服务企业行动计划项目(黔科合服企[2018]4004号)。
关键词
QUECHERS
辣椒
残留
超高效液相色谱-串联质谱
农药
QuEChERS
Capsicum spp
residue
ultra performance liquid chromatography-tandem mass spectrometry
pesticide
