分散固相萃取-高效液相色谱法测定水果中克百威残留  

Determination of carbofuran residues in fruits by dispersive solid-phase extraction and high-performance liquid chromatography

作　　者：郭新颖[1] 潘少聪 孙华闽[1] 谢超[1] 戴志英[1] 张茹月 GUO Xinying;PAN Shaocong;SUN Huamin;XIE Chao;DAI Zhiying;ZHANG Ruyue(Nantong Center for Disease Control and Prevention,Nantong,Jiangsu 226001,China)

机构地区：[1]南通市疾病预防控制中心,江苏南通226001

出　　处：《医学动物防制》2024年第6期602-605,共4页Journal of Medical Pest Control

基　　金：江苏省卫生健康委科研项目(Z2023022);江苏省预防医学科研课题面上项目(Ym2023021);江苏省中医药局项目(YB2020068);南通市科技计划基础科学研究项目(JC2021076)。

摘　　要：目的建立羧基化多壁碳纳米管的固体混合净化剂分散固相萃取技术对水果中克百威农药残留检测的新方法。方法2021年6月—2022年6月将采集的样品经乙腈充分提取,无水硫酸钠和氯化钠固相盐析、羧基化多壁碳纳米管(carboxylic multi-walled carbon nanotubes,MWCNTs-COOH)和N-丙基乙二胺(N-primary secondary amine)(PSA)混合净化后,采用高效液相色谱-柱后衍生-荧光检测器检测。结果克百威在0.2~5.0mg/L范围内线性关系良好,相关系数R^(2)为0.9998。方法检出限和定量限分别为0.01mg/kg和0.03mg/kg,在0.05、0.20和0.50mg/kg低、中、高不同质量浓度加标水平下的加标回收率为90.7%~103.2%,相对标准偏差(relative standard deviation,RSD)为2.1%~4.6%。结论羧基化多壁碳纳米管分散固相萃取联合高效液相色谱-柱后衍生-荧光检测技术操作简便、快速准确,适用于水果样品中克百威的定量检测。Objective To establish a new method for the detection of carbofuran pesticide residues in fruits using solid mixed purification agent dispersion solid-phase extraction technology with carboxylated multiwalled carbon nanotubes.Methods From June 2021 to June 2022,the collected samples were fully extracted with acetonitrile,salted out by solid-phase with anhydrous sodium sulfate and sodium chloride,and purified with a mixture of carboxylated multiwalled carbon nanotubes(MWCNTs-COOH)and N-primary secondary amine(PSA),and then detected using high-performance liquid chromatography post column derivatization fluorescence detector.Results The linear relationship of carbofuran was good in the range of 0.2 to 5.0mg/L,with a correlation coefficient R^(2) of 0.9998.The detection limit and quantification limit of the method were 0.01mg/kg and 0.03mg/kg,respectively.The recovery rates ranged from 90.7%to 103.2%at different mass concentration spiking levels of 0.05,0.20,and 0.50mg/kg with the relative standard deviation(RSD)of 2.1%to 4.6%.Conclusion The carboxylated multiwalled carbon nanotube dispersive solid-phase extraction combined with high-performance liquid chromatography post column derivatization fluorescence detection technology is a simple,rapid and accurate technique for the quantitative detection of carbofuran in fruit samples.

关 键 词：羧基化多壁碳纳米管 分散固相萃取 高效液相色谱法 克百威 水果 

分 类 号：R284.1[医药卫生—中药学]