多壁碳纳米管净化-色谱质谱技术测定水芹中多农药残留  

Detection of Multiple Pesticide Residues in Oenanthe Javanica Based on Multi-Walled Carbon Nanotuebes Coupled with Chromatography-Mass Spectrometry

作　　者：王丹 万娜 黄金妮 陈敏妮 杨兹伟 汤祝华 WANG Dan;WAN Na;HUANG Jinni;CHEN Minni;YANG Ziwei;TANG Zhuhua(Hainan Institute for Food Control,Key Laboratory of Tropical Fruits and Vegetables Quality and Safety for State Market Regulation,Haikou 570311,China)

机构地区：[1]海南省食品检验检测中心,国家市场监管重点实验室(热带果蔬质量与安全),海南海口570311

出　　处：《食品科技》2023年第9期276-284,共9页Food Science and Technology

基　　金：国家市场监管重点实验室(热带果蔬质量与安全)自主研究课题(ZZ-2022017,ZZ-2023005)。

摘　　要：以多壁碳纳米管(Multi-walled carbon nanotubes,MWCNTs)为吸附材料的前处理净化方式,结合超高效液相色谱-串联质谱技术,建立一种测定水芹中常见66种农药及其代谢物残留的分析方法。样品经乙腈提取后,通过正交实验设计得到水芹样品净化的最佳实验条件,确定MWCNTs的最佳添加量,并对影响因素进行分析。结果表明:MWCNTs作为净化色素的吸附材料,能够降低前处理过程中的农药损失。在最优实验条件下,66种农药在1~100 ng/mL之间获得了良好的线性关系(R^(2)>0.991)。应用该方法对空白样品进行2、10、30μg/kg 3个不同水平浓度加标回收,66种农药平均回收率在70.4%~121.0%之间,相对标准偏差(Relative standarddeviation,RSD,n=6)低于14%,方法的定量限(Limitofquantification,LOQ)为0.0022~1.9μg/kg。结论:该方法灵敏度高、准确性好、快速简便,适用于水芹中66种农药残留量的快速测定和方法验证。The multi-walled carbon nanotubes(MWCNTs)were taken as adsorbent,and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was combined,an analytical method was developed for the determination of 66 pesticide residues in Oenanthe javanica.After extracting the samples with acetonitrile,the optimal experimental conditions for purifying samples were tested through an orthogonal experimental design to determine the optimal amount of MWCNTs added,and the influencing factors were analyzed.The results showed that MWCNTs were used as an adsorption material can reduce pesticide losses during the pre-treatment process.Under the optimum conditions,66 pesticides obtained satisfactory linearity for analytes in the concentration range of 1–100 ng/mL(R^(2)>0.991).The standard addition tests at three levels of 2μg/kg,10μg/kg and 30μg/kg were conducted in Oenanthe javanica blank matrix,and the recoveries were 70.4%to 121.0%,with relative standard deviation(RSD)less than 14%,and the limit of quantification(LOQ)of the method was 0.0022μg/kg to 1.9μg/kg.Conclusion:the method is sensitive,accurate,rapid and simple,and suitable for the rapid determination and method validation of 66 pesticide residues in Oenanthe javanica.

关 键 词：水芹 多壁碳纳米管 超高效液相色谱-串联质谱法 农药残留 

分 类 号：TS207.53[轻工技术与工程—食品科学]