食品与发酵工业 >

2022 , Vol. 48 >Issue 15: 273 - 280

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.030990

分析与检测

QuEChERS-超高效液相色谱-串联质谱法同时检测土壤-小青菜系统中丁虫腈及其代谢物残留

  • 李晶 ,
  • 董超 ,
  • 左巍 ,
  • 安文进 ,
  • 张耀海 ,
  • 赵其阳 ,
  • 焦必宁
展开
  • 1(西南大学柑桔研究所,重庆,400712)
    2(农业农村部柑桔及苗木质量监督检验测试中心,重庆,400712)
    3(国家柑桔工程技术研究中心,重庆,400712)
第一作者:博士,副教授(李晶副教授和焦必宁研究员为共同通信作者,E-mail:lijing2018@swu.edu.cn;bining_jiao@163.com)

收稿日期: 2022-02-04

  修回日期: 2022-03-23

  网络出版日期: 2022-09-02

基金资助

中央高校基本科研业务费专项资金(SWU-KT22018);重庆市技术创新与应用发展专项面上项目(鲁渝科技协作计划项目:便携式农药残留快速检测设备在香辛料中的应用,cstc2021jscx-lyjsAX0007)

收起

The simultaneous determination of flufiprole and its metabolites in soil-pakchoi system by QuEChERS-UPLC-MS/MS

  • LI Jing ,
  • DONG Chao ,
  • ZUO Wei ,
  • AN Wenjin ,
  • ZHANG Yaohai ,
  • ZHAO Qiyang ,
  • JIAO Bining
Expand
  • 1(Citrus Research Institute, Southwest University, Chongqing 400712, China)
    2(Supervision＆Inspection＆Testing Center for Quality of Citrus Fruits＆Nursery Trees, Ministry of Agriculture and Rural Affairs, Chongqing 400712,China)
    3(National Citrus Engineering Research Center, Chongqing 400712, China)

Received date: 2022-02-04

  Revised date: 2022-03-23

  Online published: 2022-09-02

Fold

摘要

采用超高效液相色谱-串联质谱结合QuEChERS前处理技术建立了土壤-小青菜系统中的丁虫腈及其多种代谢物(丁虫腈砜、丁虫腈硫醚、丁虫腈酰胺和氟虫腈)的多残留分析方法。小青菜(根、茎和叶)和土壤样品经乙腈快速提取,多壁碳纳米管净化。丁虫腈及其代谢物采用Titank F5色谱柱(100 mm×2.1 mm,1.8 μm)分离,多反应监测模式检测,基质匹配标准曲线法定量。方法验证结果表明,在质量浓度0.5~100 μg/L,丁虫腈及其代谢物的基质匹配标准曲线的线性关系良好(r≥0.992 3);方法定量限为5 μg/kg;在不同的添加水平下,丁虫腈及其代谢物在小青菜(根、茎和叶)和土壤样品平均回收率为76%~107%,相对标准偏差为0.8%~7.6%。所建方法快速简单,适用于土壤-小青菜系统中丁虫腈及其代谢物的多残留检测分析。

关键词： 丁虫腈; 代谢物; 小青菜; 土壤; 超高效液相色谱-串联质谱

本文引用格式

李晶 , 董超 , 左巍 , 安文进 , 张耀海 , 赵其阳 , 焦必宁 . QuEChERS-超高效液相色谱-串联质谱法同时检测土壤-小青菜系统中丁虫腈及其代谢物残留[J]. 食品与发酵工业, 2022 , 48(15) : 273 -280 . DOI: 10.13995/j.cnki.11-1802/ts.030990

Abstract

A method for the analysis of flufiprole and its metabolites (flufiprole sulfone, flufiprole sulfide, flufiprole amide and fipronil) in soil-pakchoi (Brassica campestris L. ssp. chinensis) system was established using ultra-high performance liquid chromatography tandem mass spectrometry combined with QuEChERS pretreatment technology. The samples were rapidly extracted by acetonitrile and purified by multi-walled carbon nanotubes. Flufiprole and its metabolites were separated at a Titank F5 column (100×2.1 mm, 1.8 μm), detected with multiple reaction monitoring mode (MRM). Then, they were quantified with matrix matching standard curve. Excellent linear relationship of flufiprole and its metabolites in pakchoi samples (roots, stems and leaves) and soil samples were obtained in the concentration range of 0.5-100 μg/L with the correlation coefficient no less than 0.992 3. The limit of quantification (LOQ) was 5 μg/kg. The average recoveries of flufiprole and its metabolites in pakchoi samples (roots, stems and leaves) and soil samples were 76%-107%, and the relative standard deviation (RSD) was 0.8%-7.6%. The established method is suitable for the simultaneous analysis of flufiprole and its metabolites in soil-pakchoi system.

Key words： flufiprole; metabolites; pakchoi (Brassica campestris L. ssp. chinensis); soil; UPLC-MS/MS

参考文献

[1] 李彦龙. 创制杀虫剂丁虫腈[J].农药, 2014, 53(2):126-128.
LI Y L.A novel insecticide flufi prole[J].Agrochemicals, 2014, 53(2):126-128.
[2] TIAN M M, ZHANG Q, HUA X D, et al.Systemic stereoselectivity study of flufiprole:Stereoselective bioactivity, acute toxicity and environmental fate[J].Journal of Hazardous Materials, 2016, 320:487-494.
[3] 牛洪涛. 丁烯氟虫腈对小菜蛾的生物活性及抗性风险评估[D].泰安:山东农业大学, 2008.
NIU H T.Biological activities of butene-fipronil to the diamondbck moth, Plutella xylostella (L.) and its resistance risk assessment[D].Tai’an:Shandong Agricultural University, 2008.
[4] 徐士才,傅俊璋,朱磊, 等.几种药剂防治水稻稻纵卷叶螟幼虫田间药效试验报告[J].农药科学与管理,2008,29(12):23-25.
XU S C, FU J Z, ZHU L, et al.Field efficacy of several insecticides against rice leaf roller larvae[J].Pesticide Science and Administration.2008,29(12):23-25.
[5] 于建垒, 宋国春, 李瑞娟, 等.丁虫腈在甘蓝中的残留特性及安全使用[J].中国蔬菜, 2011(20):79-83.
YU J L, SONG G C, LI R J, et al.Residue studies and safe application of flufiprole in cabbage[J].China Vegetables, 2011(20):79-83.
[6] 何健, 孔德洋, 吴文铸, 等.丁虫腈在环境中的降解特性[J].生态与农村环境学报, 2012, 28(5):539-543.
HE J, KONG D Y, WU W Z, et al.Degradation of flufiprole in the environment[J].Journal of Ecology and Rural Environment, 2012, 28(5):539-543.
[7] 单正军, 陈祖义.农产品农药污染途径分析[J].农药科学与管理, 2008, 29(3):40-49;14.
SHAN Z J, CHEN Z Y.Analysis of pollution channels of agricultural products[J].Pesticide Science and Administration,2008, 29(3):40-49;14.
[8] 赵玉华, 陈子雷, 王玉涛, 等.QuEChERS结合GC-MS/MS快速检测蔬菜中丁虫腈残留[J].山东农业科学, 2016, 48(7):129-132.
ZHAO Y H, CHEN Z L, WANG Y T, et al.Rapid determination of flufiprole residue in vegetables using QuEChERS and gas chromatography-triple quadrupole mass spectrometry[J].Shandong Agricultural Sciences, 2016, 48(7):129-132.
[9] 罗智强, 章虎, 王祥云, 等.电子捕获检测器-气相色谱法测定土壤中丁虫腈农药残留量[J].理化检验-化学分册, 2014, 50(3):330-332.
LUO Z Q, ZHANG H, WANG X Y, et al.Determination of residual amount of flufiprole in soil by GC with ECD[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis), 2014, 50(3):330-332.
[10] 丁立平, 刘微, 方光伟, 等.改进QuChERS-气质联用法测定蔬菜中氟虫腈和丁烯氟虫腈残留量[J].分析试验室, 2013, 32(8):117-120.
DING L P, LIU W, FANG G W, et al.Determination of fipronil and butane-fipronil residues in vegetable by improved QuChERS-GC/MS[J].Chinese Journal of Analysis Laboratory, 2013, 32(8):117-120.
[11] GAO J, WANG F, JIANG W Q, et al.A full evaluation of chiral phenylpyrazole pesticide flufiprole and the metabolites to non-target organism in paddy field[J].Environmental Pollution, 2020, 264:114808.
[12] 何健, 孔德洋, 吴文铸, 等.稻田样品中丁虫腈及其代谢产物的残留分析方法[J].生态与农村环境学报, 2012, 28(4):451-455.
HE J, KONG D Y, WU W Z, et al.Determination of flufiprole and its metabolites in samples from paddy field[J].Journal of Ecology and Rural Environment, 2012, 28(4):451-455.
[13] 谭华东, 张汇杰, 武春媛.QuEChERS/UPLC-MS/MS法快速测定土壤中吡虫啉、啶虫脒与阿维菌素残留[J].农药, 2019, 58(1):45-49.
TAN H D, ZHANG H J, WU C Y.Rapid determination of avermectin, imidacloprid and acetamiprid residues in soil by QuEChERS/UPLC-MS/MS[J].Agrochemicals, 2019, 58(1):45-49.
[14] 田金凤, 尚远宏.QuEChERS净化-超高效液相色谱-串联质谱法测定凯特芒果中14种农药残留[J].食品与发酵工业, 2020, 46(9):272-277.
TIAN J F, SHANG Y H.Determination of fourteen kinds of pesticide residues in Kaite mango by QuEChERS with UPLC-MS/MS[J].Food and Fermentation Industries, 2020, 46(9):272-277.
[15] 范金平, 张盈, 魏进, 等.QuEChERS结合超高效液相色谱串联质谱法测定花椒中烯效唑残留量及贮藏稳定性[J].食品与发酵工业, 2021, 47(8):230-235.
FAN J P, ZHANG Y, WEI J, et al.Determination of uniconazole and storage stability in Zanthoxylum bungeanum Maxim by QuEChERS-UHPLC-MS/MS[J].Food and Fermentation Industries, 2021, 47(8):230-235.
[16] LI M M, LIU X G, DONG F S, et al.Simultaneous determination of cyflumetofen and its main metabolite residues in samples of plant and animal origin using multi-walled carbon nanotubes in dispersive solid-phase extraction and ultrahigh performance liquid chromatography-tandem mass spectrometry[J].Journal of Chromatography A, 2013, 1 300:95-103.
[17] LI J, DONG C, AN W J, et al.Simultaneous enantioselective determination of two new isopropanol-triazole fungicides in plant-origin foods using multiwalled carbon nanotubes in reversed-dispersive solid-phase extraction and ultrahigh-performance liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural and Food Chemistry, 2020, 68(21):5 969-5 979.
[18] 乐渊, 刘春华, 吴南村,等.多壁碳纳米管净化-液相色谱串联质谱法测定瓜菜中双酰胺类杀虫剂[J].食品安全质量检测学报.2019,10(10):2 961-2 966.
LE Y, LIU C H, WU N C,et al.Determination of diamide insecticide residues in melons and vegetables using multiwalled carbon nanotubes purification coupled with ultra performance liquid chromatography tandem mass spectrometry[J].Journal of Food Safety & Quality, 2019,10(10):2 961-2 966.
[19] HE Z Y, CHEN S S, WANG L, et al.Multiresidue analysis of 213 pesticides in leek and garlic using QuEChERS-based method and gas chromatography-triple quadrupole mass spectrometry[J].Analytical and Bioanalytical Chemistry, 2015, 407(9):2 637-2 643.
Options
文章导航

/

〈 〉

技术支持：北京玛格泰克科技发展有限公司