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食品与发酵工业  2022, Vol. 48 Issue (15): 273-280    DOI: 10.13995/j.cnki.11-1802/ts.030990
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
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1,2,3*, 董超1,2,3, 左巍1,2,3, 安文进1,2,3, 张耀海1,2,3, 赵其阳1,2,3, 焦必宁1,2,3*
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)
The simultaneous determination of flufiprole and its metabolites in soil-pakchoi system by QuEChERS-UPLC-MS/MS
LI Jing1,2,3*, DONG Chao1,2,3, ZUO Wei1,2,3, AN Wenjin1,2,3, ZHANG Yaohai1,2,3, ZHAO Qiyang1,2,3, JIAO Bining1,2,3*
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)
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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。
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李晶
董超
左巍
安文进
张耀海
赵其阳
焦必宁
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    
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
收稿日期:  2022-02-04      修回日期:  2022-03-23           出版日期:  2022-08-15      发布日期:  2022-09-02      期的出版日期:  2022-08-15
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)
作者简介:  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)
引用本文:    
李晶,董超,左巍,等. 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.
LI Jing,DONG Chao,ZUO Wei,et al. The simultaneous determination of flufiprole and its metabolites in soil-pakchoi system by QuEChERS-UPLC-MS/MS[J]. Food and Fermentation Industries, 2022, 48(15): 273-280.
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http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.030990  或          http://sf1970.cnif.cn/CN/Y2022/V48/I15/273
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