Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources

HUANG Jiang-peng; SUN Wen-wen; CHEN Shao-min; CHEN Hui-bing; WU Hai-jun

doi:10.12452/j.fxcsxb.241108517

您当前的位置：

首页 >

文章列表页 >

Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources

Experimental Techniques and Methods | 更新时间：2025-02-12

- Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources
- Journal of Instrumental Analysis Vol. 44, Issue 2, Pages: 342-348(2025)
- 作者机构：
  
  1.广州市花都区农业技术管理中心，广东广州 510800
  2.上海爱博才思分析仪器贸易有限公司，广东广州 510320
  3.广州海关技术中心，广东广州 510000
  4.广州南沙明曦检测服务有限公司，广东广州 511464
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.241108517
  CLC： O657.7;TS207.3
- Published：15 February 2025，
  
  Received：08 November 2024，
  
  Revised：09 December 2024，
  
  Accepted：2024-12-13
- 稿件说明：
移动端阅览
黄江鹏,孙雯雯,陈少敏,陈慧冰,吴海军.液相色谱-质谱法测定蔬菜中氟虫腈及代谢物残留与氟虫腈砜的来源探究[J].分析测试学报,2025,44(02):342-348.

HUANG Jiang-peng,SUN Wen-wen,CHEN Shao-min,CHEN Hui-bing,WU Hai-jun.Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources[J].Journal of Instrumental Analysis,2025,44(02):342-348.
黄江鹏,孙雯雯,陈少敏,陈慧冰,吴海军.液相色谱-质谱法测定蔬菜中氟虫腈及代谢物残留与氟虫腈砜的来源探究[J].分析测试学报,2025,44(02):342-348. DOI： 10.12452/j.fxcsxb.241108517.

HUANG Jiang-peng,SUN Wen-wen,CHEN Shao-min,CHEN Hui-bing,WU Hai-jun.Determination of Fipronil and Its Metabolites in Vegetables by Liquid Chromatography-Tandem Mass Spectrometry and the Investigation of Fipronil Sulfone Sources[J].Journal of Instrumental Analysis,2025,44(02):342-348. DOI： 10.12452/j.fxcsxb.241108517.

摘要

建立了液相色谱-串联质谱同时测定蔬菜中氟虫腈及代谢物氟甲腈、氟虫腈砜、氟虫腈硫醚残留的方法。样品经乙腈提取后稀释，过微孔滤膜后，在多反应监测模式下进行检测。结果表明：4种目标组分的线性范围为1~100 μg/L，相关系数均大于0.998，回收率为96.0%~117%，相对标准偏差为1.7%~5.3%，定量下限为0.005 mg/kg。该方法操作简便，回收率和重复性良好。使用该方法测定抽样蔬菜样品，检出氟虫腈砜残留，但未检出氟虫腈。针对检测出的氟虫腈砜进行了深入调查和来源研究，采用气相色谱-质谱法测定农户施用的农药，发现农药中添加氟虫腈砜。

Abstract

A method was established for the determination of fipronil and its metabolites fipronil desulfinyl，fipronil sulfone and fipronil sulfide in vegetables by liquid chromatography-tandem mass spectrometry. The sample was extracted with acetonitrile and diluted，then filtered through millipore filter and multiple reaction monitoring（MRM） mode was selected for the determination. The results showed that the linear range for four analytes was 1-100 μg/L，with the correlation coefficients（

） larger than 0.998. The limit of quantification was 0.005 mg/kg. The recoveries were ranged from 96.0% to 117%，and the relative standard deviations（RSDs） were between 1.7%-5.3%. This method proves to be simple，fast and accurate，and has relative better recoveries and repeatability. Fipronil sulfone was detected in the market sampling vegetable samples，while fipronil was not detected. In-depth investigation and source research on the detected fipronil sulfone was conducted by gas chromatography-mass spectrometry method，and the results showed that fipronil sulfone was found to be added in pesticides.

关键词

液相色谱-串联质谱法气相色谱-质谱法蔬菜农药残留氟虫腈及代谢物

Keywords

liquid chromatography-tandem mass spectrometrygas chromatography-mass spectrometryvegetablespesticide residuesfipronil and its metabolites

references

Li Q W，Zhang W L. Proceedings of the 9th National Pesticide Exchange Conference（李庆文，张伟莉. 第九届全国农药交流会论文集），2009：243-248.

Ministry of Agriculture．Announcement of the Ministry of Agriculture of the People’s Republic of China No. 1157（农业部. 中华人民共和国农业部公告第1157号）.［2024-11-12］. http：//www.moa.gov.cn/zwllm/tzgg/gg/200902/t20090227_1226994.htmhttp://www.moa.gov.cn/zwllm/tzgg/gg/200902/t20090227_1226994.htm.

GB 23200.121-2021. National Food Safety Standard—Determination of 331 Pesticides and Metabolites Residues in Foods of Plant Origin—Liquid Chromatography-Tandem Mass Spectrometry Method. National Standards of the People's Republic of China（食品安全国家标准植物源性食品中331种农药及其代谢物残留量的测定液相色谱-质谱联用法. 中华人民共和国国家标准）.

NY/T 2990-2016. Qualitative and Quantitative Determination for Banned and Restricted Pesticides. Agricultural Industry Standards of the People's Republic of China （禁限用农药定性定量分析方法. 中华人民共和国农业行业标准）.

NY/T 4119-2022. General Methods for Determination of Active Ingredient Content of Pesticides-High Performance Liquid Chromatography（HPLC）. Agricultural Industry Standards of the People's Republic of China （农药产品中有效成分含量测定通用分析方法高效液相色谱法.中华人民共和国农业行业标准）.

Guangdong Administration for Market Regulation. Ability Parameter Apply（广东省市场监督管理局.已有项目参数查询）.［2024-11-12］. https：//amr.gd.gov.cn/xksp/pub_platform/#/abilityParameterApplyhttps://amr.gd.gov.cn/xksp/pub_platform/#/abilityParameterApply.

Lin T，Peng L Y，Chen X L，Liu X Y，Li M X，Xu Y R，Zou Y H，Liu H C. Sci. Technol. Food Ind.（林涛，彭丽媛，陈兴连，刘兴勇，李茂萱，徐祎然，邹艳虹，刘宏程. 食品科技），2020，41（21）：218-223.

Dai J F，Huang Y X，Chen H J，Li Z，Xu Y Y，Shi P T，Jiang Q Q，Li S J，Liu K L. Agrochemicals（戴金凤，黄宇翔，陈红军，李政，许银玉，石鹏途，蒋青青，李双佳，刘开林. 农药），2024，63（8）： 592-597，603.

Liu L，Mao Z，Cui Q Q，Zhu X X，Jia S T，Zhao L P. Mod. Food（刘璐，毛震，崔倩倩，朱欣欣，贾松涛，赵林萍.现代食品），2024，30（3）： 182-185.

Guo H B，Peng K L，Wu J L，Yang S X，Lin L，Ye J Z，Liu Y J，Wang X F. Food Res. Dev. （郭宏斌，彭侃霖，吴金玲，杨舒娴，林玲，叶剑芝，刘元靖，王晓芳. 食品研究与开发），2024，45（4）： 158-163.

Zhou T，Xiao H X，Zhou Z J. J. Environ. Occup. Med. （周彤，肖洪喜，周志俊.环境与职业医学），2017，34（ 8）： 745－748.

Wang X Y，Zhang C，Liu Y J，Chen L，You J J，Gao H R，Cheng L. Res. Qual. Tech. Superv. 王秀云，张聪，刘亿婕，陈亮，游菁菁，高海荣，程琳.质量技术监督研究），2020，（5）：10-14，20.

Zhou Y C，Teng Y J，Wang S L，Liu H，Li Q L，Xie W D，Sun Y N，Huang H. Mod. Food（周玉春，滕玉娇，王少龙，刘慧，李其亮，谢文东，孙娅娜，黄华. 现代食品），2021，（6）：194-198.

Wang H M. Mod. Food（王红梅. 现代食品），2021，（21）：205-208.

Gao X，Chen H，Tan M，Li Y X，He H L. Food Sci.（高霞，陈辉，谭敏，李玉秀，何泓霖.食品科学），2021，42（14）：333-338.

Cao H H，Wang S，Zhao H T，Wang Y J，Zhang L，Zhang H F，Liu H H，Zhou Y C，Tang S N，Yan Y H. Mod. Food Sci. Technol.（曹慧慧，王帅，赵海涛，王雅静，张亮，张贺凤，刘会会，周彦成，汤思凝，闫艳华.现代食品科技），2022，38（1）：336-344.

Ma Y Y，Hao Y，Zhang P，Liu M M，Yu Y，Sun X Y，Yu L T. Food Sci.（马艺荧，郝宇，张鹏，刘萌萌，于洋，孙欣瑶，于力涛.食品科学），2023，44（2）：351-356.

Li M Q，An W J，Li J，Wang L，Zhuang J，He M L. J. Instrum. Anal.（李敏青，安文佳，李菊，王岚，庄嘉，何曼莉.分析测试学报），2020，39（4）：520-525.

Du X，He J G，Yi S S，Chen S H. Pestic. Sci. Adm. （杜鑫，何家国，易珊珊，陈绍辉.农药科学与管理），2023，44（11）：35-44.

Zhong M X，Ma E Y，Zhou J S，Wu Z B，Lu B L. Agric. Technol. （钟满霞，马恩耀，周劲松，吴志彬，卢柏林.农业与技术），2024，44 （17）： 37-41.

GB 2763-2021. National Food Safety Standard—Maximum Residue Limits for Pesticides in Food. National Standards of the People's Republic of China（食品安全国家标准食品中农药最大残留限量. 中华人民共和国国家标准）.

Fang L，Lin C，Wang L P，Zhang F Y，Lin Z P，Li X Y，Pan Y S. J. Anhui Agric. Sci.（方丽，林晨，王李平，张方圆，林泽鹏，李雪莹，潘云山. 安徽农业科学），2020，48（17）：206-209.

Wang Y L，Chen K Y，Liang X Q，Zhang H X，Hu M，Liu Y M，Zhu J H. J. Instrum. Anal.（王艳丽，陈克云，梁秀清，张红霞，胡梅，刘艳明，祝建华. 分析测试学报），2018，37（4）：440-445.

Tang R Y，Zhong P，Lin Q L. J. Fluorine Chem.，2006，127（7）：948-953.

Shandong Jingbo Agrochemical Technology Co.，Ltd. China Patent （山东京博农化科技股份有限公司. 中国专利），202310171800.9. ［2023-05-12］.

Wang F，Meng X H，Wang H. Hans J. Agric. Sci.（王峰，孟祥鹤，王菡. 农业科学），2014，4（5）：99-104.

Wang A E. Beijing Agric. （王爱娥. 北京农业），2006，（4）：3-39.

Xu G C，Gu Z Y，Yang Y Q，Xu D J ，Xu X L，Shi W S. Mod. Agrochem. （徐广春，顾中言，杨玉清，徐德进，许小龙，石伟山. 现代农药），2008，7（2）：1-5，11.

Ministry of Agriculture and Rural Affairs.Pesticide Registration Information （农业农村部. 农药登记信息）. ［2024-11-12］. http：//www.chinapesticide.org.cn/zgnyxxw/zwb/detail/29353http://www.chinapesticide.org.cn/zgnyxxw/zwb/detail/29353.

Ministry of Health. List of Non-edible Substances that May Be Illegally Added to Food and Food Additives that are Easily Abused （Consolidated Batches 1-5）（卫生部. 食品中可能违法添加的非食用物质和易滥用的食品添加剂名单（第1-5批汇总））. ［2024-11-12］. https：//www.sdtdata.com/fx/fcv1/tsLibCard.doViewhttps://www.sdtdata.com/fx/fcv1/tsLibCard.doView.

Ministry of Health. Ministry of Health of the People's Republic of China Announcement No. 16 of 2011（卫生部. 中华人民共和国卫生部公告2011年第16号）. ［2024-11-12］. https：//www.sdtdata.com/fx/fcv1/tsLibCard.doViewhttps://www.sdtdata.com/fx/fcv1/tsLibCard.doView.

Ministry of Agriculture and Rural Affairs. List of Prohibited and Restricted Pesticides（农业农村部. 禁限用农药名录）.［2024-11-12］. http：//www.zzys.moa.gov.cn/gzdt/201911/t20191129_6332604.htmhttp://www.zzys.moa.gov.cn/gzdt/201911/t20191129_6332604.htm.

Views

下载量

CSCD

Alert me when the article has been cited

提交

Tools

Publicity Resources

Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography－High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid－Liquid Extraction

Simultaneous Determination of Nine Pesticide Residues in Vegetables,Fruit and Edible Fungi by Reverse Phase High Performance Liquid Chromatography

Determination of 67 Pesticide Residues in Vegetables and Fruits by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Dispersive Solid Phase Extraction

MIL-101@MF Composite Material Pipette-tip Efficient Solid-phase Extraction of Chloramphenicols Residues in Eggs

Related Author

CHEN Hui-bing

BI Jun

REN Jun

ZHAO Yun-feng

CHEN Da-wei

骆冲

万凯

丁晨红

Related Institution

Guangzhou Nansha Mingxi Detection Service Co.，Ltd.

NHC Key Laboratory of Food Safety Risk Assessment， China National Center for Food Safety Risk Assessment

Panjin Center for Inspection and Testing

Wuhai Inspection and Testing Center

广东省农业科学院农产品公共监测中心

Address：100 Xianlie Middle Road, Guangzhou Postal code：510070
Tel：020-87684776,37656606 Fax：020-87684776 Email：fxcsxb@china.com
Technical support is provided by Beijing Founder electronics co., LTD 粤ICP备12017312号-3 京公网安备11010802024621
It is recommended to read the content of this site in Chrome&IE9+. Please switch to extreme mode in browser 360.
Cookies We use cookies to help provide and enhance our service and tailor content. By continuing, you agree to the use of cookies.
Total Visits：380137 Visits Today：615

⁰