分散固相萃取-液相色谱质谱法测定水稻和多环境介质中的噁唑酰草胺及其代谢产物

豆叶枝; 李菊颖; 何健; 吴文铸; 倪妮; 张悦清; 余佳; 孔德洋; 单正军

doi:10.7524/j.issn.0254-6108.2019091906

环境化学

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豆叶枝, 李菊颖, 何健, 吴文铸, 倪妮, 张悦清, 余佳, 孔德洋, 单正军. 分散固相萃取-液相色谱质谱法测定水稻和多环境介质中的噁唑酰草胺及其代谢产物[J]. 环境化学, 2020, (10): 2693-2701. doi: 10.7524/j.issn.0254-6108.2019091906

引用本文:

DOU Yezhi, LI Juying, HE Jian, WU Wenzhu, NI Ni, ZHANG Yueqing, YU Jia, KONG Deyang, SHAN Zhengjun. Determination of metamifop and its metabolites in rice and paddy field by ultra performance liquid chromatography-mass spectrometry[J]. Environmental Chemistry, 2020, (10): 2693-2701. doi: 10.7524/j.issn.0254-6108.2019091906

Citation:

DOU Yezhi, LI Juying, HE Jian, WU Wenzhu, NI Ni, ZHANG Yueqing, YU Jia, KONG Deyang, SHAN Zhengjun. Determination of metamifop and its metabolites in rice and paddy field by ultra performance liquid chromatography-mass spectrometry[J]. Environmental Chemistry, 2020, (10): 2693-2701. doi: 10.7524/j.issn.0254-6108.2019091906

分散固相萃取-液相色谱质谱法测定水稻和多环境介质中的噁唑酰草胺及其代谢产物

生态环境部南京环境科学研究所, 国家环境保护农药环境评价与污染控制重点实验室, 南京, 210042

通讯作者: 孔德洋, E-mail: kdy@nies.org ;

基金项目:
国家重点研发计划（2016YFD0200201）和江苏省基础研究计划自然科学基金（BK20190141）资助.

Determination of metamifop and its metabolites in rice and paddy field by ultra performance liquid chromatography-mass spectrometry

Nanjing Institute of Environmental Sciences, Ministry of Ecology and Environment of the People's Republic of China, Key Laboratory of Pesticide Environmental Assessment and Pollution Control, Ministry of Environmental Protection, Nanjing, 210042, China

Corresponding author: KONG Deyang, kdy@nies.org ;

Fund Project: Supported by the National Key Research and Development Program of China(2016YFD0200201)and the Natural Science Foundation of Jiangsu Province, China (BK20190141).

摘要: 建立了田水、土壤、水稻秸秆、稻壳和糙米中噁唑酰草胺及代谢产物6-CBO、HPMFPA、HFMPA的残留分析方法.本文采用乙腈为提取剂，N-丙基乙二胺（PSA）为分散净化剂的QuEChERS前处理方法，并利用超高效液相色谱-串联质谱（UPLC-MS/MS）在多反应离子监测模式（MRM）下进行检测，外标法定量.结果表明，噁唑酰草胺及3种代谢产物在0.005—0.20 mg·L^-1浓度范围内均具有良好的线性关系（R²≥0.997）；在0.01—1.00 mg·kg^-1添加水平范围内平均回收率为71.2%—109%；相对标准偏差（RSD，n=5）为1.4%—9.0%；噁唑酰草胺及3种代谢产物的方法检出限和定量限分别为0.11—0.36 μg·kg^-1和0.01 mg·kg^-1.该方法分析速度快、灵敏度高、重现性好，适用于多种基质上噁唑酰草胺及3种代谢产物6-CBO、HPMFPA、HFMPA的快速检测和确证.
- 噁唑酰草胺 /
- 超高效液相色谱-串联质谱 /
- QuEChERS /
- 水稻和多环境介质
Abstract: A method was developed for the simultaneous determination of metamifop and its metabolites in rice straw,rice husk,rice grain,paddy field water,and paddy soil. The samples were extracted with acetonitrile,and the organic phase was purified with primary secondary amine(PSA),then was determined by ultra performance liquid chromatography-mass spectrometry. The detection was carried out in multi-reaction ion monitoring mode with external standard method for quantification. The linear relationship for metamifop and its metabolites was good within 0.005—0.20 mg·L^-1,and the correlation coefficient (R²) was within 0.997—0.999. The recoveries of metamifop and its metabolites with the spiking levels (0.01—1.00 mg·kg^-1) were within 71.2%—109%,and the relative standard deviation (RSD,n=5) was within 1.4%—9.0%. The detection and quantification limits were 0.11—0.36 μg·kg^-1 and 0.01 mg·kg^-1, respectively. The method is easy to operate with stable recoveries,accurate and reliable results, which is suitable for simultaneous determination of metamifop and its metabolites in environment.
- metamifop /
- UPLC-MS/MS /
- QuEChERS /
- rice and paddy field

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分散固相萃取-液相色谱质谱法测定水稻和多环境介质中的噁唑酰草胺及其代谢产物

通讯作者: 孔德洋, E-mail: kdy@nies.org ;

生态环境部南京环境科学研究所, 国家环境保护农药环境评价与污染控制重点实验室, 南京, 210042

收稿日期: 2019-09-19

基金项目:

国家重点研发计划（2016YFD0200201）和江苏省基础研究计划自然科学基金（BK20190141）资助.

关键词:

摘要: 建立了田水、土壤、水稻秸秆、稻壳和糙米中噁唑酰草胺及代谢产物6-CBO、HPMFPA、HFMPA的残留分析方法.本文采用乙腈为提取剂，N-丙基乙二胺（PSA）为分散净化剂的QuEChERS前处理方法，并利用超高效液相色谱-串联质谱（UPLC-MS/MS）在多反应离子监测模式（MRM）下进行检测，外标法定量.结果表明，噁唑酰草胺及3种代谢产物在0.005—0.20 mg·L^-1浓度范围内均具有良好的线性关系（R²≥0.997）；在0.01—1.00 mg·kg^-1添加水平范围内平均回收率为71.2%—109%；相对标准偏差（RSD，n=5）为1.4%—9.0%；噁唑酰草胺及3种代谢产物的方法检出限和定量限分别为0.11—0.36 μg·kg^-1和0.01 mg·kg^-1.该方法分析速度快、灵敏度高、重现性好，适用于多种基质上噁唑酰草胺及3种代谢产物6-CBO、HPMFPA、HFMPA的快速检测和确证.

English Abstract

Determination of metamifop and its metabolites in rice and paddy field by ultra performance liquid chromatography-mass spectrometry

Corresponding author: KONG Deyang, kdy@nies.org ;

Nanjing Institute of Environmental Sciences, Ministry of Ecology and Environment of the People's Republic of China, Key Laboratory of Pesticide Environmental Assessment and Pollution Control, Ministry of Environmental Protection, Nanjing, 210042, China

Received Date: 2019-09-19

Fund Project: Supported by the National Key Research and Development Program of China(2016YFD0200201)and the Natural Science Foundation of Jiangsu Province, China (BK20190141).

Keywords:

Abstract: A method was developed for the simultaneous determination of metamifop and its metabolites in rice straw,rice husk,rice grain,paddy field water,and paddy soil. The samples were extracted with acetonitrile,and the organic phase was purified with primary secondary amine(PSA),then was determined by ultra performance liquid chromatography-mass spectrometry. The detection was carried out in multi-reaction ion monitoring mode with external standard method for quantification. The linear relationship for metamifop and its metabolites was good within 0.005—0.20 mg·L^-1,and the correlation coefficient (R²) was within 0.997—0.999. The recoveries of metamifop and its metabolites with the spiking levels (0.01—1.00 mg·kg^-1) were within 71.2%—109%,and the relative standard deviation (RSD,n=5) was within 1.4%—9.0%. The detection and quantification limits were 0.11—0.36 μg·kg^-1 and 0.01 mg·kg^-1, respectively. The method is easy to operate with stable recoveries,accurate and reliable results, which is suitable for simultaneous determination of metamifop and its metabolites in environment.