Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage

WANG Tan; SUN Qiang; SHEN Qin-yi; CHEN Shan-shan; WEN Guang-yue; ZHAO Li; DONG Mao-feng; WANG Wei-min

doi:10.19969/j.fxcsxb.21032403

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Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage

Scientific Papers | 更新时间：2023-02-13

- Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage
- Journal of Instrumental Analysis Vol. 40, Issue 12, Pages: 1706-1712(2021)
- 作者机构：
  
  1.上海市农业科学院农药安全评价研究中心，上海　201106
  2.上海市农业技术推广服务中心，上海　201103
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21032403
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王坦,孙强,沈沁怡等.超高压液相色谱法测定水果和蔬菜中虫螨腈及其代谢物以及在甘蓝中的残留评价应用[J].分析测试学报,2021,40(12):1706-1712.

WANG Tan,SUN Qiang,SHEN Qin-yi,et al.Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage[J].Journal of Instrumental Analysis,2021,40(12):1706-1712.
王坦,孙强,沈沁怡等.超高压液相色谱法测定水果和蔬菜中虫螨腈及其代谢物以及在甘蓝中的残留评价应用[J].分析测试学报,2021,40(12):1706-1712. DOI： 10.19969/j.fxcsxb.21032403.

WANG Tan,SUN Qiang,SHEN Qin-yi,et al.Determination of Chlorfenapyr and Its Metabolite in Fruits and Vegetables by Ultra Performance Liquid Chromatography and Its Application in Residual Evaluation of Cabbage[J].Journal of Instrumental Analysis,2021,40(12):1706-1712. DOI： 10.19969/j.fxcsxb.21032403.

摘要

建立了采用固相萃取柱净化，超高压液相色谱（UPLC）同时测定蔬菜和水果中虫螨腈及其代谢物溴代吡咯腈残留量的分析方法。方法验证结果表明，在25～5 000 ng·mL,－1,范围内目标化合物的质量浓度和仪器响应呈良好线性关系，相关系数（,r,2,）为0.997～1.000；在0.05、1、2 mg·kg,－1,加标水平下，目标化合物的回收率为84.6%～111%，相对标准偏差为1.6%～14%；方法定量下限均为0.05 mg·kg,－1,。2020年在全国12地开展田间试验，360 g·L,－1,虫螨腈悬浮剂以20 mL/亩（125.28 g a.i./ha）施药1次，甘蓝中虫螨腈的消解动态符合一级动力学方程，半衰期为4.1～11.0 d。当采样间隔为末次施药后14 d和21 d时，虫螨腈在甘蓝中的残留量分别为小于0.05～0.488 mg·kg,－1,和小于0.05～0.370 mg·kg,－1,，溴代吡咯腈的残留量均低于0.05 mg·kg,－1,。结合我国制定的虫螨腈在甘蓝上的最大残留限量，推荐采收安全间隔期为14 d。膳食风险评估结果表明：普通人群虫螨腈（膳食风险评估定义）的国家估算每日摄入量为1.28 mg，占日允许摄入量的67.7%，对一般人群健康均不会产生不可接受的风险。

Abstract

An ultra performance liquid chromatography（UPLC） with solid phase extraction was developed for the simultaneous determination of chlorfenapyr and its metabolite tralopyril in fruits and vegetables．The validation results showed that there was a good linear relationship in the range of 25－5 000 ng·mL,-1, with correlation coefficients（,r,2,） of 0.997－1.000. The average recoveries at three spiked levels of 0.05，1 and 2 mg·kg,－1, ranged from 84.6% to 111%，with relative standard deviations（RSD，,n ,= 5） of 1.6%－14%．The limits of quantitation（LOQ） were both 0.05 mg·kg,－1, for the two target compounds. Field trials were carried out in 12 areas nationwide in 2020，after 360 g·L,-1, chlorfenapyr suspension was sprayed once at 20 mL/mu（125.28 g a.i./ha），the dissipation of chlorfenapyr in cabbage accorded with the first-order kinetics equation，and the half-life period was 4.1－11.0 d．When the sampling intervals were 14 d and 21 d，the residual levels of chlorfenapyr in cabbage were lower than 0.05－0.488 mg·kg,－1, and lower than 0.05－0.370 mg·kg,－1,，respectively，while those of tralopyril in cabbage were both lower than 0.05 mg·kg,－1,．Based on the MRLs of China，14 d was selected as the post harvest interval. The dietary risk assessment revealed that the national estimated daily intake of chlorfenapyr（definition for dietary risk assessment） was 1.28 mg，accounting for 67.7% of the acceptable daily intake，which showed there was no significant dietary risk to residents' health.

关键词

超高压液相色谱虫螨腈溴代吡咯腈残留评价水果蔬菜

Keywords

ultra performance liquid chromatographychlorfenapyrtralopyrilresidual evaluationfruitsvegetables

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