Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography－Tandem Mass Spectrometry

WANG Xing-ning; WANG Tao; LI Jie; LI Zhi; TANG Ya-feng; LIANG Yi-xin; ZHU Ming

doi:10.19969/j.fxcsxb.21020902

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Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography－Tandem Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2023-02-13

- Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 40, Issue 10, Pages: 1526-1531(2021)
- 作者机构：
  
  1.贵阳海关综合技术中心，贵州贵阳 550081
  2.贵州轻工职业技术学院，贵州贵阳 540003
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21020902
  CLC：
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王兴宁,王涛,李洁等.液相色谱－串联质谱法测定植物源性食品中总氟吡禾灵残留[J].分析测试学报,2021,40(10):1526-1531.

WANG Xing-ning,WANG Tao,LI Jie,et al.Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(10):1526-1531.
王兴宁,王涛,李洁等.液相色谱－串联质谱法测定植物源性食品中总氟吡禾灵残留[J].分析测试学报,2021,40(10):1526-1531. DOI： 10.19969/j.fxcsxb.21020902.

WANG Xing-ning,WANG Tao,LI Jie,et al.Determination of Total Haloxyfop in Plant-derived Foods by Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(10):1526-1531. DOI： 10.19969/j.fxcsxb.21020902.

摘要

应用液相色谱－串联质谱（LC－MS/MS）技术，建立了植物源性食品中总氟吡禾灵的测定方法。样品经碱性乙腈提取，用无水MgSO,4,、十八烷基硅烷（C,18,）和石墨化炭黑（GCB）基质分散固相萃取净化。采用0.1%甲酸乙腈和0.1%甲酸水溶液为流动相进行梯度洗脱，C,18,色谱柱（2.1 mm × 50 mm，1.7 µm）分离，在正离子模式下采用多反应监测（MRM）扫描测定，内标法定量。结果表明：氟吡禾灵在2.5～50 ng/mL范围内线性关系良好，相关系数（,r,2,）大于0.999；0.01、0.05、0.1 mg/kg 3个加标水平下，柠檬、柑橘、马铃薯、结球甘蓝、甜椒、洋葱、大米、葵花籽及茶叶9种基质的平均回收率为80.7%～114%，相对标准偏差（RSD）为1.4%～11%；方法定量下限为0.01 mg/kg。该方法显示氟吡禾灵酯类完全转化为总氟吡禾灵，适用于植物源性食品中总氟吡禾灵的快速检测。

Abstract

A simple，fast and reliable method was developed for quantitative determination of total haloxyfop in plant-derived foods using liquid chromatography coupled to tandem mass spectrometry（LC－MS/MS）．The sample preparation consisted of a dispersive solid phase extraction（dispersive-SPE） method by addition of an alkaline hydrolysis step to release total haloxyfop．The target compound was extracted with acetonitrile，and then purified using anhydrous MgSO,4,，octadecyl（C,18,） and graphitized carbon black（GCB）．A mixture of 0.1% formic acid acetonitrile and 0.1% formic acid aqueous solution was used as the mobile phase，followed by binary gradient elution，C,18, （2.1 mm × 50 mm，1.7 µm） column separation．The analysis was performed in positive ion mode under multiple reaction monitoring（MRM） mode，and internal standard method was used for quantitative analysis．Results showed that there was a good linear relationship for haloxyfop over the range of 2.5－50 ng/mL with a correlation coefficient（,r,2,） greater than 0.999.At three spiked levels（0.01，0.05 and 0.1 mg/kg），average recoveries for total haloxyfop ranged from 80.7% to 114%，with relative standard deviations（RSD） of 1.4%－11%．The limit of quantitation was as low as 0.01 mg/kg．The method showed a fully converted step from haloxyfop-esters to haloxyfop，and it was suitable for the analysis of total haloxyfop residues in plant-derived foods．

关键词

总氟吡禾灵碱水解分散固相萃取植物源性食品液相色谱－串联质谱

Keywords

total haloxyfopalkaline hydrolysisdispersive solid phase extractionplant-derived foodsliquid chromatography－tandem mass spectrometry

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