Determination of 180 Pesticide Residues in Olive Oil by Dispersive Liquid-Liquid Microextraction with Gas Chromatography- Quadrupole-Time-of-flight Mass Spectrometry

LIANG Yan; LEI Chun-ni; WANG Bo; ZHANG Huan; WANG Xin-chao; ZHOU Xiao-ping; ZHU Meng-chen

doi:10.12452/j.fxcsxb.23103104

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Determination of 180 Pesticide Residues in Olive Oil by Dispersive Liquid-Liquid Microextraction with Gas Chromatography- Quadrupole-Time-of-flight Mass Spectrometry

Scientific Papers | 更新时间：2024-03-13

- Determination of 180 Pesticide Residues in Olive Oil by Dispersive Liquid-Liquid Microextraction with Gas Chromatography- Quadrupole-Time-of-flight Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 3, Pages: 393-404(2024)
- 作者机构：
  
  1.甘肃农业大学食品科学与工程学院，甘肃兰州 730070
  2.兰州海关技术中心，甘肃兰州 730010
  3.西北师范大学地理与环境科学学院，甘肃兰州 730070
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23103104
  CLC： O657.7;TS207.3
- Published：15 March 2024，
  
  Received：31 October 2023，
  
  Revised：13 December 2023，
- 稿件说明：
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梁艳,雷春妮,王波等.分散液液微萃取结合气相色谱-四极杆-飞行时间质谱法测定橄榄油中180种农药残留[J].分析测试学报,2024,43(03):393-404.

LIANG Yan,LEI Chun-ni,WANG Bo,et al.Determination of 180 Pesticide Residues in Olive Oil by Dispersive Liquid-Liquid Microextraction with Gas Chromatography- Quadrupole-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(03):393-404.
梁艳,雷春妮,王波等.分散液液微萃取结合气相色谱-四极杆-飞行时间质谱法测定橄榄油中180种农药残留[J].分析测试学报,2024,43(03):393-404. DOI： 10.12452/j.fxcsxb.23103104.

LIANG Yan,LEI Chun-ni,WANG Bo,et al.Determination of 180 Pesticide Residues in Olive Oil by Dispersive Liquid-Liquid Microextraction with Gas Chromatography- Quadrupole-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(03):393-404. DOI： 10.12452/j.fxcsxb.23103104.

摘要

建立了分散液液微萃取（DLLME）结合气相色谱-四极杆-飞行时间质谱（GC-QTOF MS）快速测定橄榄油中180种农药残留的分析方法，并考察了乙腈酸化浓度、水相体积、萃取剂种类的影响。通过分散液液微萃取进行样品前处理，经含2%甲酸的乙腈溶液提取后，上清液与萃取剂快速注入水相，取待测物供仪器分析，采用基质标准溶液进行定量。结果表明：87.8%农药的线性范围为0.02~2 μg/mL，12.2%农药的线性范围为0.1~2 μg/mL，相关系数（

）均大于0.99；所有待测农药的检出限为0.002~0.020 mg/kg，定量下限为0.007~0.067 mg/kg，其中有135种农药的定量下限达0.007 mg/kg，23种农药的定量下限达0.017 mg/kg，占总数量的88%；在0.02、0.1、0.2 mg/kg 3个加标水平下，回收率为70%~120%的农药占全部待测农药的76.3%，相对标准偏差（RSD）小于10%的农药占总数的94.4%以上。应用该方法对10份市售橄榄油样品进行检测，共检出5种农药，检出量为0.005 7~0.042 7 mg/kg。该方法操作简单、快速，精密度及准确度良好，试剂消耗少且绿色环保，能够满足橄榄油中多种农药残留检测的需求。

Abstract

A rapid analytical method for the determination of multi-pesticide residues in olive oil by dispersive liquid-liquid microextraction（DLLME） coupled with gas chromatography-quadrupole-time-of-flight mass spectrometry（GC-QTOF MS） was developed based on the concept of green environmental protection. The effects of acetonitrile acidification concentration，water phase volume and extractant type on the determination of pesticide residues were also investigated. First，the ions with better response and no obvious interference were selected for quantification and characterization. The sample was then pretreated by dispersive liquid-liquid microextraction.After extracted with acetonitrile solution containing 2% formic acid，the supernatant and extractant were rapidly injected into the aqueous phase，and the analytes were taken for instrumental analysis. Finally，a matrix standard solution was used for quantification. The results showed that the linear ranges were 0.02-2 μg/mL for 87.8% of the pesticides and 0.1-2 μg/mL for 12.2% of the pesticides. The correlation coefficients（

） were all greater than 0.99，and the pesticide residues were well related within their respective linear ranges. The limits of detection（LODs） of all the tested pesticides were 0.002-0.020 mg/kg and the limits of quantitation（LOQs） were 0.007-0.067 mg/kg. Among them，the LOQs of 135 pesticides can reach 0.007 mg/kg and 23 pesticides can reach 0.017 mg/kg，which accounted for 88% of the total quantity. At the three spiked levels of 0.02，0.1 and 0.2 mg/kg，the pesticides with recoveries ranging from 70% to 120% accounted for 76.3% of the total pesticides tested. The pesticides with relative standard deviations（RSDs） less than 10% accounted for more than 94.4% of the total. The method was applied to 10 samples of commercially available olive oil，and five pesticides were detected with the content range of 0.005 7-0.042 7 mg/kg. The method is simple，rapid，sensitive，precise and accurate，with low consumption of reagents and green environment，which can meet the needs of pesticide residue detection in olive oil.

关键词

分散液液微萃取气相色谱-四极杆-飞行时间质谱法橄榄油农药残留

Keywords

dispersive liquid-liquid microextraction（DLLME）gas chromatography-quadrupole-time-of-flight mass spectrometry（GC-QTOF MS）olive oilpesticide residues

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