食品与发酵工业 >

2023 , Vol. 49 >Issue 20: 294 - 299

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.033212

分析与检测

分散液液微萃取/气相色谱法检测植物油中11种有机磷农药残留

  • 李芳芳 ,
  • 王艳丽 ,
  • 李洁 ,
  • 陈倩倩 ,
  • 田其燕 ,
  • 陈克云 ,
  • 鞠香 ,
  • 赵发 ,
  • 张卉 ,
  • 刘艳明
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  • (山东省食品药品检验研究院,国家市场监管重点实验室(肉及肉制品监管技术),山东省特殊医学用途配方食品质量控制工程技术研究中心,山东省食品药品安全检测工程技术研究中心,山东 济南,250101)
第一作者：硕士,工程师(刘艳明研究员为通信作者,E-mail:msymliu@163.com)

收稿日期: 2022-08-05

  修回日期: 2022-11-04

  网络出版日期: 2023-11-20

基金资助

山东省药品监督管理局科研项目(SDNMPAFZLS202202);山东省食品药品检验研究院科研项目(SDIFDC-KY-2021011)

收起

Study on determination of 11 organophosphorus pesticide residues in vegetable oil samples by gas chromatography combined with dispersive liquid-liquid microextraction

  • LI Fangfang ,
  • WANG Yanli ,
  • LI Jie ,
  • CHEN Qianqian ,
  • TIAN Qiyan ,
  • CHEN Keyun ,
  • JU Xiang ,
  • ZHAO Fa ,
  • ZHANG Hui ,
  • LIU Yanming
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  • (Shandong Institute for Food and Drug Control, Key Laboratory of Supervising Technology for Meat and Meat Products for State Market Regulation, Shandong Research Center of Engineering and Technology for Quality Control of Food for Special Medical Purposes, Shandong Research Center of Engineering and Technology for Safety Inspection of Food and Drug, Jinan 250101, China)

Received date: 2022-08-05

  Revised date: 2022-11-04

  Online published: 2023-11-20

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摘要

基于绿色化学理念,该研究选取绿色环保的分散液液微萃取前处理技术,结合气相色谱-火焰光度检测器对有机磷农药检测的专一性,建立了植物油中11种有机磷农药残留的分析方法。样品先经正己烷溶解,然后加入N,N-二甲基甲酰胺进行提取,提取液加入微量二氯甲烷进行分散液液微萃取,目标物经火焰光度检测器检测,外标法定量。研究了影响萃取效率的因素(样品的提取条件、萃取剂种类及体积、分散剂种类及体积、氯化钠添加量等),确定了最佳实验条件。最佳条件下,在0.01~1.00 μg/mL内,11种有机磷农药线性关系良好,相关系数为0.999 1~0.999 7。当加标水平为0.01、0.10、0.50 mg/kg时,所有目标物的回收率为75.6%~116.2%,相对标准偏差为1.6%~8.7%。分析物的检出限为0.002~0.003 mg/kg,定量限为0.007~0.010 mg/kg。经验证,该方法具有快速、简单和对环境友好的特点,可用于植物油中有机磷农药的快速检测。

关键词： 分散液液微萃取; 气相色谱法; 火焰光度检测器; 有机磷农药残留; 植物油

本文引用格式

李芳芳 , 王艳丽 , 李洁 , 陈倩倩 , 田其燕 , 陈克云 , 鞠香 , 赵发 , 张卉 , 刘艳明 . 分散液液微萃取/气相色谱法检测植物油中11种有机磷农药残留[J]. 食品与发酵工业, 2023 , 49(20) : 294 -299 . DOI: 10.13995/j.cnki.11-1802/ts.033212

Abstract

Based on green chemistry, a new method for the determination of 11 organophosphorus pesticide residues in vegetable oil was established, which selected green dispersive liquid-liquid microextraction as pre-treatment technology and gas chromatography-flame photometric detector with specificity for the detection of organophosphorus pesticides. The sample was dissolved in n-hexane, and extracted with N, N-dimethylformamide. The extraction solution was added with trace dichloromethane for dispersive liquid-liquid microextraction. The dichloromethane phase was detected by a flame photometric detector and quantified by an external standard method. The factors affecting the extraction efficiency were investigated, such as the conditions of sample extraction, the type and volume of extraction and dispersive solvent, and the concentration of sodium chloride. The best operational conditions were selected. Under the best operational conditions, the calibration curves were linear in the range of 0.01-1.00 μg/mL and the correlation coefficients were 0.999 1-0.999 7 for the 11 organophosphorus pesticides. The recoveries of the 11 organophosphorus pesticides ranged from 75.6% to 116.2% with relative standard deviation (RSD) values from 1.6% to 8.7% at three spiked levels of 0.01, 0.10, and 0.50 mg/kg. The limits of detection (LODs) were 0.002-0.003 mg/kg and the limits of quantification (LOQs) were 0.007-0.010 mg/kg. The method has been proven to be rapid, simple, and environmental-friendly, which is applicable to the determination of organophosphorus pesticides in vegetable oil.

Key words： dispersive liquid-liquid microextraction; gas chromatography; flame photometric detector; organophosphorus pesticide residues; vegetable oil

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