食品科学 ›› 2021, Vol. 42 ›› Issue (8): 277-282.doi: 10.7506/spkx1002-6630-20200423-294

• 安全检测 • 上一篇    下一篇

基于低共熔溶剂的液液微萃取技术测定食用油中的新烟碱类杀虫剂

王素利,郭振福,庚丽丽   

  1. (河北北方学院 河北省农产品食品质量安全分析重点实验室,河北 张家口 075000)
  • 出版日期:2021-04-25 发布日期:2021-05-14
  • 基金资助:
    河北省自然科学基金项目(B2017405049);河北省高等学校科学重点研究项目(ZD2016139)

Liquid Phase Microextraction with Deep Eutectic Solvent Combined with High Performance Liquid Chromatography for Determination of New Neonicotinoid Insecticide Residues in Edible Oil

WANG Suli, GUO Zhenfu, GENG Lili   

  1. (Hebei Key Laboratory of Quality and Safety Analysis-testing for Agro-products and Food, Hebei North University, Zhangjiakou 075000, China)
  • Online:2021-04-25 Published:2021-05-14

摘要: 利用合成的低共熔溶剂(deep eutectic solvent,DES)作为液液微萃取技术中的萃取剂,利用超声波辅助分散,建立高效液相色谱测定食用油中4?种新烟碱类杀虫剂(噻虫嗪、吡虫啉、啶虫脒、噻虫啉)的方法。首先将合成的DES加入到含有目标分析物的食用油(正己烷稀释)中,进行超声辅助分散加速提取,然后离心,吸出上层液体,再用微量注射器吸取DES富集相(下层)进行液相色谱分析。根据单一变量法,对影响萃取效率的一些因素进行优化,如DES的种类和体积、超声萃取时间、离心时间等。在最佳条件下,回收率在81.9%~98.0%之间,相对标准偏差为5.5%~8.3%(n=5),检出限范围为3.2~5.3?μg/L,定量限范围为10.8~17.7?μg/L。并且应用所建立的基于DES超声辅助分散液液微萃取方法检测食用油实际样品大豆油、葵花籽油、亚麻籽油中的新烟碱类农药。此方法提取和浓缩一步完成,避免了毒性较大的有机溶剂的使用,具有快速、简单、有效等显著优点。

关键词: 低共熔溶剂;液液微萃取;新烟碱类杀虫剂;食用油

Abstract: In this study, a method for the determination of residues of four new neonicotinoid insecticides (thiamethoxam, imidacloprid, acetamiprid, and thiacloprid) in edible oil was developed using ultrasound-assisted liquid-liquid microextraction with deep eutectic solvent (UA-DES-LLME) followed by high performance liquid chromatography (HPLC). Samples were diluted with n-hexane and added with deep eutectic solvent (DES) before being subjected to ultrasonic-assisted dispersive liquid-liquid microextraction (UALLME). Then, the extract was centrifuged. The lower DES-rich phase was collected and injected into the HPLC system for analysis. Several important parameters influencing the extraction efficiency, such as the type and volume of DES, ultrasonication time, and centrifugation time, were investigated. Under the optimized conditions, the recoveries of the analytes were between 81.9% and 98.0%, with relative standard deviations (RSD, n = 5) of 5.5%–8.3%. The limits of detection (LODs) and limits of quantitation (LOQs) were 3.2?5.3 μg/L and 10.8?17.7 μg/L respectively. The method was successfully applied to real samples of soybean oil, sunflower seed oil and linseed oil. This method combined extraction and concentration in one step without the use of poisonous organic solvents. This method proved to be simple, rapid and efficient.

Key words: deep eutectic solvent; liquid-liquid microextraction; new neonicotinoid insecticides; edible oil

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