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利用亚临界水萃取和超高效液相色谱-串联质谱法测定鳗鱼中的新烟碱类杀虫剂残留。

Determination of neonicotinoid insecticides residues in eels using subcritical water extraction and ultra-performance liquid chromatography-tandem mass spectrometry.

机构信息

Institute of Quality Standard and Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, China.

出版信息

Anal Chim Acta. 2013 May 13;777:32-40. doi: 10.1016/j.aca.2013.03.026. Epub 2013 Mar 21.

Abstract

A rapid, sensitive, and environmental-friendly multi-residue method has been developed for the simultaneous determination of seven neonicotinoid insecticides (dinotefuran, nitenpyram, thiamethoxam, imidacloprid, clothianidin, acetamiprid, and thiacloprid) residues in eel samples. Subcritical water extraction was investigated as a novel and alternative technology for the extraction of neonicotinoids from eel matrices and the results were compared with the conventional ultrasonic and shaking extraction. The target compounds were identified and quantitatively determined by ultra-performance liquid chromatography coupled with electrospray ionization tandem mass spectrometry (UPLC-MS/MS) operated in multiple reaction monitoring mode. Under the current optimized chromatographic conditions, each LC run was completed in 5 min. Average recoveries of the seven analytes from fortified samples ranged between 84.6% and 102.0%, with relative standard deviations (RSD) lower than 10.8%. The limits of detection (LODs) and quantification (LOQs) for neonicotinoids were in the ranges of 0.12-0.36 μg kg(-1) and 0.42-1.12 μg kg(-1), respectively. The proposed method is fast, sensitive, easy to perform, water-based thus more environmentally acceptable, making it applicable for high-throughput monitoring of insecticides residues in aquatic products.

摘要

一种快速、灵敏、环保的多残留方法已经被开发出来,用于同时测定鳗鱼样品中七种新烟碱类杀虫剂(噻虫嗪、噻虫胺、噻虫啉、吡虫啉、噻虫酰胺、噻虫嗪和噻虫砜)的残留量。亚临界水萃取被研究作为一种从鳗鱼基质中提取新烟碱类杀虫剂的新技术,并与传统的超声波和振荡萃取进行了比较。目标化合物通过超高效液相色谱-电喷雾串联质谱(UPLC-MS/MS)在多反应监测模式下进行定性和定量分析。在当前优化的色谱条件下,每个 LC 运行在 5 分钟内完成。七种分析物从加标样品中的平均回收率在 84.6%到 102.0%之间,相对标准偏差(RSD)低于 10.8%。新烟碱类杀虫剂的检出限(LODs)和定量限(LOQs)分别在 0.12-0.36 μg kg(-1)和 0.42-1.12 μg kg(-1)之间。该方法快速、灵敏、易于操作,基于水相,因此更环保,适用于水产品中杀虫剂残留的高通量监测。

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