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采用液相色谱三重四级杆串联质谱法测定鱼肉组织中有机氟农药多残留量。

Multi-residue method for the determination of organofluorine pesticides in fish tissue by liquid chromatography triple quadrupole tandem mass spectrometry.

机构信息

Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan, Hubei 430223, PR China; School of Resource and Environmental Sciences, Wuhan University, Wuhan, Hubei 430079, PR China; Hubei Collaborative Innovation Center for Freshwater Aquaculture, Wuhan 430070, PR China.

Yangtze River Fisheries Research Institute, Chinese Academy of Fishery Sciences, Wuhan, Hubei 430223, PR China.

出版信息

Food Chem. 2016 Sep 15;207:195-204. doi: 10.1016/j.foodchem.2016.02.098. Epub 2016 Feb 15.

Abstract

A multiresidue method for the determination of organofluorine pesticides in fish tissue samples was developed and optimized. This method is based on a cleanup step of the extracted samples with acetonitrile, and carried out by solid phase extraction (SPE) with aminopropyl (NH2) cartridge, before the identification and quantification of the residues by liquid chromatography triple quadrupole tandem mass spectrometry (LC-MS/MS). The performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), for each pesticide were determined. The proposed method allowed high recoveries (80.4-99.2%) of spiked extracted fat samples at 0.5-10 ng g(-1), and very low LODs (between 0.10 and 0.15 ng g(-1)) and LOQs (between 0.3 and 0.5 ng g(-1)) determined in the fish samples. The practicality and high sensitivity of this method have been demonstrated in the determination of residues of OFPs in carp fish fed in water containing 10 ng mL(-1) OFPs.

摘要

建立并优化了一种用于鱼类组织样品中有机氟农药多残留的检测方法。该方法基于乙腈提取样品的净化步骤,采用氨基丙基(NH2)固相萃取(SPE)小柱,然后通过液相色谱三重四极杆串联质谱(LC-MS/MS)对残留物进行鉴定和定量。对每种农药的性能特点,如准确度、精密度、线性范围、检测限(LOD)和定量限(LOQ)进行了测定。该方法在 0.5-10ng g(-1)的浓度下,对添加的提取脂肪样品的回收率高达 80.4-99.2%,在鱼类样品中的检测限(LOD)和定量限(LOQ)分别在 0.10-0.15ng g(-1)和 0.3-0.5ng g(-1)之间,证明了该方法具有实用性和高灵敏度。该方法已成功应用于测定在含有 10ng mL(-1)OFPs 的水中喂养的鲤鱼鱼体内 OFPs 的残留量。

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