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建立一种加速溶剂萃取-超声衍生化 LC-MS/MS 法,用于测定淡水鱼中硝基呋喃类药物的标记残留。

Development of an accelerated solvent extraction, ultrasonic derivatisation LC-MS/MS method for the determination of the marker residues of nitrofurans in freshwater fish.

机构信息

National Reference Laboratory of Veterinary Drug Residues-HZAU/MOA-Key Laboratory of Food Safety Evaluation, Huazhong Agricultural University, Wuhan 430070, China.

出版信息

Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2012;29(5):736-45. doi: 10.1080/19440049.2011.651629. Epub 2012 Feb 9.

DOI:10.1080/19440049.2011.651629
PMID:22320705
Abstract

A rapid method using accelerated solvent extraction (ASE) and ultrasound enhanced derivatisation has been developed for the quantitative determination of metabolites of nitrofurans, namely 3-amino-2-oxalidinone (AOZ), 5-morpholinomethyl-3-amino-2-oxalidinone (AMOZ), 1-amino-hydantoin (AHD) and semicarbazide (SEM), in muscle and skin of carp and finless eel. The target analytes were extracted using ASE, ultrasonic derivatisation for 1 h and then purified by solid phase extraction. Averaged decision limits (CCα) and detection capability (CCβ) of the method were in the range of 0.07-0.13 and 0.31-0.49 µg kg⁻¹ in carp and finless eel, respectively. The accuracy in terms of recovery was in the range 77.2-97.4%. The simplified and traditional methods were compared with incurred residue samples. The simplified method reduced the derivatisation time and has been applied to the determination of nitrofurans residues in fish.

摘要

一种使用加速溶剂萃取(ASE)和超声增强衍生化的快速方法已被开发用于定量测定硝基呋喃代谢物,即 3-氨基-2-恶唑烷酮(AOZ)、5-吗啉甲基-3-氨基-2-恶唑烷酮(AMOZ)、1-氨基乙内酰脲(AHD)和氨基脲(SEM),在鲤鱼和鳗鱼的肌肉和皮肤中。目标分析物使用 ASE 提取,超声衍生化 1 小时,然后通过固相萃取进行纯化。该方法的平均决策限(CCα)和检测能力(CCβ)在鲤鱼和鳗鱼中的范围分别为 0.07-0.13 和 0.31-0.49μg/kg。回收的准确度在 77.2-97.4%范围内。简化和传统方法与实际残留样品进行了比较。简化方法缩短了衍生化时间,并已应用于鱼类中硝基呋喃残留的测定。

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