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Molecules. 2019 May 13;24(9). pii: E1830. doi: 10.3390/molecules24091830.

Development of an Accelerated Solvent Extraction-Ultra-Performance Liquid Chromatography-Fluorescence Detection Method for Quantitative Analysis of Thiamphenicol, Florfenicol and Florfenicol Amine in Poultry Eggs.

Wang B1,2, Xie X3, Zhao X4,5, Xie K6,7, Diao Z8,9, Zhang G10,11, Zhang T12,13, Dai G14,15.

Author information

1
College of Veterinary Medicine, Yangzhou University, Yangzhou 225009, China. yzwbo168@163.com.
2
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. yzwbo168@163.com.
3
Key Laboratory of Veterinary Biological Engineering and Technology, Ministry of Agriculture, Institute of Veterinary Medicine, Jiangsu Academy of Agricultural Sciences, Nanjing 210014, China. yzxx1989@163.com.
4
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. 18252711481@139.com.
5
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. 18252711481@139.com.
6
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. yzxkz168@163.com.
7
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. yzxkz168@163.com.
8
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. 18352764521@163.com.
9
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. 18352764521@163.com.
10
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. zgx1588@126.com.
11
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. zgx1588@126.com.
12
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. zhangt@yzu.edu.cn.
13
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. zhangt@yzu.edu.cn.
14
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China. gjdai@163.com.
15
College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China. gjdai@163.com.

Abstract

A simple, rapid and novel method for the detection of residues of thiamphenicol (TAP), florfenicol (FF) and its metabolite, florfenicol amine (FFA), in poultry eggs by ultra-performance liquid chromatography-fluorescence detection (UPLC-FLD) was developed. The samples were extracted with acetonitrile-ammonia (98:2, v/v) using accelerated solvent extraction (ASE) and purified by manual degreasing with acetonitrile-saturated n-hexane. The target compounds were separated on an ACQUITY UPLC® BEH C18 (2.1 mm × 100 mm, 1.7 μm) chromatographic column using a mobile phase composed of 0.005 mol/L NaH2PO4, 0.003 mol/L sodium lauryl sulfate and 0.05% trimethylamine, adjusted to pH 5.3 ± 0.1 by phosphoric acid and acetonitrile (64:36, v/v). The limits of detection (LODs) and limits of quantification (LOQs) of the three target compounds in poultry eggs were 1.8-4.9 µg/kg and 4.3-11.7 µg/kg, respectively. The recoveries of the three target compounds in poultry eggs were above 80.1% when the spiked concentrations of three phenicols were the LOQ, 0.5 maximum residue limit (MRL), 1.0 MRL and 2.0 MRL. The intraday relative standard deviations (RSDs) were less than 5.5%, and the interday RSDs were less than 6.6%. Finally, this new detection method was successfully applied to the quantitative analysis of TAP, FF and FFA in 150 commercial poultry eggs.

KEYWORDS:

ASE; UPLC-FLD; florfenicol; florfenicol amine; poultry eggs; thiamphenicol

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