加速溶剂萃取/超高效液相色谱-荧光法检测猪肉中氟苯尼考和氟苯尼考胺残留

doi:10.16431/j.cnki.1671-7236.2019.09.031

Abstract

Abstract: In order to provide a new safe and reliable method for simultaneous detection of florfenicol (FF) and its metabolite florfenicol amine (FFA) residues in animal-derived foods,this study established an accelerated solvent extraction/ultra-high performance liquid chromatography-fluorescence detector (ASE/UPLC-FLD) method for the determination of FF and FFA in pork.Samples were concentrated after accelerated solvent extraction,fat was removed by n-hexane saturated with ethylacetate,then concentrated and re-dissolved before analysis in UPLC-FLD system.The results showed that FF and its metabolite FFA had a good linear relationship in the range of 9.8 to 400 and 3.2 to 400 μg/kg,respectively,and the coefficient of determination (R²) were 0.9993 and 0.9999,respectively.The limit of detection (LOD) and the limit of quantification (LOQ) of FF were 3.3 and 9.8 μg/kg,for FFA were 1.2 and 3.2 μg/kg,respectively.The average recoveries of the samples at LOQ,0.5MRL,1.0MRL and 2.0MRL spiked levels ranged from 82.92% to 96.72%,and the relative standard deviations were below 3.11%.In summary,the ASE extraction method had many advantages such as high extraction efficiency,time saving,environmental protection and so on.The UPLC-FLD method had high efficiency,sensitivity and recovery,and it provided a new method for simultaneous determination of FF and FFA residues in animal-derived food and it was a new method fitting on meets testing standards.

Key words: pork; FF; FFA; residue; ASE; UPLC-FLD

CLC Number:

S859.84

DIAO Zhixiang, ZHANG Peiyang, WANG Xutang, XIE Kaizhou, WANG Bo, ZHAO Xia, GUO Yawen, ZHANG Genxi, ZHANG Tao, DAI Guojun, LIU Xuezhong. Determination of Florfenicol and Florfenicol Amine Residues in Pork by Accelerated Solvent Extraction/Ultra-high Performance Liquid Chromatography-fluorescence[J]. China Animal Husbandry and Veterinary Medicine, 2019, 46(9): 2753-2759.

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Determination of Florfenicol and Florfenicol Amine Residues in Pork by Accelerated Solvent Extraction/Ultra-high Performance Liquid Chromatography-fluorescence

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