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  

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

作　　者：刁志祥 张培杨 王旭堂 谢恺舟[1,2] 王波 赵霞[1,2] 郭亚文 张跟喜[1,2] 张涛 戴国俊[1,2] 刘学忠 DIAO Zhixiang;ZHANG Peiyang;WANG Xutang;XIE Kaizhou;WANG Bo;ZHAO Xia;GUO Yawen;ZHANG Genxi;ZHANG Tao;DAI Guojun;LIU Xuezhong(College of Animal Science and Technology,Yangzhou University,Yangzhou 225009,China;Joint International Research Laboratory of Agriculture&Agri-Product Safety,Yangzhou University,Yangzhou 225009,China;College of Veterinary Medicine,Yangzhou University,Yangzhou 225009,China)

机构地区：[1]扬州大学动物科学与技术学院,扬州225009 [2]教育部农业与农产品安全国际合作联合实验室,扬州225009 [3]扬州大学兽医学院,扬州225009

出　　处：《中国畜牧兽医》2019年第9期2753-2759,共7页China Animal Husbandry & Veterinary Medicine

基　　金：国家现代农业产业技术体系项目(CARS-41-G23);扬州大学“高端人才支持计划”项目(201801);江苏省农业科技自主创新基金项目(CX(18)3022)

摘　　要：为给动物源性食品中同时检测氟苯尼考(FF)及其主要代谢产物氟苯尼考胺(FFA)的残留提供新的安全可靠的方法,本研究建立了猪肉中FF及FFA残留检测的加速溶剂萃取/超高效液相色谱-荧光检测(ASE/UPLC-FLD)法。试验采用乙酸乙酯∶氨水(98∶2,V/V)为提取剂,样品经加速溶剂萃取后浓缩,用乙酸乙酯饱和正己烷除脂,再经浓缩复溶后进行UPLC-FLD检测。结果表明,FF及其代谢产物FFA在添加浓度为9.8~400和3.2~400μg/kg的范围内线性关系良好,相关系数(R 2)分别为0.9993和0.9999。FF的检测限(LOD)和定量限(LOQ)分别为3.3和9.8μg/kg;FFA的LOD和LOQ分别为1.2和3.2μg/kg。样品在LOQ、0.5 MRL、1.0 MRL和2.0 MRL加标水平下的平均回收率为82.92%~96.72%,相对标准偏差(RSD)低于3.11%。综上所述,加速溶剂萃取(ASE)方法省时、环保、提取效率高,超高效液相色谱-荧光检测(UPLC-FLD)检测方法高效、灵敏、回收率高,是符合检测标准的新方法。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 400μg/kg,respectively,and the coefficient of determination(R 2)were 0.9993 and 0.9999,respectively.The limit of detection(LOD)and the limit of quantification(LOQ)of FF were 3.3 and 9.8μg/kg,for FFA were 1.2 and 3.2μg/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.

关 键 词：猪肉 氟苯尼考(FF) 氟苯尼考胺(FFA) 残留 加速溶剂萃取(ASE) 超高效液相色谱-荧光检测(UPLC-FLD) 

分 类 号：S859.84[农业科学—临床兽医学]