禽蛋中氟苯尼考及其代谢产物氟苯尼考胺同时检测的超高效液相色谱-荧光检测法的建立  

Simultaneous determination of florfenicol and its metabolite florfenicol amine in poultry eggs via ultra-performance liquid chromatography-fluorescence detection

作　　者：王波 赵霞[2,3] 谢恺舟 张跟喜[2,3] 张涛 戴国俊[2,3] WANG Bo;ZHAO Xia;XIE Kaizhou;ZHANG Genxi;ZHANG Tao;DAI Guojun(College of Veterinary Medicine,Yangzhou University,Yangzhou 225009;Joint International Research Laboratory of Agriculture&Agri-Product Safety,Yangzhou University,Yangzhou 225009;College of Animal Science and Technology,Yangzhou University,Yangzhou 225009)

机构地区：[1]扬州大学兽医学院,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]扬州大学动物科学与技术学院,扬州225009

出　　处：《安徽农业大学学报》2020年第1期36-43,共8页Journal of Anhui Agricultural University

基　　金：国家现代农业产业技术体系项目(CARS-41-G23);江苏高校优势学科建设工程资助项目;扬州大学“高端人才支持计划”项目和扬州大学研究生国际学术交流专项基金项目共同资助。

摘　　要：建立超高效液相色谱-荧光检测法(UPLC-FLD)同时检测禽蛋中氟苯尼考及其代谢产物氟苯尼考胺残留。样品经过加速溶剂萃取提取、净化,乙腈饱和的正己烷去脂,设定激发波长和发射波长分别为233 nm和284 nm,经UPLC-FLD检测分析。FF和FFA添加浓度为定量限(LOQs)、0.5、1.0和2.0倍的最高残留限量(MRL)时,FF的平均回收率为83.1%~96.1%,相对标准偏差(RSD)均低于3.9%;FFA的平均回收率为84.6%~97.4%,RSD均低于3.4%。FF在禽蛋中检测限(LODs)为4.7~4.9μg·kg^-1(S/N≥3),LOQs为10.5~11.7μg·kg^-1(S/N≥10);FFA在禽蛋中LODs为1.8~1.9μg·kg^-1,LOQs为4.3~4.7μg·kg^-1。此方法快速、准确、灵敏度高,适用于批量检测禽蛋中氟苯尼考及其代谢产物氟苯尼考胺残留。An ultra-performance liquid chromatography-fluorescence detection(UPLC-FLD) method was established to simultaneously detect florfenicol(FF) and its metabolite florfenicol amine(FFA) residues in poultry eggs. The samples were extracted and purified by accelerated solvent extraction(ASE), and the hexane saturated with pure acetonitrile was used to remove the fat. The excitation and emission wavelengths of the method were set at 233 nm and 284 nm, respectively, and the purified samples were analyzed by UPLC-FLD. When the added concentration of FF and FFA were the limits of quantitation(LOQs), 0.5, 1.0, and 2.0 times the maximum residue limit(MRL), the average recoveries of FF were 83.1%-96.1%, and the relative standard deviations(RSDs) were lower than 3.9%. The average recoveries of FFA were 84.6%-97.4%, and the RSDs were lower than 3.4%. Limits of detection(LODs) were 4.7-4.9 μg·kg^-1(S/N≥3) for FF in poultry eggs, LOQs were 10.5-11.7 μg·kg^-1(S/N≥10). LODs were 1.8-1.9 μg·kg^-1 for FFA in poultry eggs, LOQs were 4.3-4.7 μg·kg^-1. The method is rapid, accurate and sensitive, which is suitable for batch detection of florfenicol and its metabolite florfenicol amine residues in poultry eggs.

关 键 词：氟苯尼考 氟苯尼考胺 禽蛋 超高效液相色谱-荧光检测法 

分 类 号：S859.84[农业科学—临床兽医学]