加速溶剂萃取/超高效液相色谱-荧光法检测鸽蛋和鹌鹑蛋中氟苯尼考和氟苯尼考胺残留  

ASE/UHPLC-FLD Determination of Florfenicol and Florfenicol Amine Residues in Pigeon and Quail Eggs

作　　者：刁志祥 王波[2,3] 张培杨 王旭堂 谢恺舟 赵霞[1,2] DIAO Zhi-xiang;WANG Bo;ZHANG Pei-yang;WANG Xu-tang;XIE Kai-zhou;ZHAO Xia(College of Animal Science and Technology,Yangzhou University,Yangzhou,Jiangsu 225009,China;Joint International Research Laboratory of Agriculture&Agri-Product Safety,Yangzhou University,Yangzhou,Jiangsu 225009,China;College of Veterinary Medicine,Yangzhou University,Yangzhou,Jiangsu 225009,China)

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

出　　处：《福建农业学报》2019年第11期1315-1322,共8页Fujian Journal of Agricultural Sciences

基　　金：国家现代农业产业技术体系建设专项(CARS-41-G23);扬州大学"高端人才支持计划"项目(201801)

摘　　要：【目的】建立鸽蛋和鹌鹑蛋中尼考(florfenicol,FF)及其主要代谢产物氟苯尼考胺(florfenicol amine,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,为动物源性食品中FF和FFA残留检测提供新的安全可靠的方法。【方法】采用加速溶剂萃取(ASE)法,用乙腈﹕氨水(98﹕2,V/V)为提取剂萃取样品,用乙腈饱和的正己烷去脂进行纯化,使用由0.005 mol·L-1 NaH2PO4、0.003 mol·L-1十二烷基硫酸钠和0.05%三甲胺组成的流动相供UPLC-FLD检测。【结果】鸽蛋和鹌鹑蛋中FF和FFA在定量限(LOQ)~400μg·kg-1范围内,目标物的峰面积与其浓度均呈现良好的线性关系,相关系数(R2)均大于0.999 2。样品在LOQ、50.0、100.0、200.0μg·kg-1的加标水平下的平均回收率为84.69%~98.04%,相对标准偏差(RSD)均低于3.7%。鸽蛋中FF的检测限(LOD)和LOQ为4.8μg·kg-1和11.2μg·kg-1,FFA的LOD和LOQ为1.9μg·kg-1和4.8μg·kg-1;鹌鹑蛋中FF的LOD和LOQ为4.7μg·kg-1和10.6μg·kg-1,FFA的LOD和LOQ为1.8μg·kg-1和4.6μg·kg-1。【结论】该方法快速、简单、灵敏度高,适合禽蛋中FF及其代谢产物FFA的检测。【Objective】 To establish an analytical method for simultaneous detections of florfenicol(FF) and its metabolite,florfenicol amine(FFA), in animal-derived foods. 【 Method】 Samples of pigeon and quail eggs were extracted by the accelerated solvent extraction(ASE) method with acetonitrile-ammonia(98:2, V/V) as the solvent. The extract was degreased and purified with acetonitrile-saturated n-hexane. A mobile phase consisting of 0.005 mol·L-1 NaH2PO4, 0.003 mol·L-1 sodium lauryl sulfate and 0.05% trimethylamine was used in the ultra-high performance liquid chromatography-fluorescence(ASE/UPLC-FLD) determination of FF and FFA contents. 【 Result】 Highly correlated linear relationships(R2>0.999 2)within the limit of quantitation(LOQ) were achieved between the peak area and concentration on the target compounds. The average recoveries of the method at the spiked levels of 50.0, 100.0, 200.0 μg·kg-1 and LOQ ranged from 84.69% to 98.04% with RSDs less than 3.7%. The method delivered the limit of detection(LOD) and LOQ on FF in the pigeon eggs at 4.8 μg·kg-1 and 11.2 μg·kg-1, respectively, and those on FFA, at 1.9 μg·kg-1 and 4.8 μg·kg-1, respectively;whereas, those on FF in the quail eggs, at 4.7 μg·kg-1 and 10.6 μg·kg-1, respectively, and those on FFA, at 1.8 μg·kg-1 and 4.6 μg·kg-1, respectively.【Conclusion】 The newly developed analytical methodology was rapid, simple, sensitive, and considered suitable for FF and FFA determinations in pigeon and quail eggs.

关 键 词：鸽蛋 鹌鹑蛋 氟苯尼考 氟苯尼考胺 加速溶剂萃取 超高效液相色谱-荧光法 

分 类 号：S859.796[农业科学—临床兽医学]