超高效合相色谱法测定鱼肉中氟苯尼考对映体及其代谢产物残留量  

Determination of Residues of Florfenicol Enantiomers and Its Metabolites in Fish by Ultra-Performance Convergence Chromatography

作　　者：张文华 吴媛 施雅梅 汪鹏 叶芮辰 徐可 谢文 徐敦明 伊雄海 ZHANG Wenhua;WU Yuan;SHI Yamei;WANG Peng;YE Ruichen;XU Ke;XIE Wen;XU Dunming;YI Xionghai(The Technical Center of Hangzhou Customs,Hangzhou 310016,China;Zhejiang Academy of Science and Technology for Inspection and Quarantine,Hangzhou 310016,China;The Technical Center of Xiamen Customs,Xiamen 361026,China;Technical Center for Animal,Plant and Food Inspection and Quarantine,Shanghai Customs,Shanghai 200135,China)

机构地区：[1]杭州海关技术中心,浙江杭州310016 [2]浙江省检验检疫科学技术研究院,浙江杭州310016 [3]厦门海关技术中心,福建厦门361026 [4]上海海关动植物与食品检验检疫技术中心,上海200135

出　　处：《食品科学》2022年第20期321-327,共7页Food Science

基　　金：“十三五”国家重点研发计划重点专项(2019YFC1605400);海关总署科研项目(2020HK196);浙江省科技计划项目(2018C37014)。

摘　　要：建立一种超高效合相色谱法分离并测定鱼肉中氟苯尼考对映体及其代谢物氟苯尼考胺残留。最优样品前处理条件:采用氨化乙酸乙酯提取样品,MCX固相萃取小柱净化。最优超高效合相色谱条件:采用CHIRALPAK AD-3手性色谱柱(150 mm×3.0 mm,3μm)分离,以超临界CO(流动相A)和氨水-甲醇溶液(0.5∶99.5,V/V)(流动相B)为流动相进行梯度洗脱,系统背压13.8 MPa,柱温40℃。在最优条件下,结果表明:两种氟苯尼考对映体在1.0~20.0 mg/L范围内及氟苯尼考胺在2.0~40.0 mg/L范围内线性相关系数均大于0.999 3,方法定量限(信噪比10)分别为0.1 mg/kg(氟苯尼考对映体)和0.2 mg/kg(氟苯尼考胺)。鱼肉中氟苯尼考对映体及氟苯尼考胺在0.1~1.0 mg/kg范围内的加标回收率为81.5%~108.0%,相对标准偏差为5.3%~9.3%。该方法实现了氟苯尼考对映体的分离及其代谢物在鱼肉样品中的残留测定。An ultra-performance convergence chromatography(UPC~2) method was established for the separation and determination of the residues of florfenicol enantiomers and its metabolite florfenicol amine in fish meat.The samples were extracted with alkalized ethyl acetate,purified on a solid phase extraction column(MCX),and separated on a CHIRALPAK AD-3 column(150 mm × 3.0 mm,3 μm) by gradient elution using a mobile phase consisting of supercritical CO(A) and aqueous ammonia-methanol in water(0.5:99.5,V/V)(B).The system’s back pressure and the column temperature were set at13.8 MPa and 40 ℃,respectively.The linear correlation coefficients were greater than 0.999 3 in the range of 1.0-20.0 mg/L for the two florfenicol enantiomers and 2.0-40.0 mg/L for florfenicol amine,and the limits of quantification(R=10) were0.1 and 0.2 mg/kg,respectively.The recoveries of the florfenicol enantiomers and florfenicol amine from spiked fish in the range of 0.1-1.0 mg/kg were 81.5%-108.0%,with relative standard deviations(RSDs) of 5.3%-9.3%.This method is suitable for the separation and determination of the residues of florfenicol enantiomers and its metabolite in fish meat.

关 键 词：超高效合相色谱 氟苯尼考 鱼肉 对映体 手性分离 

分 类 号：O657.63[理学—分析化学]