同位素稀释-液相色谱串联质谱法测定渔用饲料中氟苯尼考及氟苯尼考胺残留  

Simultaneous determination of florfenicol a nd florfenicol amine residues in fishery feed by isotope dilution-liquid chromatography tandem mass spectrometry

作　　者：杨开智 索纹纹[2] 梁丹 刘伶俐[2] 万译文[2] YANG Kaizhi;SUO Wenwen;LIANG Dan;LIU Lingli;WAN Yiwen(Changde Animal Husbandry and Aquaculture Service Centre,Changde 415000;Hunan Fisheries Science Institute,Changsha 410153)

机构地区：[1]常德市畜牧水产事务中心,湖南常德415000 [2]湖南省水产科学研究所,湖南长沙410153

出　　处：《中国饲料》2022年第12期66-69,共4页China Feed

摘　　要：文章旨在建立同时测定渔用饲料中氟苯尼考及氟苯尼考胺残留量的同位素稀释-高效液相色谱串联质谱法。以氯霉素-D5和氟苯尼考胺-D3位内标,样品用氨化乙酸乙酯提取,混合型阳离子交换固相萃取柱(MCX)净化,在金刚烷基色谱柱上分离,采用LC-MS/MS选择多反应监测(MRM)模式进行定性、定量分析。结果表明:氟苯尼考及氟苯尼考胺的检出限(LOD)为0.2和0.5μg/kg,定量限(LOQ)为1.0和2.0μg/kg,检测结果的相对标准偏差为2.04%~12.1%(n=6),加标回收率达到64.3%~97.0%。该方法具有比较高的重现性和选择性,在渔用饲料中氟苯尼考及氟苯尼考胺的残留测定中具有很好的应用前景。The article aims to establish an analytical method for the determination of florfenicol and florfenicol amine residues in fishery feed by isotope dilution-liquid chromatography-tandem mass spectrometry(LC-MS/MS).CAP-D5 and FFA-D3 was used as the internal standard.The sample was extracted with ammonia ethyl acetate,cleaned-up by MCX,and separated on a Capcell PaK ADME chromatographic column.The mass spectrometer was operated in the multi-reaction monitoring mode for the qualitative and quantitative analysis.The detection limits of this method for florfenicol and florfenicol amine residues were 0.2 and 0.5μg/kg,and the limits of quantification were 1.0 and 2.0μg/kg.The relative standard deviations ranging from 2.04%~12.1%(n=6)and the recovery rates were from 64.3%~97.0%.The method proposed by this paper possesses higher prodicibility and selectivity,It is promising in real applications of determining the florfenicol and florfenicol amine residues in fishery feed.

关 键 词：高效液相色谱-串联质谱法 同位素稀释法 氟苯尼考 氟苯尼考胺 渔用饲料 

分 类 号：S816.17[农业科学—饲料科学]