液相色谱-串联质谱法同时快速检测鸡蛋中的氟苯尼考及其代谢物残留  

Chromatography-tandem mass spectrometry based simultaneously determination of florfenicol and flufenicol-amide drugs residues in egg

作　　者：张婧 吴剑平 王博 陶玉洁 严凤 ZHANG Jing;WU Jian-ping;WANG Bo;TAO Yu-jie;YAN Feng(Shanghai Municipal Supervisory Institute Veterinary Drugs and Feedstaff,Shanghai 201103,China)

机构地区：[1]上海市兽药饲料检测所,上海201103

出　　处：《化学研究与应用》2024年第9期2210-2216,共7页Chemical Research and Application

基　　金：上海市科技兴农项目(沪农科推字(2020)第1-4号)资助。

摘　　要：建立鸡蛋中氟苯尼考及其代谢物氟苯尼考胺的液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品采用2%氨水乙酸乙酯提取并经C_(18)粉净化,以Waters HSS T3色谱柱(100mm×2.1mm,1.8μm)分离,0.01%甲酸水溶液和乙腈溶液为流动相进行梯度洗脱,并采用HPLC-MS/MS电喷雾电源(ESI)正负离子同时采集检测,以内标法定量。结果表明:氟苯尼考及氟苯尼考胺在0.1~10ng·mL^(-1)范围内线性关系良好;检出限为0.6μg·kg^(-1);方法回收率范围为89.1~109.6%,相对标准偏差范围为4.4~15.3%。该方法较传统的检测方法省去了繁琐的前处理步骤,分析速度快、效率高、灵敏度好,填补了鸡蛋中氟苯尼考及氟苯尼考胺同时检测的标准检测技术空白。A liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)was developed for rapid screening and confirmation of florfenicol and flufenicol-amide drugs residues in egg.The samples were extracted by 2%ammonia ethyl acetate,purified with C_(18) powder,and then separated on an Waters HSS T3(10mm×2.1mm,1.8μm)column using a binary solvent system composed of 0.01%formic acid aqueous solution and acetonitrile solution by gradient elution.The target compounds were ionized in the electrospray ionization and simultaneously operated in positive and negative ionization mode,quantitatived in internal standard method.Under the optimal conditions,the two analytes were separated well,with good linearity in quantitative range ofo.Ito10 ng·mL^(-1),and limits of detection(LOD)of 0.6μg·kg^(-1).Recoveries for the compounds in eggs mainly ranged from 89.1%to 109.6%,with relative standard deviations(RSD)of 4.4%to 15.3%.Compared with traditional detection methods,this method eliminated the cumbersome pre-treatment steps,and had the advantages of fast analysis speed,high efficiency and good sensitivity.It would open a new standard detection technology for simultaneous detection of flufenicol and flufenicol-amide in eggs.

关 键 词：鸡蛋 氟苯尼考 氟苯尼考胺 液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学]