鸽蛋中氯霉素甲砜霉素氟苯尼考及其代谢物氟苯尼考胺同时检测的超高效液相色谱-串联质谱法的建立  

Simultaneous determination of chloramphenicol,thiamphenicol,florfenicol and its metabolite florfenicol amine in pigeon eggs by UPLC-ESI/MS/MS

作　　者：王波 赵霞[2,3] 谢恺舟 王雅娟[2,3] 郭亚文 卜晓娜[2,3] 刘楚君 张跟喜[2,3] 张涛 刘学忠[1,2] WANG Bo;ZHAO Xia;XIE Kai-zhou;WANG Ya-juan;GUO Ya-wen;BU Xiao-na;LIU Chu-jun;ZHANG Gen-xi;ZHANG Tao;LIU Xue-zhong(College of Veterinan Medicine,Yangzhou University,Yangzhou 225009,China;Joint International Research Laboratory of Ariculture & Agri-Product Scifety of the Ministry of Educalion,Yangzhou 225009,China;College of Animal Science and Technology,Yangzhou Unirersity,Yangzhou 225009,China)

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

出　　处：《中国兽医科学》2019年第3期393-402,共10页Chinese Veterinary Science

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(PAPD);2017年农业行业标准制定和修订项目[农财项函(2017)15号];扬州大学"高端人才支持计划"项目(201801);江苏省农业科技自主创新基金项目[CX(18)3022]

摘　　要：为建立同时检测鸽蛋中氯霉素(CAP)、甲砜霉素(TAP)、氟苯尼考(FF)及其代谢物氟苯尼考胺(FFA)多残留的超高效液相色谱-串联质谱(UPLC-MS/MS)法,将样品经过液-液萃取(LLE)或者加速溶剂萃取(ASE)提取、净化,采用电喷雾离子源(ESI)模式和多反应监测模式(MRM),通过UPLC-MS/MS检测和确证分析。结果显示,CAP、TAP、FF和FFA添加水平分别为定量限(LOQ),0.5、1.0和2.0倍的最低要求执行限量(MRPL)或最高残留限量(MRL)时,平均回收率在91.55%～105.47%范围内,相对标准偏差(RSD)均低于3.04%,日内RSD为1.83%～3.70%,日间RSD为2.72%～4.62%。CAP、TAP、FF和FFA在鸽蛋中的检测限(LODs)为0.03～0.4ug/kg(S/N≥3),LOQs为0.08～1.2ug/kg(S/N≥10),其显著低于最大残留限量(MRL)。结果表明,此方法快速、准确、灵敏度高,定性、定量准确,适用于鸽蛋中氯霉素、甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺多残留的检测。A widely applicable method involving ultra-performance liquid chromatography-electrospray ionization tandem triple quadrupole mass spectrometry(UPLC-ESI/MS/MS)was developed for the simultaneous determination of chloramphenicol(CAP),thiamphenicol(TAP),florfenicol(FF)and florfenicol amine(FFA)in pigeon eggs.Samples was extracted and purified by liquid-liquid extraction(LLE)or accelerated solvent extraction(ASE),using ESI mode and multiple reaction monitoring mode(MRM)by UPLC-MS/MS detection and confirmation analysis.When the added concentration of CAP,TAP,FF and FFA were the limit of quantification(LOQ),0.5,1.0 and 2.0 times of the minimum required performance limit(MRPL)or maximum residue limit(MRL),respectively,the average recoveries of the four analytes from pigeon egg samples were from 91.55%to 105.47%,with relative standard deviations(RSDs)of less than 3.04%.The intra-day RSD values were from 1.83%to 3.70%,and the inter-day RSD values were from 2.72%to 4.62%.Limits of detection(LODs)were from 0.03 to 0.4 ug/kg(S/N≥3)for CAP,TAP,FF and FFA in pigeon eggs,and LOQs were from 0.08 to 1.2 ug/kg(S/N≥10),these values were significantly below the maximum residue limit(MRL).In conclusion,the method is rapid,accurate,sensitive,accurate qualitative and quantitative,which is suitable for multi-residue detection of chloramphenicol,thiamphenicol,florfenicol and its metabolite florfenicol amine in pigeon eggs.

关 键 词：氯霉素类药物 氟苯尼考胺 鸽蛋 超高效液相色谱-串联质谱 

分 类 号：S859.796[农业科学—临床兽医学]