QuEChERS-超高效液相色谱-串联三重四极杆质谱联用法快速测定羊肉中氯霉素、甲砜霉素、氟苯尼考的残留量  

Rapid Determination of Chloramphenicol, Thiamphenicol and Florfenicol Residues in Mutton by QuEChERS-UPLC-MS/MS

作　　者：杜春艳 吴发旺 赖淼菊 吴劲竹 曹渟渟 邹晓莉[4] DU Chun-yan;WU Fa-wang;LAI Miao-ju;WU Jing-zhu;CAO Ting-ting;ZOU Xiao-li(Bijie Medical College,Bijie 551700,China;Bijie Center for Disease Control and Prevention,Bijie 551700,China;Putuo District Center for Disease Control and Prevention,Shanghai 200333,China;West China School of Public Health,Sichuan University,Chengdu 610000,China)

机构地区：[1]毕节医学高等专科学校,贵州毕节551700 [2]毕节市疾病预防控制中心,贵州毕节551700 [3]上海市普陀区疾病预防控制中心,上海普陀200333 [4]四川大学华西公共卫生学院,四川成都610000

出　　处：《食品与药品》2024年第3期199-205,共7页Food and Drug

基　　金：2021年毕节市科学技术局毕节医学高等专科学校科学技术联合基金项目(编号:毕科联合字yz〔2021〕4号)。

摘　　要：目的建立QuEChERS-超高效液相色谱-串联三重四极杆质谱法测定羊肉中氯霉素、甲砜霉素、氟苯尼考残留量的分析方法。方法样品经研磨机匀浆后用乙腈提取,提取液经QuEChERS-1010,QuEChERS-0101净化,采用电喷雾负离子扫描,多反应监测模式,内标法定量。结果氯霉素、甲砜霉素、氟苯尼考在4~50μg/L范围内具有良好的线性关系,相关系数均大于0.998,3种药物在5.0,10.0,30.0μg/kg浓度水平加标回收率在93.17%~109.91%范围内,相对标准偏差(RSD)为2.33%~6.14%。方法的检出限为0.01~0.03μg/kg,定量限为0.02~0.09μg/kg。结论该方法具有操作简单,准确度和灵敏度高等特点,满足测定羊肉中氯霉素、甲砜霉素、氟苯尼考残留量的检测要求。Objective To establish an analytical method for the determination of chloramphenicol,thiamphenicol and florfenicol residues in mutton by QuEChERS-ultra performance liquid chromatography-tandem triple quadrupole mass spectrometry(QuEChERS-UPLC-MS/MS).Methods The samples were homogenized by a grinder and extracted with acetonitrile.The extract was purified by QuEChERS-1010 and QuEChERS-0101,determined by UPLC-MS/MS and quantified by internal standard method.For detection,electrospray negative ion scanning and multiple reaction monitoring were adopted.Results Chloramphenicol,thiamphenicol and florfenicol showed good linear relationships in the range of 4-50μg/L,with correlation coefficients above 0.998.At the concentrations of 5.0,10.0,30.0μg/kg,the recoveries of three drugs were in the range of 93.17%-109.91%,and the relative standard deviations(RSDs)ranged from 2.33%to 6.14%.The limits of detection of the method were 0.01-0.03μg/kg,and the limits of quantification were 0.02-0.09μg/kg.Conclusion This method is simple,rapid,accurate and sensitive,and meets the detection requirements for the determination of chloramphenicol,thiamphenicol and florfenicol residues in mutton.

关 键 词：羊肉 氯霉素 甲砜霉素 氟苯尼考 QuEChERS-超高效液相色谱串联三重四极质谱法 

分 类 号：O657.63[理学—分析化学] TS207[理学—化学]