QuEChERS结合液相色谱-串联质谱法快速测定奶酪中多类兽药残留  

Multi-residue determination of veterinary drugs in cheese by QuEChERS and liquid chromatography-tandem mass spectrometry

作　　者：曹亚飞[1,2] 康健[2,3] 常巧英[2,3] 胡雪艳[2] 王志斌[2,3] 范春林[2] 王明林[1] 

机构地区：[1]山东农业大学食品科学与工程学院,山东泰安271018 [2]中国检验检疫科学研究院,北京100123 [3]燕山大学环境与化学工程学院,河北秦皇岛066004

出　　处：《色谱》2015年第2期132-139,共8页Chinese Journal of Chromatography

基　　金："十二五"国家科技支撑项目(2012BAD29B01)

摘　　要：建立了一种快速测定奶酪中大环内酯类、磺胺类、喹诺酮类和四环素类共50种兽药残留的分析方法。方法采用改进后的QuEChERS对奶酪进行前处理。样品在加入Na2EDTA缓冲液和陶瓷均质子后，在5锸（v／v）醋酸乙腈条件下进行振荡提取，氯化钠和无水硫酸钠用于盐析，经C18吸附剂净化后，供液相色谱-串联质谱（LC—MS／MS）测定。目标化合物经ZORBAX—SB—C18柱梯度分离，在正离子动态多反应监测模式下进行检测。结果表明，奶酪中50种兽药的定量限（LOQ）为0．05—20μg／kg；在3个添加浓度（20、50、100μg／kg）下（n=6），平均回收率在70％-120％范围内的比例分别为94％、92％和96％，相对标准偏差（RSD）为1％-14％。对市售的7个样品进行测定，其中两个样品分别检出了微量的罗红霉素和氟甲喹兽药残留。该方法快速简便，适用于奶酪中兽药残留的快速检测和日常监控。A rapid and sensitive method has been developed for the simultaneous determination of 50 veterinary drugs （including macrolides, quinolones, sulfonamides, and tetracyclines） in cheese using a modified QuEChERS method coupled with liquid chromatography-tandem mass spectrometry （LC-MS/MS）, After adding Na：EDTA buffer solution and ceramic homogenizer, the cheese sample was extracted by 5% （v/v） acetic acid-acetonitrile, sodium chloride and anhydrous sodium sulfate were used for salting-out process. The resulting supernatant solution was purified by C18 sorbent and the re-dissolved solution was analyzed by LC-MS/MS under dynamic multi-reaction monitoring （dynamic MRM） mode via positive electrospray ionization with a ZORBAX-SB-C18 column. The limits of quantification （ LOQ, S/N= 10） of the target com- pounds ranged from 0.05 μg/kg to 20μg/kg in cheese. At spiked levels of 20, 50, 100 μg/kg （n= 6）, the percentages of drug with a recovery between 70% and 120% were 94%, 92%, and 96%, respectively. The relative standard deviations （RSDs） were between 1% and 14%. This method has been applied to determine seven real samples from markets. Roxithromycin andflumequine have been detected in two samples separately. The simple, rapid and accurate method is suitable for the detection in cheese. results demonstrated that this of multi-class veterinary drugsin cheese.

关 键 词：QUECHERS 液相色谱-串联质谱 兽药 奶酪 多残留 

分 类 号：O658[理学—分析化学]