QuEChERS-超高效液相色谱-串联质谱技术同时测定乳制品中磺胺类和喹诺酮类抗生素残留  

Determination of sulfonamides and quinolones in milk by QuEChERS and ultra performance liquid chromatography-tandem mass spectrometry

作　　者：曹慧[1,2] 陈小珍 朱岩[2] 李祖光[3] 武晓光 祝颖 

机构地区：[1]浙江省质量检测科学研究院,杭州310013 [2]浙江大学化学系,杭州310012 [3]浙江工业大学化学工程与材料学院,杭州310014

出　　处：《食品科技》2013年第6期323-329,共7页Food Science and Technology

基　　金：浙江省科技厅分析测试科技计划项目(2011C37072);浙江省质量技术监督系统科研计划项目(20110203)

摘　　要：采用QuEChERS-超高效液相色谱-串联质谱技术同时测定乳制品中磺胺类和喹诺酮类抗生素残留。样品加乙腈提取,经分散固相萃取净化后,采用WatersC18色谱柱分离,以乙腈和0.1%的甲酸水溶液为流动相进行梯度洗脱,采用电喷雾-正离子多反应监测模式,内标法定量。在1～200μg/L的质量浓度范围内,磺胺类和喹诺酮类抗生素的相关系数均大于0.9965,该方法的检出限在0.3～2.5μg/kg之间,定量限在1.0～7.5μg/kg之间。添加10、20、50μg/kg3个浓度水平,磺胺类和喹诺酮类抗生素的平均回收率在71.6%～120.7%之间,相对标准偏差在0.1%～7.2%之间。将该技术应用于市售多种类乳制品的测试,结果表明,该方法简便、快速、灵敏度高,适用于乳制品中磺胺类和喹诺酮类抗生素残留的同时测定。A method was established for determining sulfonamides and quinolones residues in milk by QuEChERS and ultra performance liquid chromatography-tandem mass spectrometry （UPLC/MS/MS） with isotopes dilution. The analytes were extracted with acetonitrile and cleaned up with dispersive- solid phase extraction. The target analytes were separated by Waters C18 column with gradient elution using acetonitrile and 0.1% formate in water as mobile phases. The analytes were detected by tandem quadrupole mass spectrometry after positive electrospray ionization by multiple reaction monitoring （MRM）. Internal standard method was used to determine the results. In the linear range （1~200 μg/L） of each antibiotics, the correlation coefficient was greater than 0.9965 for each analytes. The limit of detection （LOD） were 0.3-2.5 μg/kg, and the limit of quantitation （LOQ） were 1.0-7.5 μg/kg. The mean recoveries at the three spiked levels of 10-50 μg/kg were 71.6%~120.7%. The relative standard deviation （RSD） were 0.1%-7.2%. The proposed method was successfully applied to the analysis of real samples. The simplicity, sensitivity and good precision of the method made it be well suitable for determination of sulifonamides and quinolones residues in milk.

关 键 词：QUECHERS 超高效液相色谱-串联质谱 磺胺 喹诺酮 残留 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]