过滤型固相萃取-超高效液相色谱/质谱法快速测定牛奶中喹诺酮及磺胺类药物  

Rapid determination of quinolone and sulfonamides in milk by filtration solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：王建凤[1,2] 杜振霞[1] 王颖[2] 曹沅[2] 马立利[2] 冯月超[2] 贾丽[2] 范筱京[2] WANG Jian-feng;DU Zhen-xia;WANG Ying;CAO Yuan;MA Li-li;FENG Yue-chao;JIA Li;FAN Xiao-jing(Analysis and Testing Center, Beijing University of Chemieal Teehnology, Beijing 100029;Beijing Center for Physieal and Chemical Analysis, Beijing Engineering Researeh Center of Food Safety Analysis, Beijing 100089)

机构地区：[1]北京化工大学分析测试中心,北京100029 [2]北京市理化分析测试中心北京市食品安全分析测试工程技术研究中心,北京100089

出　　处：《分析试验室》2018年第5期599-603,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了同时测定牛奶中喹诺酮和磺胺类药物的过滤型固相萃取-超高效液相色谱/串联质谱的分析方法。牛奶样本经酸化乙腈提取,分别通过过滤型固相萃取柱中性氧化铝和Prime HLB净化,BEH C_(18)色谱柱分离,0.2%的甲酸水溶液和甲醇梯度洗脱,电喷雾电离源电离,采用多反应监测模式检测,外标法定量。结果表明,33种药物在12 min内能够有效分离;线性范围1~100 ng/m L,相关系数(R^2)均大于等于0.994;在3个添加水平下,除磺胺喹恶啉外,其余物质的回收率为50.4%~116.4%,RSD小于16%;检出限0.01~0.5μg/kg;定量限0.05~2.0μg/kg。A method for the simultaneous determination of quinolones and sulfonamides in milk was developed by filtration solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry. The samples were extracted by acidified acetonitrile and purified by neutral alumina and Prime HLB solid phase extraction column. The separation was performed on an ACQUITY UPLC BEH C（18） column（ 50 mm × 2. 1 mm,1. 7 μm） by using 0. 2% formic acid solution and methanol as the mobile phases with gradient elution at a flow rate of 0. 2 m L/min. The electrospray ionization（ ESI） source was used in the multiple reaction monitoring（ MRM） mode,and the analytes were quantified with external standard curve. The good correlation coefficient of each compound was obtained in the concentration range of 1 ～ 100 ng/m L. The recoveries at three spiked levels were 50. 4% ～116. 4% with the relative standard deviation less than 16%. The limits of detection（ LOD） and limits of quantitation（ LOQ） for the analytes were in the range of 0. 01 ～ 0. 5 μg/kg and 0. 05 ～ 2. 0 μg/kg,respectively. The method is simple, rapid, reproducible and can be used for the simultaneous determining trace quinolones and sulfonamides in milk.

关 键 词：过滤型固相萃取 超高效液相色谱质谱 喹诺酮 磺胺 牛奶 

分 类 号：TS207.5[轻工技术与工程—食品科学]