SPE—UPLC—MS／MS法测定生鲜乳中舒巴坦残留  

Determination of Sulactam Residues in Milk by SPE-UPLC-MS/MS

作　　者：孙涛[1] 陈贺[1] 宋斌[1] 赵子刚[1] 古丽斯坦[1] 刘圣红[1] 安静[1] 王成[1] 

机构地区：[1]新疆农业科学院农业质量标准与检测技术研究所/农业部农产品质量安全风险评估实验室,乌鲁木齐/新疆农产品质量安全实验室新疆乌鲁木齐830091

出　　处：《现代科学仪器》2016年第3期64-67,共4页Modern Scientific Instruments

基　　金：自治区公益性科研院所基本科研项目（KY2015080）;2016年生鲜乳质量安全风险评估项目

摘　　要：摘要本试验应用固相萃取技术（SPE），结合超高效液相色谱-串联质谱联用仪（UPLC—MS／MS），建立了快速测定生鲜礼中舒巴坦残留量的方法。生鲜乳样品经乙腈提取，OaissPgiMEHLB固相萃取小柱净化后，以50％乙腈水溶液为流动相，Waters Hilic色谱柱进行分离；多反应监测模式，外标法进行定量。结果发现：方法回收率在73．8％～93．5％之间；相对标准偏差（n=3）范围为1．5％～5．3％；线性范围为0．1～1．0mg／L；舒巴坦检出限为1．5×10-2mg／kg。表明该方法专属性强、灵敏度高，适用于生鲜乳中舒巴坦残留量的测定。This paper developed a SPE-UPLC-MS/MS method for the determination of sulactam residues in milk. Sulactam was extracted with acetonitrile, and cleaned up with PRIME HLB cartridge. The UPLC analyses was performed on an Acquity UPLC Hilic column with gradient elution using acetonitrile and water（50：50） as mobile phase. The mass spectrometric acquisitions were carried out by means of multiple reaction monitoring（MRM） in electrospray negative ionization mode. Resulting in the average recoveries of sulactam ranged from 73.8% to 93.5%, with the relative standard deviation from 1.5% to 5.3%, the calibration curve was liner from 0.01 to 1.0mg/L, the detection limits of sulactam was 15μg/kg and the limit of quantitation was 50 pg/kg. The results showed that this method had specific, sensitive and suitable for determination on sulactam in the milk.

关 键 词：固相萃取 超高效液相色谱-串联质谱 生鲜乳 舒巴坦 

分 类 号：O657.63[理学—分析化学]