dd液相色谱-电喷雾串联四极杆质谱法检测.pdfVIP

液相色谱- 电喷雾串联四极杆质谱法检测 牛奶中磺胺类抗生素的残留 丁梨慧 邵双良 任一平 浙江省疾病预防控制中心 浙江省食品安全重点实验室 中国浙江省杭州 310009 【摘要】 本文采用液相色谱- 电喷雾串联四极杆质谱仪，用多离子反应监测 （MRM ）定量 法检测牛奶中的磺胺类抗生素。牛奶样品液液萃取、SPE 净化去除蛋白质等杂质，在反相 HLB 柱上用甲醇和乙酸乙酯作为淋洗剂，吹干后，在优化的色谱条件和质谱参数等条件下 进行方法学验证，建立了定量检测牛奶中的23 种磺胺类抗生素的方法。该方法的检出限在 2 0.07~3.2 ng/ml 之间，在 1~200 ng/ml 的线性范围中，相关系数 r 0.99 ，回收率在 50.56%~ 114.85% 之间。该方法去除了蛋白质干扰、灵敏度高，为牛奶中磺胺类抗生素检测 的实用方法。 关键词：HPLC-MS/MS ，磺胺类抗生素， 牛奶 Simultaneous Determination of Sulfa Antibiotics Residue in Milk by Liquid Chromatography Tandem Mass Spectrometry Ding Lihui Shao Shuangliang Ren Yiping Zhejiang Provincial Center for Disease Prevention and Control ，Hangzhou 310009 Abstract A HPLC-MS/MS method was developed for the simultaneous determination of 23 sulfa antibiotics residue in milk. Isotope dilution method was used for the quantification of sulfa antibiotics. For clean-up and concentration solid phase extraction (SPE) with OASIS HLB cartridges were used. LC analysis was performed on a Capcell Pak C ( 150 ⅹ2.0mm I.D., 5µm) 8 column, acidified water and acidified methanol was used as mobile phase. The detection limits (LOD) for 23 sulfa antibiotics residue were between 0.07% and 3.2%. The linear range was from 1 to 200 ng/mL with correlation coefficients above 0.99. The mean recoveries were between 50.56% and 114.85%. This method was an valid method for the determination of sulfa antibiotics residue in milk for the eliminating of disturbance of protein and its high sensitivity. Keywords HPLC-MS/MS, sulfa antibiotics ， milk 绪 论 两性磺胺类化合物被广泛运用于畜牧产业中,作为有效的抗生素