dd液相色谱-电喷雾串联四极杆质谱法检测dd液相色谱-电喷雾串联四极杆质谱法检测.pdf

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 0.07~3.2 ng/ml 之间，在 1~200 ng/ml 的线性范围中， 相关系数 r20.99 ， 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 C8 (150ⅹ2.0mm I.D., 5μm) 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,作为有效的抗生素在治疗细菌和原生动物 感染领域已占居重要地位。为了提高动物的抗病性，其也被广泛的应用于动物饲养的过程中， 从而造成了牛奶中抗生素的残留，危害人类健康。为进一步提高工作效率，近几年来，检测 者越来越注重多残留的同时检测。