和乳粉中四环素类药物残留.PDFVIP

※分析检测 Journal of Dairy Science and Technology 2018, Vol.41 No.5 16 超高效液相色谱-串联质谱法测定牛乳、发酵乳 和乳粉中四环素类药物残留 段国霞，张立佳，吕志勇，莫 楠，谢瑞龙，刘丽君，李翠枝，胡 雪* （内蒙古伊利实业集团股份有限公司，内蒙古呼和浩特 010110 ） 摘  要：建立超高效液相色谱- 串联质谱法同时检测牛乳、发酵乳和乳粉3 种基质中4 种四环素类药物残留的检测 方法。对前处理方法和仪器上机条件进行研究。以EDTA-Mcllvaine缓冲液进行提取，经HLB 固相萃取柱净化，甲 / V V 醇- 乙酸乙酯（1∶9 ， ）洗脱，氮吹后复溶，采用电喷雾离子源正离子模式、多反应监测模式进行检测。结果表 μ / 明：乳粉中四环素、土霉素、金霉素和强力霉素的定量限均为10 g kg ；液态乳和发酵乳中4 种药物的定量限均为 2 μg/kg ；四环素类药物添加量为2～100 μg/kg时，回收率为63.1%～100.6%，相对标准偏差为1.8%～10.7%，基质效 应为100.5%～122.1% 。该方法准确、快速、灵敏度高、重复性好、线性范围宽，适用于液态乳、发酵乳和乳粉中 4 种四环素类药物残留的测定。 关键词：超高效液相色谱- 串联质谱；四环素类药物；兽药残留；牛乳；乳粉 Quantitative Determination of Tetracycline Residues in Milk, Fermented Milk and Milk Powder by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry DUAN Guoxia, ZHANG Lijia, LÜ Zhiyong, MO Nan, XIE Ruilong, LIU Lijun, LI Cuizhi, HU Xue* (Inner Mongolia Yili Industrial Group Co. Ltd., Hohhot 010110, China) Abstract: An ultra performance liquid chromatography-tandem mass spectrometry method for the simultaneous quantitative determination of four tetracycline residues in dairy products, including milk, yogurt and milk powder, has been established. In this method, the pretreatment and instrument operating conditions were optimized. Tetracycline residues were extracted into EDTA-Mcllvaine buffer and then cleaned up by an HLB solid-phase V V extraction cartridge. After the residues were elut