超高效液相色谱-串联质谱法测定牛奶和奶粉中6种聚醚类抗生素残留量  

Determination of Six Polyether Antibiotics Residues in Milk and Milk Powder by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：薄海波 雒丽丽[2] 曹彦忠[3] 星玉秀[4] 庞国芳[3] 

机构地区：[1]青海出入境检验检疫局,西宁810000 [2]甘肃农业大学,兰州730070 [3]秦皇岛出入境检验检疫局,秦皇岛066002 [4]中国科学院西北高原生物研究所,西宁810008

出　　处：《分析化学》2009年第8期1161-1166,共6页Chinese Journal of Analytical Chemistry

基　　金：国家标准2007年第七批制修订计划项目(No.20079609-T-469)资助

摘　　要：建立了用于检测牛奶和奶粉中拉沙洛菌素、莫能菌素、尼日利亚菌素、盐霉素、甲基盐霉素和马杜霉素铵6种聚醚类抗生素残留量的超高效液相色谱-串联质谱分析方法。用乙腈提取样品中的聚醚类抗生素,提取液经HLB固相萃取柱净化,采用超高效液相色谱分离,以电喷雾离子源正离子多反应监测模式进行质谱分析。6种抗生素在0.5～100.0μg/L范围内均呈线性,相关系数r>0.99。在空白样品中添加6种聚醚类抗生素的回收率均在74.0%～98.5%之间;精密度(RSD)4.8%～17.2%。牛奶中6种聚醚类抗生素检出限均为0.2μg/L;奶粉中6种聚醚类抗生素检出限均为1.6μg/kg。A sensitive and seleetive method was developed for the determination of asalocid, monensin, nigericin, salinomycin, narasin and maduramiein ammonium residues in milk and milk powder. The polyether antibiotics in the test samples were extracted with acetonitrile. The extract was cleaned up with HLB solid phase extract column and analysis by ultra performance liquid chromatography-tandem mass spectrometry. Electrospray ionization was applied and operated in the positive ion mode. The calibration curves were good linear between area and the concentration of polyether antibiotics from 0. 5 - 100.0 μg/kg with the correlation coefficient over 0.99. The average recoveries from spiked milk and milk powder at the three concentrations of 0. 5, 10.0 and 20.0 mg/kg ranged from 74.0% to 98.5% with relative standard deviation from 4.8% to 17.2%. The limits of detection were 0. 2 μg/L and 1.6 μg/kg in milk and milk powder, respectively.

关 键 词：聚醚类抗生素 残留分析 超高效液相色谱-串联质谱 牛奶 奶粉 

分 类 号：TS252.7[轻工技术与工程—农产品加工及贮藏工程]