摘要
建立了牛奶和奶粉中β-内酰胺类头孢族,喹诺酮类和大环内酯类20种抗生素残留的超高效液相色谱-二极管阵列检测器测定的方法。采用0.5 mol/LHClO4沉淀牛奶或奶粉中的蛋白质成分后,样品用乙腈+水(2+8,V/V)提取,HLB固相萃取小柱净化,以含有2 g/L甲酸的乙腈和0.006 mol/L乙酸铵为流动相,BEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,UPLC-PDA进行测定。方法的检出限和定量限分别为8～60μg/kg和25～200μg/kg。对于0.5～1.5倍最大允许限量加标水平的样品回收率为48.6%～91.2%,RSD为2.3%～13%。
An ultra performance liquid chromatographic method for the simultaneous determination of 20 antibiotic including cephalosporins,quinolones and macrolides in milk and powdered milk samples was established.After precipitating protein with 0.5 mol/L perchloric acid,the samples of milk or powdered milk were extracted with acetonitrile and water（8＋2）.The extract was cleaned up with HLB cartridge and the chromatographic operating conditions were on a BEH C18 column（50 mm×2.1 mm i.d.,1.7μm）,acetonitrile（containing 0.2% formic acid）-0.006 mol/L ammonium acetate as mobile phase at a flow rate of 0.4 mL/min.The LODs of milk and powdered milk samples were in the ranges of 8～60μg/kg and the LOQs were in the ranges of 25～200μg/kg at a S/N of 10.The intra-assay precisions were in the ranges of 2.3%～13% and spiked recoveries of ten antibiotics were 48.6%～91.2%.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第6期23-27,共5页
Chinese Journal of Analysis Laboratory
基金
四川省卫生厅课题(07326)
四川省医学重点实验室项目资助
关键词
牛奶
奶粉
抗生素残留
固相萃取
超高效液相色谱
Milk
Powdered milk
Antibiotic residues
Solid phase extraction
Ultra performance liquid chromatography
