超高效液相色谱-串联质谱法测定奶粉中聚醚类抗生素残留

Determination of Polyether Antibiotics Residues in Milk Powder by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立了检测奶粉中聚醚类抗生素(马杜霉素铵、尼日利亚菌素、拉沙洛菌素、莫能菌素、甲基盐霉素、盐霉素)残留量的超高效液相色谱-串联质谱分析方法,样品在乙腈溶液提取下经PRIME HLB固相萃取柱净化,氮吹浓缩后定容过膜上机检测。6种聚醚类抗生素在0.2~16.0 ng/L线性范围内均呈线性,相关系数均大于0.999,方法检出限均低于1.6μg/kg,满足国家标准要求,在空白样品中添加6种聚醚类抗生素的回收率均在74.1%~111.9%之间,精密度(RSD)1.9%~14.6%。

A sensitive and selective method was developed for the determination of Polyether antibiotics(maduramicin ammonium、nigericin、lasalocid,monensin,narasin,salinomycin)residues in milk powder.The samples were purified by PRIME HLB solid phase extraction column under the extraction of acetonitrile.After drying and concentrating,the samples were reused and were tested over the membrane.The calibration curves were good linear between area and the concentration of polyether antibiotics from 0.2~16.0 ng/L with the correlation coefficient over 0.999.The methods detection limit was lower than 1.6 g/kg,which met the requirements of national standard.The recoveries from milk powder at the three concentrations of 1.6,3.2,16μg/kg range from 74.1%~111.9%,with relatives standard deviation from 1.9%~14.6%.