液相色谱-串联质谱法测定动物性食品中20种抗生素类药物残留

DETERMINATION OF 20 KINDS OF ANTIBIOTICS RESIDUES IN ANIMAL DERIVED FOOD BY LC-MS/MS

建立了一种专属、灵敏的方法用于同时检测动物性食品中β-内酰胺类青霉素类抗生素、大环内酯类抗生素、四环族抗生素和林可胺类共20种抗生素药物残留。首先对动物性食品中的抗生素类药物进行提取,再经HLB固相萃取柱净化,采用电喷雾离子源,以正离子检测方式进行质谱分析。实验结果表明,在10～200μg/L质量浓度范围内上述20种抗生素类药物浓度与峰面积均呈线性,相关系数r>0.99。在低、中、高3个质量浓度添加水平下,20种抗生素类药物的平均回收率为73.6%～114.6%,相对标准偏差为1.1%～12.0%(n=5)。20种抗生素类药物的定量限为0.5～10μg/kg。

A specific, sensitive method for detecting the residues about 20 kinds of β-1actam antibiotics in animal derived food was established. These antibiotics were β-lactam antibiotics, macrolide antibiotics, tetracycline antibiotics and Lincosamide antibiotics. First, antibiotics in animal foods were extracted, then purified by HLB solid phase extraction cartridges. Electro spray ionization and mass spectrometer were used to analyse these antibiotics by using positive ion. The experimental results showed that the 20 kinds of antibiotics had linearity as the concentrations in the range of 10 - 200μg/L with the correlation coefficient more than 0. 99. These 20 kinds of antibiotics were added in low, medium and high concentration, the average recoveries were 73.6% -114.6% and relative standard deviation was 1.1% - 12.0% （ n = 5 ）. The detection limits of 20 kinds of antibiotics were 0.5 - 10 μg/kg.