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采用超高效液相色谱串联质谱建立了牛奶中14种β-内酰胺类抗生素残留检测方法。样品经过乙腈提取、氮吹、HLB柱净化后,经Acquity UPLC BEH Shield RP18(100 mm×2.1 mm,1.7μm)分离,以乙腈和体积分数0.02%甲酸溶液为流动相进行梯度洗脱,14种化合物在8 min内分离效果良好。方法的定量限均低于2.5μg/L,在2.5~250μg/L范围内线性良好,相关系数均在0.99以上;通过2,10,100μg/L 3个浓度的加标回收实验表明,回收率为73.2%~109.8%,RSD%为1.5%~12%,方法满足牛奶中β-内酰胺类抗生素药物残留检测要求。
High performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) was established for the determination of 14 β-lactam antibiotics residues in milk. The sample was separated by acetonitrile, extracted with acetonitrile and purified by HLB column, and then eluted with acetonitrile. The mobile phase consisted of acetonitrile and 0.02% formic acid as mobile phase and 14 Compounds separated well in 8 min. The limit of quantification of the method was less than 2.5μg / L, and the linearity was good in the range of 2.5 ~ 250μg / L with the correlation coefficients above 0.99. The recoveries of the two methods were 2, 10 and 100μg / L 73.2% ~ 109.8%, RSD% was 1.5% ~ 12%, the method to meet the requirements of milk β-lactam antibiotic drug residues detection.