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建立高效液相色谱-电喷雾串联质谱法检测牛奶中土霉素、四环素及金霉素残留的分析方法。采用酸化乙腈提取样品并沉淀蛋白,离心、浓缩、正己烷脱脂,经Agilent ZOBAX SB-C18柱分离,以0.1%甲酸-乙腈对待测成分进行梯度洗脱。采用高效液相色谱-串联质谱多反应监测正离子模式检测,外标法定量。结果表明,3种抗生素浓度在50~1 000μg/L范围内线性关系良好,方法定量限(LOQ,S/N=10)为15~25μg/kg,检出限(LOD,S/N=3)为8~15μg/kg,加标回收率为79.6%~88.7%,相对标准偏差为3.2%~6.0%。该方法前处理简单、可靠,灵敏度高,适用于牛奶中四环素类抗生素残留的快速测定。
To establish a method for the determination of oxytetracycline, tetracycline and chlortetracycline residues in milk by high performance liquid chromatography-electrospray ionization tandem mass spectrometry. Samples were extracted with acidified acetonitrile and the protein was precipitated, centrifuged, concentrated and defatted with n-hexane. The residue was separated on an Agilent ZOBAX SB-C18 column and the fractions eluted with 0.1% formic acid-acetonitrile. High performance liquid chromatography - tandem mass spectrometry multiple reaction monitoring positive ion mode detection, external standard quantitative. The results showed that the linear range of the three antibiotics was in the range of 50-1 000 μg / L. The limit of quantification (LOQ, S / N = 10) was 15-25 μg / kg and the limit of detection (LOD, S / N = 3 ) Was 8 ~ 15μg / kg, the recoveries were 79.6% ~ 88.7% with relative standard deviations of 3.2% ~ 6.0%. The method has the advantages of simple, reliable pretreatment, high sensitivity and is suitable for the rapid determination of tetracycline antibiotic residues in milk.