建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定牛奶中5类(磺胺类、喹诺酮类、四环素类、氯霉素类和大环内酯类)38种抗生素的分析方法。牛奶样品以0.5%(体积分数)甲酸乙腈提取,利用Oasis PRiME HLB固相萃取小柱进行净化,经Acquity UPLC HSS T3柱(100 mm×2.1 mm i.d.
An analytical method was developed for the simultaneous determination of 38 antibiotics residues in 5 classes of drugs
including sulfonamides
quinolones
tetracyclines
chloramphenicols and macrolides in milk by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile containing 0.5%(by volume) formic acid
and cleaned up with an Oasis PRiME HLB solid phase extraction column.The target components were separated using an Acquity UPLC HSS T3 column(100 mm×2.1 mm i.d.
1.8 μm)
then identified and quantified by UPLC-MS/MS with electrospray ion source(ESI) under multi-reaction ion monitoring(MRM) mode.Results showed that 38 antibiotics had good linear relationships in their respective linear ranges with correlation coefficients(r2) higher than 0.99.The limits of quantitation for 38 antibiotics were between 0.10 μg/kg and 1.0 μg/kg.Average recoveries for 38 antibiotics in milk at spiked levels of 1.0
5.0
10.0 μg/kg ranged from 70.7%to 94.9%
with relative standard deviations(RSD
n=6) of 4.0%-9.4%.With the advantages of easy operation
high sensitivity and good reproducibility
the method was applicable for the determination of antibiotics residues in milk.