Determination of Six Kinds of Antibiotic Residues in Eggs by High Performance Liquid Chromatography-Tandem Mass Spectrometry
A high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the fast detection of six antibiotic residues in eggs. Samples were extracted with acetonitrile, 1% formic acid acetonitrile and 80% acetonitrile water (containing 1% formic acid) respectively. The extract was dried by nitrogen at 40 ℃ and then redissolved with 50% acetonitrile water (containing 0.1% formic acid) solution. The samples were separated by C18 column and monitored by Tandem mass spectrometry with electrospray ion in positive and negative ion multi-reaction monitoring mode. The results showed that the recoveries of six antibiotics were higher when 80% acetonitrile water (containing 1% formic acid) was used as extraction solvent. Metronidazole, enrofloxacin, ciprofloxacin, tilmicosin and florfenicol showed a good linear relationship between mass concentration and peak area in the mass fraction range of 0.4 ~ 20.0 μg·kg-1, and amoxicillin in the mass fraction range of 4 ~ 200 μg·kg-1, with r > 0.998. The detection limits were between 0.1 μg·kg-1 and 2.0 μg·kg-1. The recoveries were ranged from 85.3% to 115.0% with the relative standard deviations of 1.5% ~ 4.0% when the spiked levels of metronidazole, enrofloxacin, ciprofloxacin, tilmicosin and florfenicol were 2, 5 and 10 μg·kg-1, and the spiked levels of amoxicillin was 10, 20 and 50 μg·kg-1. The proposed method is simple, fast, low-cost, accurate and reliable,which is suitable for rapid determine of various antibiotics in eggs.
Ultra performance liquid chromatography-tandem mass spectrometryAntibioticsEggs