LC-MS/MS를 이용한 축산물 중 클로람페니콜 잔류 분석법

Determination of chloramphenicol residues in food of animal origins using liquid chromatography-tandem mass spectrometry

A confirmatory method based on liquid chromatography/electrospray ionization tandem mass spectrometry (LC-MS/MS) was developed for the determination of the antibiotic chloramphenicol (CAP) in muscle of bovine, porcine, and chicken, milk, and chicken egg. CAP residues were extracted from all samples with ethyl acetate, via liquid-liquid extraction and concentrated by evaporation under nitrogen. The final dissolved extracts were analyzed by using a reversed-phase column and analyzed by electrospray negative mode tandem mass spectrometry. Mass spectral acquisition was done in the negative mode applying multiple reaction monitoring (MRM) of two diagnostic transition reactions for CAP (m/z 321→ 257 and m/z 321→152). Method validation was conducted through MRM LC-MS/MS analysis of negative control, fortified, and incurred samples. In the fortified samples the CAP was fully separated from all endogenous interferences of matrix. The limit of detection (LOD) and limit of quantification (LOQ) for CAP were 0.002 and 0.01 ng/g, respectively. Mean recoveries of CAP from samples spiked at levels of 0.15 to 0.6 ng/g were 86.5 % in bovine muscle, 87.7 % in porcine muscle, 84.7 % in chicken muscle, 87.0 % in chicken egg, and 76.2% in milk, respectively. The percent relative standard deviation for the described method was less than 9.0% over the range of concentrations studied.