液相色谱串联质谱法在检测鸡肉和鸡蛋中氯霉素残留的应用

Determination of the residues of chloramphenicols in chicken and eggs by high performance liquid chromatography-tandem mass spectrometry

建立了鸡肉、鸡肝和鸡蛋中氯霉素的高效液相色谱串联质谱测定方法,试样经三氯乙酸除蛋白及乙酸乙酯液液萃取提取和净化后,C18柱HPLC进行分离,多反应选择离子检测。方法的回收率和变异系数分别在80%~110%和8%~10%。该方法对鸡肉中氯霉素检测限为0.1μg/kg。

A high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） method was developed for the quantitative determination of chloramphenicols respectively in the chicken and liver of chicken and eggs. The chloramphenicols in eggs were deproteinated with acetocaustin acid and acetic ether followed by liquid-liquid extraction.Further clean-up was performed by solid phase extraction（SPE） through mixed mode columns（PEP SPE）.The separation of the compounds was carried on a Agilent Eclipse Plus C18 column（C18, 3.5 μm×100 mm×2.1 mm（id） by a gradient elution using acetonitrile and 0.1% formic acid as mobile phases.The analytes were detected by tandem mass spectrometry in multiple reaction monitoring（MRM） mode with negative electrospray ionization.The chloramphenicols quantified by internal standard method.The linear ranges were 0.1~20. 0 μg/L and the correlation coefficients were not less than 0.9995.The average recoveries and relative standard deviations ranged from80%-110% and 8%~10% respectively at the spiked levels of 0.1,0.2 and 1.0 μg/kg for the both markers. The limit of quantitation（LOQ） was 0.1 μg /kg.The method is sensitive,accurate and suitable for the determination and confirmation of chloramphenicols in chicken and eggs.