液相色谱-串联质谱法测定鸡肉中氯霉素残留

Determination of Chloramphenicol in chicken by HPLC-MS/MS

目的:建立鸡肉中氯霉素残留量检测的高效液相色谱-串联质谱法。方法:液相色谱条件:采用krom asil C18(250 mm×4.6 mm,5μm)色谱柱,流动相:甲醇+水(50+50),流速:0.8 m l/m in,柱温35℃,进样量10μl。质谱条件:电喷雾离子源,负离子模式,MRM模式扫描,以氘代氯霉素为内标定量。结果:氯霉素在0.05 ng/m l^2.0 ng/m l范围内线性关系良好(r=0.9999),方法检出限为0.1μg/kg,0.1μg/kg、0.2μg/kg、1.0μg/kg三个添加浓度检测结果平均回收率为90%~108%,批内RSD均小于10%(n=3)。结论:本操作简单,灵敏度高,可用于鸡肉中氯霉素残留的测定。

Objective：To establish a liquid chromatography-tandem mass spectrometric method（LC-MS/MS） for the determination of chloramphenicol in chicken.Methods： HPLC condition： the chromatography column was kromasil C18 column（250 mm×4.6 mm,5 μm）,the mobile phase was methanol and water（1∶ 1,V/V）,and the column temperature was 35℃,flow rate was 0.8 ml/min,injection volume was 10 μl.Mass spectrometry condition： ESI-and MRM mode,used deuterium-labelled chloramphenicol as internal standard.Results： Calibration curve was linear in the range from 0.05 ng/ml^2.0 ng/ml with a correlation coefficient of 0.9999,and the detection limit of the method was 0.1 μg/kg.The average recoveries at the three concentrations of 0.1 μg/kg,0.2 μg/kg,1.0 μg/kg ranged from 90%~108%,and the intra-batch variation coefficients were less than 10%（n=3）.Conclusion： The method is a simple,sensitive and specific assay for the quantitative determination of chloramphenicol in chichen.