超高效液相色谱-串联质谱法快速测定禽蛋中氯霉素、氟苯尼考及其代谢物残留

Rapid Determination of Chloramphenicol,Florfenicol and Its Metabolites in Poultry Eggs by UPLC-MS/MS

建立了快速测定禽蛋中氯霉素、氟苯尼考及氟苯尼考胺的超高效液相色谱-串联质谱分析方法。禽蛋用乙腈提取后,正己烷液液萃取除脂,浓缩后超高效液相色谱分离,以乙腈和10%甲醇水为流动相进行梯度洗脱,MRM反应监测模式检测。结果表明在5~200μg/L的系列浓度范围内均呈良好线性关系,相关系数均大于0.999。氯霉素、氟苯尼考、氟苯尼考胺的检测限为0.5μg/kg,定量限为2.0μg/kg,在2~20μg/kg添加浓度范围内平均回收率为60%~100%,精密度小于20%。该方法方便快捷、定性准确,适于禽蛋中的氯霉素、氟苯尼考及氟苯尼考胺药物残留检测。

A UPLC - MS / MS method was developed and established to rapidly determine chloramphenicol,florfenicol and florfenicol-amine in poultry eggs. The eggs were extracted with acetonitrile and then separated byn-hexane liquid. After enrichment, the samples were separated by UPLC, elutedwith acetonitrile and 10% methanolas the mobile phase and the MRM reaction was monitored. The results showed that there was a good linearity in therange of 5 ～ 200 μg / L , and the correlation coefficients were more than 0. 999. The detection limit of thechloramphenicol, florfenicol and florfenicol-amine was 0.5 μg / kg, and the limit of quantification was 2 μg / kg.The average recoveries were 60%～100% in the range of from 2 μg / kg to 20 μg / kg, and the precision was lessthan 20%. The method was convenient, rapid, accurate and it was suitable for the detection of chloramphenicol inpoultry eggs.