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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
曾勇,董文婷,龚波,金灵,周青
0
(湖北省兽药监察所)
摘要:
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,再用正己烷液液分配除脂,浓缩后用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2.0 μg/kg,本方法在2μg/kg~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。
关键词:  禽蛋  氯霉素类药物  残留  超高效液相色谱-串联质谱
DOI:
投稿时间:2017-06-20修订日期:2017-11-20
基金项目:
Rapid Determination of Chloramphenicol,Florfenicol and its metabolites in poultry Eggs by UPLC-MS/MS
(Hubei Institute of Veterinary Drug Control)
Abstract:
Abstract :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 by n-hexane liquid. After enrichment, the samples were separated by UPLC, elutedwith acetonitrile and 10% methanol as the mobile phase and the MRM reaction was monitored. The results showed that there was a good linearity in the range of 5-200μg/L ,and the correlation coefficients were more than 0.999. The detection limit of the chloramphenicol, florfenicol and florfenicol-amine was 0.5μg/kg, and the limit of quantification was 2μg/kg. The average recoveries were 60% ~ 100% in the range of 2μg/kg to 20μg/kg, and the precision was less than 20%. The method was convenient, rapid, accurate and it was suitable for the detection of chloramphenicol in poultry eggs.
Key words:  poultry eggs  chloramphenicol  residues  UPLC-MS/MS

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