禽类肌肉中氟苯尼考残留检测方法对比分析

Comparative experimental study on the detection of florfenicol residues in poultry muscle

本文分别建立高效液相色谱荧光检测法(HPLC)与液相色谱-串联质谱法(LC-MS/MS)检测禽肉中氟苯尼考残留的方法。试样用碱化乙酸乙酯或乙腈提取,正己烷除脂净化,用高效液相色谱荧光检测法(HPLC)与液相色谱-串联质谱联用法(LC-MS/MS)分别测定,经验证检测方法线性关系均良好,相关系数分别为0.9993和0.9991。当添加氟苯尼考量为5~200μg/kg时,高效液相色谱荧光检测法的样品加标回收率为82.0%~92.0%,液相色谱-串联质谱法为90.0%~100.0%,高效液相色谱荧光检测法相对标准偏差为1.34%~3.78%,液相色谱-串联质谱法为1.95%~3.68%;高效液相色谱荧光检测法的检出限为10μg/kg、定量限为30μg/kg,液相色谱-串联质谱法的检出限为5μg/kg、定量限为10μg/kg。本次试验旨为“禽类肌肉中检测氟苯尼考药物残留时根据实验室具体条件选择检测方法”。

In this paper,methods for the detection of florfenicol residues in poultry meat by high performance liquid chromatography(HPLC)and liquid chromatography-tandem mass spectrometry(LC-MS/MS)were established respectively.The samples were extracted with alkalized ethyl acetate or acetonitrile,purified by n-hexane degreasing,and determined by HPLC and LC-MS/MS,respectively.The good correlation coefficients of the method linear relationship were 0.9993 and 0.9991,respectively.When the addition of florfenil is considered to be 5~200μg/kg,the recovery rate of the samples is 82.0%~92.0%by HPLC,and 90.0%~100.0%by LC-MS/MS.The deviation is 1.34%~3.78%by HPLC,and 1.95%-3.68%by LC-MS/MS;the detection limit of HPLC is 10μg/kg,The quantitative limit of detection was 30μg/kg;the detection limit of LC-MS/MS was 5μg/kg,and the quantification limit was 10μg/kg.The purpose of this experiment is to“determine florfenicol drug residues in poultry muscle according to the specific testing conditions of the laboratory”.