超高液相色谱荧光检测法测定鹌鹑蛋和鸽蛋中甲砜霉素残留量

Determination of thiamphenicol residues in quail eggs and pigeon eggs by ultra-high performance liquid chromatography with fluorescence detection

本研究旨在建立鹌鹑蛋和鸽蛋中甲砜霉素(TAP)残留的超高效液相色谱-荧光检测(UPLC-FLD)方法。以鹌鹑蛋和鸽蛋为试验材料,采用加速溶剂萃取(ASE)技术提取目标物,以乙腈饱和的正己烷去脂,净化后用UPLC-FLD法进行检测分析。结果表明,在鹌鹑蛋和鸽蛋中TAP的添加质量比在定量限(LOQ)至250.0μg/kg内,线性关系良好,决定系数均大于0.9992。TAP添加质量比为LOQ、0.5 MRL、1.0 MRL和2.0 MRL时,在鹌鹑蛋和鸽蛋中的回收率分别为83.23%~95.72%、84.37%~97.12%,检测限(LOD)分别为3.4μg/kg、3.3μg/kg,LOQ分别为9.9μg/kg、9.7μg/kg。检测方法快速、高效、灵敏度高,为鹌鹑蛋和鸽蛋中TAP残留检测提供了新方法。

This study aimed to establish an ultra-high performance liquid chromatography-fluorescence detection(UPLC-FLD)method for the determination of thiamphenicol(TAP)residues in quail eggs and pigeon eggs.Using quail eggs and pigeon eggs as test materials,the target compound was extracted by accelerated solvent extraction(ASE)technique,and degreased by n-hexane saturated with acetonitrile.After purification,it was detected and analyzed by UPLC-FLD method.The results showed that the mass ratio of TAP in quail eggs and pigeon eggs was in the range of the limit of quantification(LOQ)to 250.0μg/kg,and the linear relationship was good.The coefficients of determination were greater than 0.9992.When TAP was added at mass ratios of LOQ,0.5 maximum residue limit(MRL),1.0 MRL and 2.0 MRL,the recoveries in quail eggs and pigeon eggs were 83.23%-95.72%,84.37%-97.12%,the detection limits were 3.4μg/kg and 3.3μg/kg,and the quantitative limits were 9.9μg/kg and 9.7μg/kg,respectively.The detection method used in this study is rapid,efficient and sensitive,which provides a new method for the detection of TAP residues in quail eggs and pigeon eggs.