王旭堂 刁志祥 张培杨 谢恺舟 王波 刘楚君 张跟喜 张涛 刘学忠 戴国俊

摘要：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250.0 μg/kg内，线性关系良好，决定系数均大于0.999 2。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3.4 μg/kg、3.3 μg/kg，LOQ分别为9.9 μg/kg、9.7 μg/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。

关键词：鹌鹑蛋;鸽蛋;甲砜霉素;加速溶剂萃取;超高效液相色谱-荧光检测法

中图分类号：S859.84文献标识码：A文章编号：1000-4440（2020）01-0206-06

Abstract： 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 250.0 μg/kg， and the linear relationship was good. The coefficients of determination were greater than 0.999 2. 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 3.4 μg/kg and 3.3 μg/kg， and the quantitative limits were 9.9 μg/kgand 9.7 μg/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.

Key words：quail eggs;pigeon eggs;thiamphenicol;accelerated solvent extraction;ultra-high performance liquid chromatography with fluorescence detection

甲砜霉素（Thiamphenicol，TAP），別名硫霉素，甲砜氯霉素，是人工合成的氯霉素的同类物，属于广谱抗菌药物。主要用于防治需氧革兰氏阴性菌及革兰氏阳性菌、厌氧菌、立克次体属病菌、螺旋体病菌和衣原体属病菌等引起的疾病。通过抑制细菌蛋白质的形成，起到抑菌效果。由于其对畜禽的多种细菌性疾病有良好的治疗效果，在畜禽生产中已被广泛使用。

禽蛋作为来源最广，蛋白质含量较高的动物性食品，近年来其需求量日益增大。而养殖者为了提高经济效益，常将TAP等抗生素药物不合理地用于禽类，导致药物残留于禽蛋中。因为TAP具有较强的抑制红细胞、白细胞和血小板生成的作用，影响人类健康，所以许多国家都对这种药物的最高残留限量做出了规定[1-3]。……