梯度洗脱HPLC法测定鸡蛋中替米考星的残留  

Determination of Tilmicosin Residues in Egg by Gradient Elution HPLC Method

作　　者：张莉[1,2] 郑举 吴昊[1,2] 刘红云[1,2] 吴蕾 明文庆[1,2] 蔡一杰 ZHANG Li;ZHENG Ju;WU Hao(Anhui Province Institute of Veterinary Drug and Feedstuff,Hefei,Anhui 230091;Anhui Province Key Laboratory of Livestock and Poultry Product Safety Engineering,Hefei,Anhui 230061;Anhui Province Animal Disease Prevention and Control Center,Hefei,Anhui 230091)

机构地区：[1]安徽省兽药饲料监察所,安徽合肥230091 [2]畜禽产品安全工程安徽省重点实验室,安徽合肥230061 [3]安徽省动物疫病预防与控制中心,安徽合肥230091

出　　处：《安徽农业科学》2019年第20期217-219,共3页Journal of Anhui Agricultural Sciences

摘　　要：[目的]建立鸡蛋中替米考星的高效液相色谱残留分析方法。[方法]样品在乙腈提取下经OasisPRIMEHLB固相萃取小柱净化,氮吹浓缩后定容过膜上机检测。采用十八烷基硅烷键合硅胶色谱柱(4.6mm×250mm,5μm),以水-磷酸二丁胺缓冲液(97∶25)为流动相A、乙腈为流动相B进行梯度洗脱。检测波长280nm。[结果]替米考星在0.05~10.00μg/mL具有良好的线性关系(R2=0.9998)。替米考星在鸡蛋中的添加水平为0.1、1.0、5.0μg/mL时,回收率为80.6%~95.7%,批内、批间的相对偏差小于10%。[结论]该试验建立的HPLC法简便、灵敏、准确,适用于鸡蛋中替米考星的测定。[Objective] The research aimed to establish a method for determination of tilmicosin in eggs by high performance liquid chromatography.[Method]The samples were purified by Oasis PRIME HLB solid phase extraction column under the extraction of acetonitrile.After drying and concentrating,the samples were reused and tested over the membrane.Analysis was performed on a C 18 column (4.6 mm×250 mm,5 μm) by gradient elution using water-butyl amine phosphate(975 ∶25)(A)-acetonitrile(B)as mobile phase.The determination wave length was 280 nm.[Result]The tilmicosin had a good linear relationship (R2 = 0.9998) at 0.05-10.00 μg/mL. When the addition level of tilmicosin in eggs was 0.1, 1.0, 5.0 μg/mL, the recovery was 80.6%- 95.7%, and the relative deviation within and between batches was less than 10%.[Conclusion]The HPLC method established in this experiment is simple, sensitive and accurate, and is suitable for the determination of tilmicosin in eggs.

关 键 词：鸡蛋 替米考星 梯度洗脱HPLC法 残留 

分 类 号：S851.347[农业科学—预防兽医学]