摘要
应用高效液相色谱(HPLC)对动物性食品中土霉素(OTC)和四环素(TC)进行测定,样品经含乙二胺四乙酸二钠的丁二酸钠缓冲液除蛋白后,由SPE-C_(18)小柱提纯净化,经ODS—C_(18)柱分离后,用8％氧氯化锆溶液柱后衍生,与锆离子的螯合物在激发波长(Ex):406nm和发射波长(Em):515nm处检测。实验优化了锆试剂的浓度和柱后衍生的条件,提高了检出的灵敏度,土霉素和四环素的回收率分别为89.59％和92.59％,变异系数(CV)分别为4.98％和6.74％。土霉素和四环素的最低检出浓度(信噪比5:1)分别为3μg/L和5μg/L,线性范围为0.01～10μg/L,土霉素和四环素的相关系数分别为0.999 9和1.000 0。
High-performance liquid chromatography was applied to determine oxytetracycline(OTC) and tetracycline (TC) in original foodstuffs of animals. The sample was eluted by SPE-C18 column and separated by ODS-C18 column after protein was removed. Post-column derivative was done by 8% Zirconyl chloride octahydrate toget final sample to be determined the zirconium chelation at excitation bandwidth of 406 nm and emission bandwidth of 515 nm.The zirconium reagent concentration and post-column derivative of condition were optimized. The recovery rates of OTC and TC were 89.59% and 92.59% . The coefficient of variation (CV) was found to be 4.98% and 6.74% for OTC and TC, separately. The detection limits of the assay (signal-to-noise = 5:1) were 3 μg/L and 5 μg/L for OTC and TC, respectively. The fluorescence intensity was linear in a concentration range of 0.01-10 μg/L OTC or TC(r(OTC)=0.999 9,r(TC)= 1.000 0).
出处
《浙江科技学院学报》
CAS
2003年第B11期50-53,共4页
Journal of Zhejiang University of Science and Technology
