高效液相色谱-荧光法测定水产品中多种四环素残留

Determination of tetracyclines residue in aquatic products by HPLC with fluorescence detector

建立了鲤鱼、鳗鲡、对虾和海参中四环素、土霉素、金霉素和盐酸多西环素残留的高效液相色谱-荧光检测方法。样品用柠檬酸缓冲溶液提取,HLB固相萃取柱净化,以咪唑缓冲溶液-甲醇为流动相,经C18反相色谱柱分离后用荧光检测器测定。土霉素、四环素、金霉素和盐酸多西环素的定量限分别为20、20、40和40μg/kg,4种四环素类药物残留的加标回收率均在70.5%～100%,批内相对标准偏差(RSD)小于10.0%,批间相对标准偏差(RSD)小于15.0%。

The residue of tetracycline antibiotics including oxytetracycline（OTC）, tetra cycline（TC）, doxycycline（DC） and chlorotetracycline（CTC） in carps,eels, shrimps and sea cu cumbers were determined with the optimized method of high performance liquid chromatography （HPLC） coupled with fluorescence detection（FL）. The target compounds were extracted with acidic EDTA-Mcllvaine buffer solution, then enriched and cleared up using a hydrophilic-li- pophilic balance（HLB） SPE cartridge, followed by separation by the C^sRP-HPLC column with imidazole buffer-methanol. The limit of quantification of tetracycline antibioitics in samples were 20, 20, 40, 40μg/kg for TC,OTC.CTC and DC respectively. The average recovery for all the compounds were 70.5%~100%. The inter-variation coefficients were under 10.0%, and intra- variation coefficients were under 15.0%. The method is rapid, sensitive, accurate, reliable and can be applied in the analysis of antibiotics residues in aquatic products.