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高效液相色谱-荧光法测定水产品中多种四环素残留
吴海燕1, 郭萌萌1, 李兆新1, 谭志军1, 乔玉玲2
1.中国水产科学研究院黄海水产研究所,青岛 266071;2.青岛亚是加食品有限公司中心实验室, 266071
摘要:
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40 μg/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%。
关键词:  高效液相色谱  水产品  四环素类  药物残留
DOI:
分类号:
基金项目:中央级公益性科研院所基本科研业务费项目(2012A1002)和农业部标准行业标准项目(2010)
Determination of tetracyclines residue in aquatic products by HPLC with fluorescence detector
Abstract:
The residue of tetracycline antibiotics including oxytetracycline(OTC), tetracycline(TC), doxycycline(DC) and chlorotetracycline(CTC) in carps,eels, shrimps and sea cucumbers 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-lipophilic balance(HLB) SPE cartridge,followed by separation by the C18 RP-HPLC column with imidazole buffer-methanol. The limit of quantification of tetracycline antibioitics in samples were 20, 20, 40, 40 μg/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.
Key words:  High performance liquid chromatography(HPLC)  Aquatic products  Tetracycilne anitbioitcs  Residue