高效液相色谱法测定畜禽肉及三文鱼中土霉素、四环素和金霉素残留

Determination of terramycin, minocycline and aureomycin in the Livestock and poultry meat and salmon by High Performance Liquid Chromatography

中文关键词:  高效液相色谱法  土霉素  四环素  金霉素  残留量

英文关键词:high performance liquid chromatography  oxytetracycline  tetracycline  chlortetracycline  residue

中文摘要:

      目的 建立一种用高效液相色谱法同时测定畜禽肉与三文鱼中的土霉素、四环素和金霉素残留的分析方法。方法 Na2EDTA-Mcllvaine缓冲溶液(pH=4.0)对样品进行提取, 三氯乙酸沉淀样品中的蛋白质, 固相萃取柱富集待测样品中的抗生素, 流动相为0.01 mol/L草酸溶液:乙腈:甲醇(73::17:10, v:v:v)混合溶液, 检测波长为350 nm, 外标法定量。结果 土霉素、四环素和金霉素分别在100~4000、100~4000、200~8000 ng/mL范围内线性关系良好, 相关系数r>0.99, 土霉素、四环素和金霉素检出限分别为20、20、40 μg/kg, 加标回收率为74%~90%, 相对标准偏差为3%~8%。结论 该方法简便、快速、灵敏, 适用于畜禽肉和水产品中土霉素、四环素和金霉素残留的检测。

英文摘要:

      Objective To establish a method that can determine the content of oxytetracycline (OTC), tetracycline(TC) and chlortetracycline(CTC) residues in the livestock and poultry meat and salmon using high performance liquid chromatography (HPLC). Methods The samples were extracted by Na2EDTA-Mcllvaine buffer solution (pH=4.0) and removed the protein by chloroacetic acid. Then the samples were cleaned up by solid phase extraction column. The mobile phase was 0.01 mol/L oxalic acid:acetonitrile:methanol (73:17:10, v:v:v). The detection wave-length was 350 nm and the external standard quantitation was adopted. Results This method showed a good linear relationship in the range of 100~4000, 100~4000 ng/mL, and 200~8000 ng/mL for OTC, TC and CTC, respectively. The correlation coefficient was over 0.99. The detect limits were 20, 20 μg/kg, and 40 μg/kg for OTC, TC and CTC, respectively. The recoveries was 74%~90% with the relative standard deviation of 3%~8%, respectively. Conclusion The method is convenient, fast, sensitive and repro-ducible and it is suitable for determining OTC, TC and CTC residues in fresh meat and aquatic products.