高效液相色谱荧光检测法同时测定水产品中4种四环素族药物残留的研究

Simultaneous Determinatior） of Four Tetracycline Antibiotics Residues in Aquatic Products by High Performance Liquid Chromatography

建立了一种高效液相色谱荧光检测法同时测定水产品中4种四环素族抗生素残留的分析方法。水产品样品用柠檬酸缓冲液提取，清液用Oasis HLB固相萃取柱净化，1．36％的KH2PO4溶液定容后，荧光检测器于λex=380nm、λem=520nm测定。土霉素、四环素在0．05～5.0mg/L范围内，金霉素、强力霉素在0．1～5．0mg/L范围内呈良好的线性关系，检出限分别为0．01、0．01、0．03、0．03mg/kg（S／N≥3），添加平均回收率80％～110％，相对标准差在2．0％-6．6％之间。具有方法简便、分离度高、检出限低的特点，满足常规检测及水产品安全控制的需要。

A high performance liquid chromatographic method was developed for simultaneous determination of four Tetracychne antibiotics （TCs） residues in aquatic products. Samples were extracted with C6 H8 O7 · H2 O buffer solutions and centrifuged. The sample extracts were cleaned up by Oasis HLB solid - phase extraction cartridge and then were determined by KH2PO4（ 1.36% ） solution- FLD detection at λex = 380 nm, λem = 520 nm. The calibration graphs were linear in the concentration range of 0.05 - 2.5 mg/L, and 0.1 - 5.0 mg/L for OTC, TC and CTC, DOTC, respectively. The limits of detection were 0.01 mg/kg for OTC, TC, and 0.03 mg/kg for DOTC, CTC （S/N≥3）. The average recovery is not less than 80.0%, with RSD in the range of 2.62% - 6.11%. The method is simple and reliable. It can be used to analyze the OTC, TC, CTC and DOTC residues in aquatic products with satisfactory results.