固相萃取-高效液相色谱法测定蜜源生物液中3种四环素族抗生素的残留

目的]建立固相萃取-高效液相色谱法同时测定蜜源生物液中土霉素(OTC)、四环素(TC)、金霉素(CTC)残留量的方法。方法]采用0.1 mol/L Na2EDTA-Mcllvaine溶液提取样品,Oasis HLB固相萃取柱净化,以0.01 mol/L草酸-乙腈-甲醇对待测成分进行梯度洗脱。结果]OTC、TC在0.2～20.0μg/ml范围内线性关系良好,相关系数在0.999 6～0.999 8;CTC在0.5～20.0μg/ml范围内线性关系良好,相关系数为0.999 8;各组分在0.05～0.20 mg/kg添加浓度范围内,平均回收率在98.4%～104.9%,相对标准偏差为1.9%～5.0%。结论]该方法简单、可靠、灵敏度高,适用于蜜源生物液中四环素族抗生素残留的检测。

SPE-HPLC Determination of Tetracycline Antibiotics Residues in Honey-original Biological Fluids

Objective] The aim was to establish a reliable method for the simultaneous determination of residues for oxytetracycline(OTC),tetracycline(TC) and chlortetracycline(CTC) by solid-phase extraction with high-performance liquid chromatography(SPE-HPLC) in honey-original biological fluids.Method] 0.1 mol/L Na2EDTA-Mcllvaine solution was used as extraction solvent.After cleaning by Oasis HLB SPE column,TCs were separated by the mobile phase which included 0.01 mol/L oxalic acid,acetonitrile,methanol,and the separation mode was gradient elution.Result] OTC and TC showed a good linear relationship in the range of 0.2-20.0 μg/ml,and the correlation coefficients were 0.999 6-0.999 8,CTC showed a good linear relationship in the range of 0.5-20.0 μg/ml,and the correlation coefficients was 0.999 8,and the average recoveries(n=5) of the three compounds concerned were 98.4%-104.9%.and the relative standard deviations were 1.9%-5.0%.Conclusion] The method is simple,reliable,sensitive and suitable for the detection of the residuals for TCs in honey-original biological fluids.