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

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

[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。

[ 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 hon- ey-original biological fluids. [ Method] 0.1 mol/L Na2EDTA-Mcllvaine solution was used as extraction solvent. After cleaning by Oasis HLBSPE 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 co- efficients 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 devia- tions were 1.9% -5.0%. [ Conclusion] The method is simple, reliable, sensitive and suitable for the detection of the residuals for TCs in honev-orizinal biological fluids.