高效液相色谱法同时测定鸡肉中3种四环素类抗生素残留

Simultaneous Determination of 3 Tetracycline Residues in Chicken Tissues by High-Performance Liquid Chromatography

建立同时测定鸡肉组织中四环素、土霉素、金霉素3种四环素类抗生素残留的高效液相色谱分析方法。样品经柠檬酸缓冲液(pH4)、20%三氯乙酸提取后,C-18E固相萃取柱净化,用高效液相色谱C18柱分离,乙腈-甲醇-草酸作为流动相,流速为1.0mL/min,梯度洗脱,紫外检测波长为351nm,外标法峰面积定量。3种四环素类抗生素在质量浓度范围内线性良好,R2均大于0.99,鸡肉组织样品在500μg/kg添加水平的添加回收率为86.2%～89.3%,相对标准偏差为0.854%～1.213%(n=10),方法的定量限为10μg/kg。该方法灵敏度高、重复性好,适用于鸡肉组织中四环素、土霉素、金霉素残留的检测。

A simultaneous high performance liquid chromatography（HPLC） method was developed for the determination of 3 tetracycline residues in chicken tissues.Chicken tissue samples were extracted with citrate buffer（pH 4） and 20% TCA,and clean-up on C-18Esolid phase（SPE） cartridge.Chromatographic separation was performed on a C18column with a mobile phase consisting of acetonitrile and methanol and oxalic acid at a flow rate of 1.0 mL/min by gradient elution.Detection wavelength was 351 nm and external standard method was used for quantification.The calibration curves of 3 tetracyclines exhibited good linearity with correlation coefficients of 0.99.The average recovery rate for 3 tetracyclines in chicken tissues spiked at 500 μg/kg varied from 86.2% to 89.3%,with relative standard deviations between 0.854% and 1.213%（n = 10）.The limit of quantification was 10 μg/kg.