高效液相色谱法测定鸡蛋中4种氟喹诺酮类药物的含量

Determination of 4 kinds of fluoroquinolones in egg by high performance liquid chromatography

目的采用高效液相色谱法同时测定鸡蛋中环丙沙星、恩诺沙星、沙拉沙星和达氟沙星4种药物的残留量。方法样品经磷酸盐提取液提取后,经反相C_（18）柱分离,采用0.05 mol/L磷酸-三乙胺溶液：乙腈（85：15,V：V）流动相进行等度洗脱,流速为0.8 m L/min,采用荧光检测器在激发波长280 nm、发射波长450 nm的条件下进行测定,以外标法定量。结果环丙沙星、恩诺沙星和沙拉沙星在0.005~0.5μg/m L、达氟沙星在0.001~0.1μg/m L浓度范围内具有良好的线性关系,相关系数为0.9998,加标回收率为96.5%~103%,相对标准偏差为0.83%~1.28%。结论该方法精确可靠,重复性、稳定性和分离效果好,可适用于测定鸡蛋中氟喹诺酮类药物的残留量。

Objective To establish a method for determination of 4 kinds of fluoroquinolones residues including ciprofloxacin, enrofloxacin, sarafloxacin and danofloxacin in eggs by high performance liquid chromatography （HPLC）.Methods The samples were extracted with phosphate, separated by a reversed-phase C18 column using 0.05 mol/L phosphoric acid-triethylamine and acetonitrile （85：15,V：V） as the mobile phase for isocratic elution at the flow rate of 0.8 mL/min, and then detected by fluorescence detector at the excitation wavelength of 280 nm and the emission wavelength of 450 nm with the external standard method for quantification.Results The method showed good linearities in the ranges of 0.005~0.5 μg/mL for ciprofloxacin, enrofloxacin, and sarafloxacin and 0.001~0.1 μg/mL for danofloxacin with the correlation coefficients of 0.9998. The recoveries were 96.5%~103% with relative standard deviations in the range of 0.83%~1.28%.Conclusion The established method is accurate, reproducible, stable and has good separation effect, which can be used for the determination of fluoroquinolones residues in eggs.