高效毛细管电泳法测定鸡蛋中环丙沙星的研究

目的]建立高效毛细管电泳测定鸡蛋中环丙沙星含量的方法。方法]通过对电泳缓冲液类型、离子浓度和pH值、样品溶剂种类、分离电压、分离温度和冲洗程序等电泳条件进行考察,确立测定鸡蛋中环丙沙星的高效毛细管电泳法,并测定电泳参数对检测结果的影响。结果]在检测波长为277 nm时,最佳电泳条件为:电泳缓冲液为30 mmol/LNa2B4O7-10 mmol/LKH2PO4溶液(pH值8.53),未涂层石英毛细管(50μm×47 cm,有效长度38.5 cm)为分离通道,分离电压为18 kV。在鸡蛋中对环丙沙星的检测结果显示,在最佳电泳条件下,环丙沙星在11 min内实现基线分离,在0.25～80.00μg/ml浓度范围内其浓度和峰面积呈良好的线性关系(R2=0.999 2),平均加标回收率为101.48%,平均RSD为2.466 4%(n=5)。结论]该方法快速简便、灵敏度高、重现性好,可用于鸡蛋中环丙沙星含量的测定。

Study on High Performance Capillary Electrophoresis for Determination of Ciprofloxacin in Egg

Objective] The study aimed to establish a method of determining the ciprofloxacin in egg by the high performance capillary electrophoresis(HPCE).Method] Through the examination on the electrophoresis conditions such as the electrophoresis buffer types,ion concn.and pH value,sample solvent kinds,separation voltage,separating temperature and washing procedure,the HPCE method for determining the ciprofloxacin in egg were established and the effects of the electrophoretic parameters on the testing results were determined.Result] When the detection wavelength was set at 277 nm,the optimum electrophoretic conditions were as follows: the electrophoretic buffer was 30 mmol/L Na2B4O7-10 mmol/L KH2PO4 solution(pH 8.53),the non coating quartz capillary(50 μm×47 cm,effective length of 38.5 cm) was as the separating channel,the separation voltage was 18 kV.The testing on ciprofloxacin in egg showed that,under the optimal electrophoresis conditions,the ciprofloxacin could realize the baseline separation within 11min;the regression curve for the peak area and the melamine concn.revealed a good linearity in the range of 0.25-80.00 μg/ml,with a correlation coefficient of 0.999 2;the standardized recovery was averaged at 101.48%,with the mean RSD of 2.466 4%(n=5).Conclusion] The method exhibits the characteristics of rapidity and simplicity,high sensitivity and good repeatability,which could be used to the determination of ciprofloxacin in egg.