HPLC-FL法测定盐酸环丙沙星缓释胶囊在健康人体尿样中尿药浓度

Exploration on determinating the concentration of ciprofloxacin hydrochloride sustained-release capsules in urine samples of healthy human by HPLC-FL

目的:建立快速测定盐酸环丙沙星缓释胶囊在健康人体尿样中药物浓度的HPLC-FL方法。方法:色谱柱为Lichrospher-ODS(150mm×4.6mm ID,5μm);缓冲液:20mmol/L磷酸二氢钠溶液与20mmol/L磷酸氢二钠溶液按500∶334体积比混合(0.1%的三乙胺调pH为3.95),流动相:缓冲液-乙腈-甲醇(80∶10∶10);荧光检测器激发波长为338nm,发射波长为450nm;流速为1.0ml/min;柱温:30℃。结果:盐酸环丙沙星缓释胶囊人体尿样浓度在0~5μg/ml范围内,峰面积与浓度呈良好的线性关系(r=0.9997);重复性试验相对标准偏差RSD为1.23%;日内精密度实验平均RSD为1.7%,日间精密度实验平均RSD为2.2%;平均回收率为101.94%(n=9)。结论:本方法快速,准确,精密度良好,可用于盐酸环丙沙星缓释胶囊的含量测定和人体尿样浓度测定。

Objective：To establish a rapid determination method of the concentration of ciprofloxacin hydrochloride sustainedrelease capsules in healthy human urine samples by HPLC-FL.Methods：The column was Lichrospher-ODS（150 mm×4.6 mm ID,5μm）;buffer solution were 20 mmol/L sodium dihydrogen phosphate solution with 20 mmol/L disodium hydrogen phosphate solution（mixed by volume ratio of 500∶334,0.1% triethylamine pH=3.95）;mobile phase was buffer-acetonitrile-methanol（80∶10∶10）;fluorescence detector excitation wavelength 338 nm;emission wavelength was 450 nm;the flow rate was 1.0 ml/min;column temperature was 30℃.Results：The concentration of ciprofloxacin hydrochloride sustained-release capsules in human urine was 0~5μg/ml;the peak area and concentration showed a good linear relationship（r=0.9997）;RSD in repeatability experiment was 1.23%;the average RSD of day precision test was 1.7%;the average RSD of inter-day precision test was 2.2%;the average recovery was 101.94%（n=9）.Conclusion：This method is rapid,accurate,precise,can be used for determining the concentration of ciprofloxacin hydrochloride sustained-release capsules and the concentration in human urine samples.