HPLC法同时测定雌激素类药物尼尔雌醇片和己烯雌酚片中主药含量

Simultaneous Determination of Main Components in Estrogenic Hormone Drug Nilestriol Tablets and Diethylstilbestrol Tablets by HPLC

目的:建立同时测定尼尔雌醇片和己烯雌酚片中主药含量的方法。方法:采用高效液相色谱法。色谱柱为Waters Sym-metry C18,流动相为0.02 mol/L乙酸铵水溶液-乙腈(40∶60,V/V),流速为1.0 mL/min,检测波长为280 nm,柱温为35℃,进样量为20μL。结果:尼尔雌醇、己烯雌酚检测质量浓度线性范围均为0.01～0.5 mg/mL(r均为0.999 9);定量限分别为187、192 ng/mL,检测限分别为56、58 ng/mL;精密度、稳定性、重复性试验的RSD均小于1%(n=6);加样回收率分别为99.13%～100.80%(RSD=0.52%,n=9)、99.20%～100.90%(RSD=0.58%,n=9)。结论:该方法灵敏度高、重复性好,可用于同时测定雌激素类药物尼尔雌醇片中尼尔雌醇和己烯雌酚片中己烯雌酚的含量。

OBJECTIVE:To establish the method for simultaneous determination of main drug contents in Nilestriol tablet and Diethylstilbestrol tablet.METHODS:HPLC method was adopted.The determination was performed on Waters Symmetry C18 column with mobile phase consisted of 0.02 mol/L ammonium acetate water solution-acetonitrile(40∶60,V/V)at a flow rate of 1.0 mL/min.The detection wavelength was set at 280 nm,and column temperature was 35℃.The sample size was 20μL.RESULTS:The linear range of nilestriol and diethylstilbestrol were 0.01-0.5 mg/mL(r=0.999 9);the limits of quantitation were 187 and 192 ng/mL,and the limits of detection were 56 and 58 ng/mL.RSDs of precision,stability and reproducibility tests were all lower than 1%(n=6).The recoveries of them were 99.13%-100.80%(RSD=0.52%,n=9)and 99.20%-100.90%(RSD=0.58%,n=9).CONCLUSIONS:The method is more sensitive and reproducible,and suitable for simultaneous determination of nilestriol content in estrogenic hormone drug Nilestriol tablets and diethylstilbestrol content in Diethylstilbestrol tablets.