甘草酸铋散的质量标准研究

Study on Quality Standard of Bismuth Glycyrrhetate Power

目的:建立甘草酸铋散的质量标准。方法:采用高效液相色谱法测定甘草酸的含量,色谱柱为十八烷基硅烷键合硅胶柱(C_(18)),流动相为磷酸二氢钾溶液-乙腈(V∶V=72∶28),流速为1.0 ml/min,检测波长为250 nm,柱温为35℃,进样量为10μl;采用乙二胺四乙酸(EDTA)容量法测定铋的含量。结果:甘草酸含量测定浓度线性范围为3.5～353.8μg/ml(r=0.999 995),精密度RSD为0.17%(n=6),稳定性RSD为0.63%(14 h内),重复性RSD为0.03%;平均加样回收率为96.64%,RSD为0.49%;定量限(S/N=10)为1.061μg/ml;10批样品的甘草酸含量为5.0%～5.1%。铋含量测定重复性RSD为0.3%(n=6);加样回收率为99.32%(RSD=0.3%,n=6);10批样品的铋含量为12.6%～13.2%。结论:该方法可用于甘草酸铋散的质量控制。

OBJIECTIVE:To establish the quality standards for bismuth glycyrrhetate power.METHODS:HPLC method was adopted to determine the content of glycyrrhetinic acid.The determination was performed on C18column with mobile phase consisted of monopotassiumphosphate solution-acetonitril(72∶28,V/V)with the flow rate of1.0ml/min.The detection wavelength was set at250nm,and the column temperature was35℃.The sample size was10μl.The content of Bi was determined by the ethylenediaminetetraacetic acid(EDTA)volumetric method.RESULTS:The linear range of glycyrrhetinic acid were3.5μg/ml-353.8μg/ml(r=0.999995),RSD of precision,stability and reproducibility were respectively0.17%(n=6),0.63%(14h)and0.03%,the average recovery was96.64%(RSD=0.49%),the limit of qualification(S/N=10)was1.061μg/ml,and the content of glycyrrhetinic acid of ten batches was5.0%-5.1%.The reproducible RSD of strontium content was0.3%(n=6);the recovery of sample was99.32%(RSD=0.3%,n=6);and the content of Bi in10batches was12.6%-13.2%.CONCLUSIONS:This method can be used for quality control of bismuth glycyrrhetate power.