玫瑰糠疹合剂质量标准研究

Quality Standard of Gibert′s Disease Mixture

目的：建立玫瑰糠疹合剂的质量标准。方法：采用薄层色谱法对玫瑰糠疹合剂中赤芍、防风进行定性鉴别;通过高效液相色谱法测定制剂中芍药苷、升麻素苷和5-O-甲基维斯阿米醇苷的含量。芍药苷的色谱条件为ZORBAX SB-C18色谱柱（4.6 mm×250 mm,5μm）,流动相以乙腈-0.2%磷酸和0.04%三乙胺溶液（14∶86）,柱温30℃,流速1.0 m L/min,检测波长230 nm;升麻素苷和5-O-甲基维斯阿米醇苷色谱条件为ZORBAX SB-C18色谱柱（4.6 mm×250 mm,5μm）,流动相以乙腈-0.1%磷酸水（40∶60）,柱温30℃,流速1.0 m L/min,检测波长为254 nm。结果：赤芍、防风薄层鉴别斑点清晰,分离度好,阴性对照无干扰。芍药苷在10~60μg/m L范围内,芍药苷峰面积与质量浓度有良好的线性关系（r=1）,平均加样回收率为98.53%,RSD为1.18%;升麻素苷在5.98~35.88μg/m L范围内,升麻素苷峰面积与质量浓度有良好的线性关系（r=0.999 9）,平均加样回收率为98.3%,RSD为1.77%;5-O-甲基维斯阿米醇苷在2.86~17.1 6μg/m L范围内,峰面积与质量浓度有良好的线性关系（r=1）,平均加样回收率为99.07%,RSD为1.09%。结论：本实验方法可靠、准确,可以用于该制剂的质量控制。

Objective： To establish quality standard of gibert＇s disease mixture. Methods： ChiShao（Radix paeoniae rubra） and Fang Feng（Radix Saposhnikoviae） in gibert＇s disease mixture were qualitatively identified by TLC; the contents of peoniflorin, prim-O-glucosylcimifugin and 4＇-O-beta-Glucopyranosyl-5-O-Methylvisamminol in the preparations were determined by HPLC. Chromatographic conditions of peoniflorin were ZORBAX SB-C18 chromatographic column（4.6 mm ×250 mm, 5 μm）, acetonitrile-0.2% phosphoric acid and 0.04% triethylamine solution as mobile phase, column temperature 30℃, flow rate 1.0m L/min, detection wavelength 230nm;chromatographic conditions of prim-O-glucosylcimifugin and 4＇-O-beta-Glucopyranosyl-5-O-Methylvisamminol were ZORBAX SB-C18 chromatographic column（4.6 mm×250 mm, 5 μm）, acetonitrile-0.1% phosphoric acid（40：60）as mobile phase, column temperature 30℃, flow rate 1.0m L/min, detection wavelength 254 nm. Results： ChiShao and Fang Feng showed clear spots, good separation and non-interference in negative control in TLC identification.Peoniflorin showed a good linear relationship in the range between 10 and 60μg/m L, its peak area and concentrations demonstrated better linear relationship（r=1）, average recovery rate was 98.53%, RSD was 1.18%;prim-O-glucosylcimifugin showed a good linear relationship in the range between 5.98 and 35.88 μg/m L, its peak area and concentrations were in a good linear relationship（r=0.999 9）, average recovery rate was 98.3%, RSD was 1.77%;4＇-O-beta-Glucopyranosyl-5-O-Methylvisamminol showed a good linear relationship in the range between 2.86 and17.16 μg/m L, its peak area and concentrations demonstrated better linear relationship（r=1）, average recovery rate was 99.07%, RSD was 1.09%. Conclusion： The method, reliable and accurate, could be used for quality control of the preparation.