玫瑰糠疹合剂质量标准研究

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。

Quality Standard of Gibert's Disease Mixture

Objective: To establish quality standard of gibert's disease mixture. Methods: ChiShao (Radix paeoniae rubra) and FangFeng (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, 5μm), acetonitrile-0.2% phosphoric acid and 0.04% triethylamine solution as mobile phase, column temperature 30℃, flow rate 1.0mL/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, 5μm), acetonitrile-0.1% phosphoric acid(40:60) as mobile phase, column temperature 30℃, flow rate 1.0mL/min, detection wavelength 254 nm. Results: ChiShao and FangFeng 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/mL, 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 35.88μg/mL, 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 and 17.16μg/mL, 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.