瑶药红牛膝质量控制方法研究

瑶药红牛膝为苋科植物柳叶牛膝(Achyranthes longifolia)的根及根茎,为瑶族地区习用药材,目前仅有个别省区收载了其质量控制方法。该文对广西壮族自治区区内采集的14批红牛膝药材进行了性状鉴别、显微鉴别和薄层色谱鉴别,并采用飞诺美Gemini-NX C₁₈色谱柱(250 mm × 4.6 mm,5 μm),以乙腈-水溶液(15:85)进行等度洗脱,柱温25 ℃,流速1.0 mL·min^-1,检测波长243 nm,建立红牛膝中β-蜕皮甾酮的HPLC含量测定方法。结果表明:(1)红牛膝药材性状、显微鉴别特征明显,显微鉴别可见栓内层、维管束、异常维管束、导管、射线细胞、草酸钙砂晶或方晶等。(2)薄层色谱分离好,β-蜕皮甾酮和人参皂苷R_O对应的斑点清晰。(3)含量测定中,β-蜕皮甾酮在5.606～224.224 μg范围内线性关系良好(r=0.999 9),平均加样回收率为97.68%,RSD为1.37%(n=6)。(4)14批样品中β-蜕皮甾酮含量为0.005%～0.158%,平均含量为0.095%。该研究建立了完整的显微鉴别、薄层鉴别及含量测定方法,为合理评价红牛膝质量和临床合理用药提供科学依据。

Quality control method for Yao medicine Hongniuxi

Yao medicine Hongniuxi is the root and rhizome of Achyranthes longifolia, which is a commonly used medicinal herb in Yao ethnic areas. Currently, only a few provinces and regions have recorded the method for quality control of Hongniuxi. Microscopic method and thin layer chromatography(TLC)were qualitatively identified on the roots and rhizomes of 14 batches of Yao Medicine Hongniuxi collected in Guangxi Zhuang Autonomous Region in the study. The content of β-ecdysterone was determined by high performance liquid chromatography(HPLC). The Phenomenex column(250 mm × 4.6 mm, 5 μm)was used, the mobile phase was acetonitrile-water(15:85), the column temperature was 25 ℃, the flow rate was 1.0 mL·min^-1, and the detection wavelength was at 243 nm. The results were as follows:(1)The character and microscopic identification methods of Hongniuxi were obvious. Microscopic identification showed the inner layer of thrombus, vascular bundle, abnormal vascular bundle, duct, ray cell, calcium oxalate sand crystal or square crystal, etc.(2)The TLC identification spots of β-ecdysterone and ginsenoside R_O were clear, and the separation effect was good.(3)The β-ecdysterone showed a good linear relationship within the range of 5.606-224.224 μg(r=0.999 9), whose average recovery(n=6)was 97.68%, with the RSD of 1.37%.(4)Among 14 batches of samples, the contents of β-ecdysterone ranged from 0.005% to 0.158%, with an average content of 0.095%. This study establishes a complete method for microscopic identification, thin layer identification, and content determination, providing a scientific basis for rational evaluation of the quality of Hongniuxi and clinical rational drug use.