脉络宁颗粒的质量标准提升研究

Study on the Improvement of Mailuoning Granule's Quality Standard

关键词:  脉络宁颗粒  鉴别  含量测定  薄层色谱法  高效液相色谱法  质量标准

Key words:  Mailuoning granules  identification  content determination  TLC  HPLC  quality standard

摘要:

目的 提升脉络宁颗粒的产品质量标准。方法 对现有质量标准进行增修订，修订组方中牛膝和玄参的薄层色谱（TLC）鉴定方法，增加石斛的HPLC鉴定方法，修订玄参的HPLC含量测定法。结果 脉络宁颗粒中牛膝和玄参的TLC图谱均与对应的对照药材及对照品在相同位置上显现相同颜色的斑点，且阴性对照样品无干扰，石斛的HPLC图谱中供试品色谱中呈现与对照品色谱峰保留时间相一致的色谱峰，且阴性对照样品无干扰。玄参含量测定采用Alltima^TMC₁₈色谱柱（4.6 mm×250 mm，5 μm）；流动相为乙腈-0.03%磷酸溶液（梯度洗脱）；流速为1.0 mL·min^-1；检测波长为203 nm（0~20 min）、280 nm（20~40 min），柱温25℃。哈巴苷、哈巴俄苷进样量分别在0.070 51~1.057 6，0.021 42~0.321 4 μg内线性关系良好（r均>0.999 7）；平均加样回收率分别为97.87%，100.96%，RSD均<2%（n=6）。结论 本研究建立的方法操作简便、准确可靠、专属性强，提升和完善了该制剂的质量标准。

Abstract:

OBJECTIVE To improve the product quality standard of Mailuoning granules. METHODS The existing quality standards were added and revised, the thin layer chromatography(TLC) identification method of Achyranthis Bidentatae Radix and Scrophulariae Radix in the formula was revised, and the HPLC identification method of Dendrobii Caulis was added, the HPLC determination method of Scrophulariae Radix was revised. RESULTS The TLC patterns of Achyranthis Bidentatae Radix and Scrophulariae Radix in Mailuoning granules showed spots of the same color on the same position as the corresponding control medicinal materials or the reference substance, and the negative control had no interference. The HPLC pattern of Dendrobii Caulis for testing the product chromatogram presented a chromatographic peak consistent with the retention time of the reference chromatographic peak, and the negative control had no interference. The content of Scrophulariae Radix was determined using Alltima^TM C₁₈ chromatographic column(4.6 mm×250 mm, 5 μm), the mobile phase was acetonitrile-0.03% phosphoric acid solution(gradient elution), the flow rate was 1.0 mL·min^-1; the detection wavelength was 203 nm(0-20 min) and 280 nm(20-40 min). The column temperature was 25℃. The linear range of harpagide and harpagoside was 0.070 51-1.057 6 and 0.021 42-0.321 4 μg(r>0.999 7); the average recoveries were 97.87% and 100.96%(RSD<2%, n=6). CONCLUSION The developed methods is simple, accurate, reliable and specific, which can improve the quality standard of this preparation.