芪丹利心丸薄层色谱的构建及3种指标成分的测定

Establishment of Thin-Layer Chromatography Identification for Qidan Lixin Pills and Determination of Three Marker Components

摘要

目的：建立芪丹利心丸3种指标成分的液相色谱含量测定方法、3种药材薄层色谱鉴别方法。方法：采用薄层色谱（thin-layer chromatography，TLC）法定性鉴别芪丹利心丸中党参、刺五加。采用高效液相色谱法测定芪丹利心丸中丹酚酸B、柚皮苷、新橙皮苷的含量。色谱柱：色谱柱为Waters XTerra MS C₁₈ 5 μm 4.6×250 mm，流动相为乙腈-0.1%磷酸水溶液（22:78），检测波长为283 nm，流速为1.0 mL·min^-1，柱温为30 ℃。理论板数按丹酚酸B峰计算应不低于6 000，按柚皮苷、新橙皮苷峰计算应不低于3 000。结果：党参、刺五加定性鉴别斑点清晰，阴性无干扰；含量测定结果中丹酚酸B、柚皮苷、新橙皮苷分别在进样量为0.300 3~3.003 1 μg、0.135 8~1.358 2 μg、0.125 6~1.255 5 μg范围内具有良好的线性关系。平均加样回收率分别为102.53%、99.37%、100.48%，RSD分别为2.20%、1.23%、1.08%（n=6）。结论：该实验建立的方法重复性好、方法稳定可行，可用于芪丹利心丸的质量控制。

Abstract

Objective: To establish liquid chromatography methods for three index components of Qidan Lixin Pills and thin-layer chromatography methods for three medicinal materials. Methods: The thin-layer chromatography (TLC) method was adopted to qualitatively identify Codonopsis pilosula and Acanthopanax senticosus in Qidan Lixin Pills. The contents of salvianolic acid B, naringin and neohesperidin in Qidan Lixin Pills were determined by high performance liquid chromatography. Chromatographic column: The chromatographic column was Waters XTerra MS C₁₈ 5 μm 4.6×250 mm, the mobile phase was acetonitrile-0.1% phosphoric acid aqueous solution (22:78), the detection wavelength was 283 nm, the flow rate was 1.0 mL·min^-1, and the column temperature was 30 ℃. The theoretical plate count, calculated based on the peak of salvianolic acid B, should be no less than 6 000, and calculated based on the peaks of naringin and neohesperidin, should be no less than 3 000. Results: The qualitative identification of Codonopsis pilosula and Acanthopanax senticosus exhibited clear and distinct spots with no interfering signals observed. In the quantitative analysis, salvianolic acid B, naringin, and neohesperidin demonstrated good linearity within the injection ranges of 0.300 3~3.003 1 μg, 0.135 8~1.358 2 μg, and 0.125 6~1.255 5 μg, respectively. The average recoveries were 102.53%, 99.37%, and 100.48%, with corresponding relative standard deviations RSD of 2.20%, 1.23%, and 1.08% (n=6), indicating satisfactory precision and accuracy. Conclusion: The method established in this experiment has good repeatability, is stable and feasible, and can be used for the quality control of Qidan Lixin Pills.

关键词

芪丹利心丸 / 薄层色谱 / 含量测定

Key words

Qidan Lixin pills / thin-layer chromatography / content determination

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基金资助

国家科技重大专项重大新药创制项目(2010ZX09102-202)