十大功劳叶药材的质量标准提高研究
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篇名: 十大功劳叶药材的质量标准提高研究
TITLE:
摘要: 目的:提高十大功劳叶药材的质量标准。方法:采用薄层色谱法(TLC)对药材样品进行定性鉴别。测定药材样品水分、灰分、醇浸出物。采用高效液相色谱法测定药材样品中盐酸小檗碱的含量,色谱柱为WondaSil C18,流动相为乙腈-0.05 mol/L磷酸二氢钾溶液(25 ∶ 75,V/V),流速为1.0 mL/min,检测波长为264 nm,柱温为30 ℃,进样量为10 μL。结果:药材样品TLC图斑点清晰,分离度好。药材样品水分为3.92%~7.03%,总灰分为3.65%~6.95%,酸不溶性灰分为0.05%~1.03%,醇浸出物为10.87%~33.14%。盐酸小檗碱检测进样量线性范围为0.183~0.915 μg(r=0.999 9);定量限、检测限分别为0.143、0.095 μg;精密度、稳定性、重复性试验的RSD<2.0%(n=6);加样回收率为95.21%~103.10%(RSD=2.95%,n=6)。结论:药材水分、总灰分、酸不溶性灰分分别不得过8.0%、6.0%、0.4%,醇浸出物、盐酸小檗碱含量分别不得低于16.0%、1.0%。所建标准可用于十大功劳叶药材的质量控制。
ABSTRACT: OBJECTIVE: To improve the quality standard of Folium Mahoniae. METHODS: TLC was used for qualitative identification. The contents of moisture, ash and ethanol extract were determined. The content of berberine hydrochloride was determined by HPLC. The determination was performed on WondaSil C18 column with mobile phase consisted of acetonitrile-0.05 mol/L monopotassium phosphate solution (25 ∶ 75,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was 264 nm, column temperature was 30 ℃, and sample size was 10 μL. RESULTS: TLC spots were clear and well-separated. The contents of moisture, total ash, acid-insoluble ash and ethanol extract were 3.92%-7.03%, 3.65%-6.95%, 0.05%-1.03% and 10.87%-33.14%, respectively. The linear range of berberine hydrochloride was 0.183-0.915 μg(r=0.999 9); quantitation limit and detection limit was 0.143, 0.095 μg, respectively. RSDs of precision, stability and reproducibility tests were lower than 2.0% (n=6); recovery was 95.21%-103.10%(RSD=2.95%,n=6). CONCLUSIONS: The content of moisture, total ash and acid-insoluble ash of medicinal materials is not exceed 8.0%, 6.0% and 0.4%, respectively. The content of ethanol extract and berberine hydrochloride is not less than 16.0% and 1.0%, respectively. Established standard can be used for quality control of Folium Mahoniae.
期刊: 2018年第29卷第4期
作者: 杨昌贵,肖承鸿,江维克,周涛,胡红莲
AUTHORS: YANG Changgui,XIAO Chenghong,JIANG Weike,ZHOU Tao,HU Honglian
关键字: 十大功劳叶;质量标准;高效液相色谱法;薄层色谱法
KEYWORDS: Folium Mahoniae; Quality standard; HPLC; TLC
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