山紫菀药材的质量标准研究
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篇名: 山紫菀药材的质量标准研究
TITLE:
摘要: 目的: 建立山紫菀药材的质量标准。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、浸出物的含量;采用高效液相色谱法测定药材样品中阿魏酸的含量,色谱柱为Waters SunFire C18, 流动相为乙腈-0.1%磷酸溶液(13 ∶ 87,V/V),流速为1.0 mL/min,检测波长为319 nm,柱温为30 ℃,进样量为10 μL。结果:山紫菀的TLC图斑点清晰,分离度好,阴性对照无干扰。药材样品水分为7.6%~9.4%,总灰分为11.7%~19.6%,酸不溶性灰分为5.9%~14.1%,浸出物为25.4%~37.5%。阿魏酸检测进样量线性范围为0.021 2~0.636 8 μg(r=0.999 9);定量限为2.25 ng,检测限为0.75 ng;中间精密度、重复性、稳定性试验的RSD均小于3.0%;加样回收率为97.81%~100.59%(RSD=1.02%,n=9)。结论:初步拟定山紫菀药材水分不得过10.0%,总灰分不得过19.0%,酸不溶性成分不得过12.0%,浸出物不得少于25.0%,阿魏酸含量不得少于0.1%;所建标准可为山紫菀药材的质量控制提供参考。
ABSTRACT: OBJECTIVE: To establish the quality standard of Ligularia fischeri. METHODS: TLC was used for qualitative identification of samples. The contents of moisture, ash and extract were determined. The content of ferulic acid in samples was determined by HPLC. The determination was performed on Waters SunFire C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid (13 ∶ 87,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 319 nm, and column temperature was 30 ℃. The sample size was 10 μL. RESULTS: TLC spots were clear and well-separated without interference from genitive control. The moisture, total ash, acid-insoluble ash and extract of samples were 7.6%-9.4%, 11.7%-19.6%, 5.9%-14.1% and 25.4%-37.5%, respectively. The linear range of ferulic acid were 0.021 2-0.636 8 μg(r=0.999 9). limited of quantation was 2.25 ng, the limited of detection was 0.75 ng. RSDs of intermediate precision, reproducibility and stability tests were all lower than 3.0%. The recoveries ranged 97.81%-100.59%(RSD=1.02%,n=9). CONCLUSIONS: The moisture, total ash and acid-insoluble ash of samples are no more than 10.0%, 19.0%, 12.0%; the extract and the content of ferulic acid are no less than 25.0% and 0.1%. Established standard can provide reference for quality control of L. fischeri.
期刊: 2018年第29卷第8期
作者: 曲艳丽,刘治民,孙冶,刘雨过,杨建龙
AUTHORS: QU Yanli,LIU Zhimin,SUN Ye,LIU Yuguo,YANG Jianlong
关键字: 山紫菀;质量标准;阿魏酸; 水分;灰分;浸出物;薄层色谱法;高效液相色谱法
KEYWORDS: Ligularia fischeri; Quality standard; Ferulic acid; Moisture; Ash; Extract; TLC; HPLC
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