藏药水柏枝的质量标准研究

摘要

目的:建立藏药水柏枝的质量标准.方法:从性状特征、显微特征、薄层色谱(TLC)方面对药材进行定性鉴别;检测药材水分、灰分和浸出物的含量;采用高效液相色谱法(HPLC)测定药材中没食子酸的含量:色谱柱为Diamonsil C18,流动相为乙腈-0.1%磷酸溶液(5:95,V/V),流速为1.0 mL/min,检测波长为270 nm,柱温为30℃,进样量为10μL.结果:水柏枝呈圆柱形,有多数窄条形互生小叶,质脆,易折断,气微,味淡.木栓细胞表面和下表皮细胞表面可见多角形,木纤维多成束,草酸钙簇晶众多.TLC图斑点清晰,分离度良好.水分为6.83%~8.12%,总灰分为4.01%~5.01%,酸不溶性灰分为1.06%~1.98%,水浸出物为17.91%~22.65%,醇浸出物为11.29%~15.51%.没食子酸检测质量浓度线性范围为3.13~50μg/mL(r=0.9997),精密度、稳定性、重复试验的RSD<1.0%,没食子酸加样回收率为94.0%~100.8%(RSD=2.27%,n=9).结论:该研究所建标准可用于藏药水柏枝的质量评价.%OBJECTIVE:To establish the quality standard of Tibetan medicine Myricaria germanica. METHODS:M. germani-ca was identified in respects of properties,microscopic characteristics and TLC. The contents of moisture,ash and extract were de-termined. HPLC method was adopted for content determination of gallic acid. The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution(5:95,V/V)at the flow rate of 1.0 mL/min. The detection wavlengths were set at 270 nm. The column temperature was 30 ℃ and the sample size was 10 μL. RESULTS:M. ger-manica was cylindrical in shape,and there were many narrow strip alternate leaflets,which were brittle,easily broken,weak in smell,mild in flavor. Cork cell surface and lower epidermal cell surface showed polygon;most of xylon were bunched;there were many clusters of calcium oxalate. TLC spots were clear and well-separated. The contents of moisture,total ash,acid-insoluble ash, water-soluble extract and ethanol were 6.83%-8.12%,4.01%-5.01%,1.06%-1.98%,17.91%-22.65%,11.29%-15.51%. The linear range of gallic acid were 3.13-50 μg/mL(r=0.9997);RSDs of precision,stability and reproducibility tests were lower than 1.0%;the recoveries were 94.0%-100.8%(RSD=2.27%,n=9). CONCLUSIONS:Established standard can be used for quality evalua-tion of Tibetan medicine M. germanica.