红背桂药材的质量标准研究

Study on Quality Standard of Excoecaria cochinchinensis

目的:制订红背桂药材的质量标准,为其开发利用提供科学依据。方法:分别对红背桂药材的性状、显微特征进行观察鉴别;按照《中国药典》方法对10个不同产地药材中浸出物、灰分和水分进行测定;以没食子酸为对照品,采用薄层色谱(TLC)法对其进行定性鉴别;采用高效液相色谱法测定药材中没食子酸的含量:色谱柱为迪马C18(250mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸水(10∶90,V/V),检测波长为273nm。结果:对红背桂药材的性状、显微特征进行了描述。暂定红背桂药材中总灰分不得过11%,不溶性灰分不得过3%,水浸出物不得少于12%,醇浸出物不得少于14%,水分不得过12%。TLC中主斑点清晰、分离度好。没食子酸的进样量在0.0095～1.9000μg范围内与其峰面积积分值呈良好的线性关系(r=0.9999);精密度、稳定性、重复性试验的RSD均<2%;平均加样回收率为101.93%,RSD=1.67%(n=6)。结论:所建标准可用于红背桂药材的质量控制。

OBJECTIVE： To provide scientific basis for the utilization and development of Excoecaria cochinchinensis by setting up the quality standard of E. cochinchinensis. METHODS： The property and microscopic characteristics of E. cochinchinensis were determined respectively. Extract, moisture and ash of medicinal material from 10 producing areas were determined according to Chinese Pharmacopeia; E. cochinchinensis was qualitatively determined by TLC using gallic acid as control; the content of gallic acid was determined by HPLC： the determination was performed on Diamonsil C18（250 mm×4.6 mm,5 μm） column with mobile phase consisted of methanol-0.1% phosphoric acid （10 ∶ 90,V/V）. The detection wavelength was set at 273 nm. RESULTS： The property and microscopic characteristics of E. cochinchinensis were described. The contents of total ash, acid-insoluble ash, aqueous extract, ethanol extract and moisture were no more than 11%, 3%, 12%, 14% and 12%. TLC spots were clear and well-separated without interference from negative control. The linear range of gallic acid were 0.009 5-1.900 0 μg（r=0.999 9）; RSDs of precision, stability and reproducibility tests were all lower than 2%; average recovery rates were 101.93%（RSD=1.67%,n=6）. CONCLUSIONS： The established standard can be used for the quality control of E. cochinchinensis.