苗药酢浆草药材的质量标准研究

Study on the Quality Standards of Miao Medicine Oxalis corniculata

目的:完善和提高苗药酢浆草药材的质量标准,为其深度开发提供科学依据。方法:以采集自贵州、安徽、河南等地的12批酢浆草药材为样品。观察其药材粉末的显微特征;按2015年版《中国药典》(四部)通则相关方法,对其进行薄层色谱(TLC)鉴别[展开剂为三氯甲烷-甲醇-甲酸(8:1:0.1,V/V/V)]和水分、总灰分、酸不溶性灰分及醇溶性浸出物的含量测定;采用高效液相色谱(HPLC)法测定其中异牡荆苷含量[色谱柱为Venusil XBP C18(L),流动相为乙腈-0.1%磷酸溶液(15:85,V/V),流速为1 mL/min,柱温为35℃,检测波长为338 nm,进样量为10μL]。结果:显微观察可见,本品粉末呈灰褐色至黄褐色,具有非腺毛甚多、纤维纹孔明显等特点;TLC鉴别结果显示,在供试品色谱上与对照药材色谱相应位置显相同颜色的斑点;12批药材的水分含量为6.66%~12.13%,总灰分含量为9.16%~13.79%,酸不溶性灰分含量为1.58%~4.63%,醇溶性浸出物含量为5.22%~15.79%;HPLC测定结果显示,异牡荆苷质量浓度在5.20~78.3μg/mL范围内与其峰面积具有良好的线性关系(r=0.999 0),重复性(n=9)、中间精密度(n=6)、稳定性(24 h,n=6)试验的RSD均<2.0%,加样回收率为97.54%~99.52%(RSD=0.74%,n=6),12批酢浆草药材中异牡荆苷的含量为0.036%~0.144%(n=3)。结论:本研究建立了苗药酢浆草定性、定量鉴别的方法,对提升酢浆草药材的质量标准有一定参考价值。

OBJECTIVE:To provide scientific basis for the utilization and development of Miao medicine Oxalis corniculata by promoting the quality standard of it.METHODS:Total of 12 batches of O.corniculata were collected from Guizhou,Anhui and Henan,etc.Microscopic characteristics of 12 batches of O.corniculata powder were observed.According to the corresponding methods in 2015 edition of Chinese Pharmacopoeia(part IV),TLC was used for qualitative identification[developing solvent was trichloromethane-methanol-formic acid(8:1:0.1,V/V/V)],and the contents of moisture,total ash,acid insoluble ash and alcohol soluble extractive from 12 batches of O.corniculata were determined.The content of isovitexin was determined by HPLC.The determination was performed on Venusil XBP C18(L)with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution(15:85,V/V)at the flow rate of 1 mL/min.The column temperature was 35 ℃,and the detection wavelength was set at 338 nm.The sample size was 10μL.RESULTS:Microscopic observation showed that the powder was grayish brown to yellowish brown,with many non-glandular hairs and obvious fibrous pore.Results of TLC identification showed that the spots of the same color appeared in the corresponding positions of the test and the control chromatogram.The contents of moisture,total ash,acid insoluble ash and alcohol soluble extract from samples were 6.66%-12.13%,9.16%-13.79%,1.58%-4.63% and 5.22%-15.79%,respectively.Results of HPLC method showed that the concentration of isovitexin showed a good linear relationship in the range of5.20-78.3 μg/mL(r=0.999 0);RSDs of reproducibility(n=9),intermediate precision(n=6)and stability(24 h,n=6)tests were all lower than 2.0%;and the recovery rates were 97.54%-99.52%(RSD=0.74%,n=6);the contents of isovitexin in 12 batches of O.corniculata were 0.036%-0.144%(n=3).CONCLUSIONS:Qualitative and quantitative identification methods of O.corniculate were established,which can be used as a reference for improving the quality standard of O.corniculata.