大蒜质量标准中商榷内容的研究

目的:参照美国药典、欧盟药典和英国药典对2010版中国药典收载的大蒜薄层鉴别和含量测定等进行研究。方法:采用微波灭酶法处理样品,对大蒜药材进行薄层色谱鉴别;采用阳离子交换色谱柱,以磷酸盐缓冲溶液为流动相,流速0.5 mL.min-1,检测波长214 nm,测定大蒜药材中蒜氨酸含量。结果:不同产地大蒜药材的薄层色谱在与蒜氨酸和精氨酸对照品斑点Rf值相同的位置上,均检出相同的斑点。建立的蒜氨酸含量测定HPLC法,经方法学实验表明,蒜氨酸浓度在31.2～374.4μg.mL-1范围内呈良好线性关系(r=0.9999);低、中、高浓度平均回收率(n=9)分别为102.8%(RSD=4.0%),101.8%(RSD=3.0%),111.0%(RSD=3.8%)。结论:本研究建立了大蒜药材的薄层色谱鉴别和高效液相色谱含量测定方法,可用于大蒜药材的定性与定量分析,建议作为大蒜质量标准进一步研究的参考。

Study on the discussion about quality specification of garlic

Objective:To study on the thin-layer chromatographic identification method and the assay method for garlic in Chinese Pharmacopoeia(2010)with reference to USP,EP and BP.Method: The enzyme activity was inhibited by micro-wave,and garlic was identified by thin-layer chromatography.The content of alliin in garlic was performed on a cation exchange chromatography column,with the phosphate buffered solution as the mobile phase,at the flow rate of 0.5 mL·min-1 and the detected wavelength was 214 nm.Results: The thin-layer chromatograms of garlic from different regions showed spots corresponding in Rf value to that obtained from the chromatograms of standard solution alliin and arginine.The method experiment of the established HPLC to detect the content of alliin showed that the calibration curve of alliin was linear in the range of 31.2-374.4 μg·mL-1(r=0.9999)and the average recoveries(n=9)at low,medium and high concentration were 102.8%(RSD=4.0%),101.8%(RSD=3.0%),111.0%(RSD=3.8%),respectively.Conclusion: The TLC identification and assay methods for garlic were established in this study.The methods can be used in the quantitative and qualitative analysis of garlic,which was suggested to be referenced in the further study of the quality specification of garlic.