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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。
OBJECTIVE: To investigate the TLC identification and determination of garlic in Chinese Pharmacopoeia (2010 edition) according to the United States Pharmacopoeia, the European Union Pharmacopoeia and the British Pharmacopoeia. Methods: The sample was treated by microwave enzyme inactivation method, and the garlic was identified by TLC. The cation exchange column was used, the mobile phase was phosphate buffer solution, the flow rate was 0.5 mL.min-1 and the detection wavelength was 214 nm. Alliin content. Results: The same spot was detected by TLC on the medicinal materials of Garlic from different areas with the same Rf value as that of alliin and arginine reference substance. The established alliin HPLC method, the methodological experiments showed that the alliin concentration in the range of 31.2 ~ 374.4μg.mL-1 showed a good linear relationship (r = 0.9999); low, medium and high concentration average recovery (n = 9) were 102.8% (RSD = 4.0%), 101.8% (RSD = 3.0%) and 111.0% (RSD = 3.8%). Conclusion: This study established the determination of garlic herbs by TLC and HPLC method, which can be used for qualitative and quantitative analysis of garlic medicinal materials, which is recommended as a reference for further study of garlic quality standards.