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目的建立高速逆流色谱技术分离纯化钩吻素己和1-甲氧基钩吻碱的方法。方法采用高速逆流色谱分离技术分离纯化钩吻生物碱单体,以氯仿-甲醇-0.1mol/LHCl(4:4:2)为溶剂体系;高效液相色谱技术分析所提产物的质量分数;核磁共振谱、质谱分析确证单体的化学结构。结果从300mg钩吻总碱中经过一次高速逆流色谱技术分离纯化获得19.4mg钩吻素己和21.2mg1-甲氧基钩吻碱,质量分数分别为95.4%、98.6%;经过电喷雾质谱及核磁共振的结构鉴定分析,证实分离得到的两种生物碱分别是钩吻素己和1-甲氧基钩吻碱。结论高速逆流色谱技术可高效分离纯化钩吻素己和1-甲氧基钩吻碱,为钩吻生物碱的研发提供了制备技术。
Objective To establish a high-speed counter-current chromatographic technique for the separation and purification of crocin and 1-methoxyl-Galstonine. Methods High-speed countercurrent chromatographic separation technology was used to separate and purify the homogenized alkaloids. Chloroform-methanol-0.1mol/L HCl (4:4:2) was used as the solvent system. The mass fraction of the product was analyzed by high performance liquid chromatography. Resonance spectroscopy and mass spectrometry confirmed the chemical structure of the monomer. RESULTS Separation and purification of 300 mg of the total alkaloids from Crotalula argenteus resulted in 19.4 mg of clomazone and 21.2 mg of 1-methoxy-l-quercetin. The mass fractions were 95.4% and 98.6%, respectively; electrospray ionization mass spectrometry and nuclear magnetic resonance were performed. The structural identification analysis of the resonance confirmed that the two isolated alkaloids were Crocin and 1-methoxyl-olactone. Conclusion High-speed counter-current chromatography can be used to separate and purify the gentamicin and 1-methoxylcomicin efficiently, which provides a preparation technique for the research and development of genus alkaloids.