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目的:建立高速逆流色谱(HSCCC)法分离制备山芝麻中三萜类成分的方法。方法:山芝麻乙酸乙酯萃取部位采用二步分离法进行HSCCC分离;所得各组分用质谱与核磁共振波谱法进行结构鉴定,并用红外光谱法进行表征分析。结果:从山芝麻乙酸乙酯萃取部位分离制备得到6个化合物,各化合物经鉴定为:山芝麻宁酸甲酯(1)、山芝麻酸甲酯(2)、山芝麻宁酸(3)、山芝麻酸(4)、白桦脂酸(5)、齐墩果酸(6)。6个化合物进行HPLC分析,质量分数均大于95.0%。结论:HSCCC适用于分离制备山芝麻中的三萜类成分,方法快速,可以实现产品高纯度和高得率的制备。
OBJECTIVE: To establish a method for the separation and preparation of triterpenoids from Sesame (Sesamum indicum) by high-speed countercurrent chromatography (HSCCC). Methods: Two-step separation method was used to separate the ethyl acetate extract of mountain sesame seeds by HSCCC. The components were identified by mass spectrometry and nuclear magnetic resonance spectroscopy and characterized by infrared spectroscopy. Results: Six compounds were isolated and purified from the ethyl acetate extract of Sesame seeds. The compounds were identified as: Sesamonic acid methyl ester (1), Sesaminic acid methyl ester (2), Sesamonic acid (3) Sesanic acid (4), Betulinic acid (5), oleanolic acid (6). Six compounds were analyzed by HPLC with the mass fraction greater than 95.0%. Conclusion: HSCCC is suitable for the separation and preparation of triterpenoids from Sesamica sesame. The method is rapid and can be used for the preparation of products with high purity and high yield.