芜菁子化学成分的基础研究
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摘要
目的:研究芜菁子(Brassica rapa L.seed)的化学成分并建立芜菁子中有效成分含量测定的方法。方法:①将芜菁的干燥种子用95%乙醇提取,浸膏经过不同极性的溶剂萃取后得到四个部位:石油醚部位、乙酸乙酯部位、正丁醇部位、水部位。石油醚部位、乙酸乙酯部位、正丁醇部位再采用硅胶柱层析、大孔吸附树脂、Sephadex LH-20、制备薄层色谱、重结晶等方法进行分离纯化,利用现代波谱技术(1H-NMR,13C-NMR)并结合化学方法对化合物结构进行解析;②采用气相色谱法测定芜菁子油脂中6种脂肪酸的含量;③采用高效毛细管电泳法测定芜菁子多糖中单糖的组成。结果:①从芜菁子石油醚部位、乙酸乙酯部位、正丁醇部位分离得到了9个化合物,其中鉴定了8个化合物的结构,分别为齐墩果酸(1)、β-谷甾醇(2)、软脂酸单甘油脂(3)、邻苯二甲酸二丁酯(4)、熊果酸(5)、槲皮素(6)、山萘酚-3-O-芸香糖苷(7)、5-羟基-3’,4’,6,7-四甲氧基黄酮(8);②通过采用气相色谱法测定芜菁子油脂中6种脂肪酸的含量,结果表明,软脂酸、硬脂酸、油酸、亚油酸、亚麻酸、芥酸的含量分别为19.99mg/g、2.22mg/g、25.63mg/g、31.67mg/g、12.06mg/g、50.94mg/g;③通过采用高效毛细管电泳法测定芜菁子多糖中单糖的组成,由校正因子法计算得知芜菁子多糖中阿拉伯糖、葡萄糖、鼠李糖、半乳糖、甘露糖、葡萄糖醛酸、半乳糖醛酸摩尔比为8.09/1.79/0.28/5.11/0.78/0.32/0.38。结论:①化合物(1)、(3)、(4)、(5)、(6)、(7)、(8)为首次从芜菁子中得到;②用气相色谱法测定芜菁子油脂中6种脂肪酸含量的方法,其精密度好,准确可靠;③用高效毛细管电泳法测定芜菁子多糖中单糖的组成,该方法操作简便,稳定可行。
Objective: To study the chemical constituents of Brassica rapa L. seed. and to establishes the method of determination the content of active ingredients in Brassica rapaL. seed. Methods:①The dry seed of Brassica rapa L. were extracted with 95% EtOH. The 95% EtOH extract was distributed with solvents of diffrernt polarity into four fractions, namely the petroleum ether fraction, EtOAc fraction, BuOH fraction and H2O fractions. Then adopt silica gel column chromatography, macroporous adsorptive resins, sephadex LH-20, preparation of thin layerchromatography, crystallization and recrystallization for separation and purification of the petroleum ether fraction, EtOAc fraction, BuOH fraction. Apply chemical method and modern spectroscopy such as 1H-NMR, 13C-NMR to identify the structure of the compounds.②To assay six acids in the fatty oil of Brassica rapa L. seed by GC.③To assay the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE. Results:①Nine monomer compounds were isolated from petroleum ether fraction, EtOAc fraction and BuOH fraction. to identify eight structure of the compounds, they were identified as oleanolic acid (1),β-sitosterol (2), palmitic monoglycerolester (3), dibutylphthalate (4), ursolicacid (5), quercetin (6), kaempferol-3-O-rutinoside (7), 5-hydroxy-3’,4’,6,7- tetramethoxyflavone (8).②Through to assay six acids in the fatty oil of Brassica rapa L. seed by GC, the experimental result to indicate that the content of palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid and erucic acid were 19.99mg/g, 2.22mg/g, 25.63mg/g, 31.67mg/g, 12.06mg/g, 50.94mg/g.③Through to determine the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE, to calculate the molar ratio of arabinose, amylaceum, rhamnose, galactose, mannose, glycuronic acid, galacturonic acid were 8.09/1.79/0.28/5.11/0.78/0.32/0.38 bycorrection factor method. Conclusion:①We study the chemical compositions of Brassica rapa L. seed., the compound (1), (3), (4), (5), (6), (7), (8) were discovered in Brassica rapa L. seed. for the first time.②To determine the content of effective constituent in Brassica rapa L. seed. by GC, the method were perfect, accurate, and reliable.③To assay the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE, the method were convenient and feasible.
Objective: To study the chemical constituents of Brassica rapa L. seed. and to establishes the method of determination the content of active ingredients in Brassica rapaL. seed. Methods:①The dry seed of Brassica rapa L. were extracted with 95% EtOH. The 95% EtOH extract was distributed with solvents of diffrernt polarity into four fractions, namely the petroleum ether fraction, EtOAc fraction, BuOH fraction and H2O fractions. Then adopt silica gel column chromatography, macroporous adsorptive resins, sephadex LH-20, preparation of thin layerchromatography, crystallization and recrystallization for separation and purification of the petroleum ether fraction, EtOAc fraction, BuOH fraction. Apply chemical method and modern spectroscopy such as 1H-NMR, 13C-NMR to identify the structure of the compounds.②To assay six acids in the fatty oil of Brassica rapa L. seed by GC.③To assay the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE. Results:①Nine monomer compounds were isolated from petroleum ether fraction, EtOAc fraction and BuOH fraction. to identify eight structure of the compounds, they were identified as oleanolic acid (1),β-sitosterol (2), palmitic monoglycerolester (3), dibutylphthalate (4), ursolicacid (5), quercetin (6), kaempferol-3-O-rutinoside (7), 5-hydroxy-3’,4’,6,7- tetramethoxyflavone (8).②Through to assay six acids in the fatty oil of Brassica rapa L. seed by GC, the experimental result to indicate that the content of palmitic acid, stearic acid, oleic acid, linoleic acid, linolenic acid and erucic acid were 19.99mg/g, 2.22mg/g, 25.63mg/g, 31.67mg/g, 12.06mg/g, 50.94mg/g.③Through to determine the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE, to calculate the molar ratio of arabinose, amylaceum, rhamnose, galactose, mannose, glycuronic acid, galacturonic acid were 8.09/1.79/0.28/5.11/0.78/0.32/0.38 bycorrection factor method. Conclusion:①We study the chemical compositions of Brassica rapa L. seed., the compound (1), (3), (4), (5), (6), (7), (8) were discovered in Brassica rapa L. seed. for the first time.②To determine the content of effective constituent in Brassica rapa L. seed. by GC, the method were perfect, accurate, and reliable.③To assay the composition of monosaccharide in the polysaccharide of Brassica rapa L. seed. by HPCE, the method were convenient and feasible.
引文
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