Methods for purifying proanthocyanidin oligomers
一种原花色素、低聚物的技术，应用在有机化学等方向，能够解决不适合工业分离方法等问题
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Embodiment 1
[0077] Example 1 Purification by solid-liquid extraction (A)
[0078] 300 ml of methyl acetate was added to 30 g of the proanthocyanidin fraction obtained in Reference Example 1, and then solid-liquid extraction was performed at room temperature for 1 hour. The extraction was carried out twice in total, and the extracts from the two extractions were combined and filtered. Next, the extracted residue was washed with a small amount of methyl acetate. The methyl acetate extracts and washings were combined and concentrated under reduced pressure. A small amount of distilled water was added thereto, followed by concentration again under reduced pressure, and the extracted components were dissolved in an aqueous solution. The resulting aqueous solution was freeze-dried to obtain 17.5 g of a powdery methyl acetate extract. Then, the extraction residue was dried to obtain 12.5 g of a powdery non-extract after extraction with methyl acetate. The contents of dimeric and trimeric pro...
Embodiment 2
[0081] Example 2 Purification by Solid-Liquid Extraction (B)
[0082] Methyl acetate and different solvents were mixed in a volume ratio of 9:1 (when mixing with methyl acetate:hexane, the ratio was 9:5), thus preparing a solvent for solid-liquid extraction. Among the various solvents used are methyl acetate-miscible organic solvents: methanol, ethanol, propanol, butanol, ethyl formate, ethyl acetate, acetone, acetonitrile, tetrahydrofuran, hexane or acetic acid. 10 ml of a solvent for extraction was added to 1 g of each proanthocyanidin fraction obtained in Reference Example 1, and the mixture was subjected to solid-liquid extraction at room temperature for 1 hour (single extraction). After removing solid components from the extract by centrifugal filtration, a certain amount of the extract was diluted 100-fold with distilled water (0.01→1 ml). The contents of PB1, PB2 and PC1 were then measured by the reversed-phase liquid chromatography described in Reference Example 2. A...
Embodiment 3
[0084] Example 3 Purification by Solid-Liquid Extraction (C)
[0085] Methyl acetate and ethyl acetate were mixed at the volume ratios listed in Table 3, followed by solid-liquid extraction. 10 ml of solvents for extraction having different volume ratios were added to 1 g of each proanthocyanidin fraction obtained in Reference Example 1, followed by solid-liquid extraction at 30° C. for 1.5 hours. This step was repeated three times. These extracts were combined, concentrated under reduced pressure, and freeze-dried, whereby a powdery product (extract) was obtained. The contents of PB1, PB2 and PC1 in the powder product were measured by reversed-phase liquid chromatography described in Reference Example 2. Table 3 has listed the result with the solvent extraction of different volume ratios, comprises the total yield (%) of solid content yield (%), PB1, PB2 and the total yield of PC1 and the total yield of PC1, PB2 and PC1 respectively purity.
[0086] solvent for e...
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