Method for purifying rebaudioside c
一种乙酸乙酯、丁醇的技术,应用在化学仪器和方法、有机化学、糖衍生物等方向,能够解决产率物质纯度未公开等问题
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Embodiment 1
[0034] Example 1; Initial Purification of Rebaudioside C from Crude Extract
[0035] Using a number of different solvent systems, a mixture of acetone and water was observed to be a suitable solvent for the recrystallization of rebaudioside C from the crude starting material (i.e., the "waste" produced in the rebaudioside A production process) . Therefore, the yield of recrystallized rebaudioside C from the starting material was determined. For these experiments, the crude starting material was mixed with acetone / water (85 / 15, w / w). Typically, for 1 g of solid, 4-6 g of solvent is used. The mixture was heated to 48°C and all solids were allowed to dissolve. The mixture was cooled to room temperature and stirred for 3-4 days. The solution was filtered to collect a white precipitate, which was then washed with acetone and dried under vacuum at 50°C for 8 hours.
[0036] Table 2
[0037] Amount of crude starting material
RebC content in crude product
The am...
Embodiment 2
[0047] Example 2: Purification of Rebaudioside C
[0048] 20 g of starting material are dissolved in 500 ml of a THF / water mixture containing 70-80% (preferably 75% (v / v)) water. The resulting solution was extracted twice with 500 ml of ethyl acetate / 1-butanol mixture (85 / 15, v / v). The 1-butanol / ethyl acetate layer was removed.
[0049] The THF-water phase is then further extracted twice with 500 ml of an ethyl acetate / butanol mixture containing 30-40% 1-butanol, preferably 35% (v / v). The ethyl acetate / butanol layers from the two extractions were combined and concentrated under vacuum to give 8.70 g of material. It was determined by HPLC analysis that the content of rebaudioside C in this substance reached 24.5% (Table 5).
[0050] table 5
[0051] Retention time (minutes)
components
total percentage
12.702
unknown
1.10
15.722
unknown
4.62
18.547
unknown
4.20
22.811
unknown
1.06
24.473
...
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