Crystallization of β-sitosterol using a water-immiscible solvent hexane
Crystallization of β-sitosterol using a water-immiscible solvent hexane
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DOI：
10.1252/jcej.39.869
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发表时间：
2006-08
影响因子：
0.8
通讯作者：
H. Kawachi;R. Tanaka;Masaru Hirano;Koichi Igarashi;H. Ooshima
中科院分区：
文献类型：
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作者：
H. Kawachi;R. Tanaka;Masaru Hirano;Koichi Igarashi;H. Ooshima
进行作为一种植物甾醇的β-谷甾醇的冷却结晶，其中使用含有ppm水平的水的水不混溶性溶剂己烷作为溶剂。本工作中采用的水和β-谷甾醇浓度的初始比例分别为330/10、1315/10和645/20 ppm/（g/L），分别对应于水/β-谷甾醇摩尔比为0.51、2.0和0.50。当水与β-谷甾醇的初始浓度比为1315/10 ppm/（g/L）时，沉淀出薄板状晶体，经鉴定为β-谷甾醇的一水合物晶体。另一方面，当水和β-谷甾醇浓度的初始比率为645/20 ppm/（g/L）时，沉淀出半水合物的针状晶体。这一结果意味着水的ppm水平对假多晶型起重要作用。由于β-谷甾醇半水合物的晶体结构未见报道，我们通过单晶XRD分析确定了它。
Cooling crystallization of β-sitosterol that is a kind of phytosterol was carried out, where a water-immiscible solvent hexane containing a ppm level of water was used as a solvent. The initial ratio of water and β-sitosterol concentration adopted in this work was 330/10, 1315/10 and 645/20 ppm/(g/L), which corresponded to 0.51, 2.0, and 0.50 in water/β-sitosterol mole ratio, respectively. When the initial ratio of water and β-sitosterol concentration was 1315/10 ppm/(g/L), thin plate-like crystals were precipitated and were identified as the monohydrate crystals of β-sitosterol. On the other hand, when the initial ratio of water and β-sitosterol concentration was 645/20 ppm/(g/L), needle-like crystals of hemihydrate were precipitated. This result meant that the ppm level of water plays an important role for the pseudo-polymorphism. Since the crystal structure of β-sitosterol hemihydrate had never been reported, we determined it by a single crystal XRD analysis.