Reduced coenzyme Q10 crystal with excellent stability and composition containing said reduced coenzyme Q10 crystal
A technology of reduction and composition, applied in the field of crystallization of reduced coenzyme Q10, which can solve the problems of mixing and difficult removal
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reference example 1
[0112] Add 100g of oxidized coenzyme Q to 1000g of ethanol 10 , 60g of L-ascorbic acid, stirred at 78°C for reduction reaction. After 30 hours, it was cooled to 50°C, and 400 g of ethanol and 100 g of water were added while maintaining the same temperature. While stirring the ethanol solution (the power required for stirring is 0.3kW / m 3 ), while cooling to 2°C at a rate of 10°C / hour, a white slurry was obtained. The obtained slurry was filtered under reduced pressure, and the wet crystals were washed in the order of cold ethanol, cold water, and cold ethanol, and then the wet crystals were dried under reduced pressure (20~35℃, 1~30mmHg), thereby obtaining a white 95 g of dried crystals (apparent yield (positive yield) 95 mol%). In addition, all operations except for drying under reduced pressure were performed under a nitrogen atmosphere. The obtained crystallized reduced coenzyme Q 10 / Oxidized Coenzyme Q 10 The weight ratio is 99.5 / 0.5.
Embodiment 1
[0114] The 10g reduced coenzyme Q obtained in Reference Example 1 10 (Reduced Coenzyme Q 10 / Oxidized Coenzyme Q 10 The weight ratio of 99.5 / 0.5) was added to 190g rapeseed oil at 25℃, while stirring at 60℃ (the power required for stirring was 0.3kW / m 3 ) While making reduced coenzyme Q 10 completely dissolved. While stirring (the power required for stirring is 0.3kW / m 3 ), while crystallizing at a cooling rate of 10°C / hour. In addition, all the above operations are performed under a nitrogen atmosphere. The obtained slurry was filtered under reduced pressure, and after sufficiently washing with hexane, the wet crystals were dried under reduced pressure (20 to 35°C, 1 to 30 mmHg), thereby obtaining a Cu-Kα-ray X-ray diffraction method. X-ray diffraction pattern such as figure 1 Reduced coenzyme Q shown 10 Crystal 8.7g. In the above-mentioned X-ray diffraction pattern, this crystal has intermediate intensity peaks at a diffraction angle (2θ) of 3.1°, strong peaks at 20.2° and 23.0...
Embodiment 2
[0116] The 10g reduced coenzyme Q obtained in Reference Example 1 10 (Reduced Coenzyme Q 10 / Oxidized Coenzyme Q 10 The weight ratio of 99.5 / 0.5) was added to 190g of medium-chain fatty acid triglycerides (MCT, carbon number 8: carbon number 10 = 6:4) at 25°C, while stirring at 60°C (the power required for stirring) 0.3kW / m 3 ) While making reduced coenzyme Q 10 completely dissolved. While stirring (the power required for stirring is 0.3kW / m 3 ), while cooling to 5°C at a cooling rate of 10°C / hour to precipitate crystals. In addition, all the above operations are performed under a nitrogen atmosphere. The obtained slurry was filtered under reduced pressure, and after sufficiently washing with hexane, the wet crystals were dried under reduced pressure (20 to 35°C, 1 to 30 mmHg), thereby obtaining 6.5 g of reduced coenzyme Q 10 crystallization. The obtained crystallized reduced coenzyme Q 10 / Oxidized Coenzyme Q 10 The weight ratio is 99.3 / 0.7.
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