Polymorphic substance of alpha-lipoic acid as well as preparation method and application of polymorphic substance
A technology of lipoic acid and crystals, which can be used in applications, food preparation, medical preparations containing active ingredients, etc., and can solve problems such as poor thermal stability
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Embodiment 1
[0026] Example 1 Preparation of ɑ-lipoic acid crystal Ⅰ
[0027] 4.5g of lipoic acid was added to 40ml of n-hexane and 10ml of ethyl acetate, and stirred in a water bath at 50°C for 1 hour. The solution was cooled to 20°C, filtered, and dried under vacuum to obtain 2.9 g of crystal I with a yield of 64.44%.
[0028] PXRD pattern of crystal Ⅰ (radiation source is CuKα 1 )for figure 1 As shown, there are diffraction peaks at 2θ values of 7.96, 11.92, 13.88, 17.82, 18.20, 23.32, 23.98, 24.46, 25.60, 31.66, 32.16, 40.52, 43.86, 49.06, and the error range of 2θ values is ±0.2.
[0029] The DSC spectrum of crystal Ⅰ is as follows figure 2 As shown, there is an endothermic peak at 64.50±5.0°C.
Embodiment 2
[0030] Example 2 Preparation of ɑ-lipoic acid crystal Ⅱ
[0031] 4.1g of lipoic acid was added to 25ml of petroleum ether and 7.5ml of ethyl acetate, and stirred in a water bath at 50°C for 1 hour. The solution was cooled to 20°C, filtered, and vacuum-dried to obtain 2.5 g of crystal II with a yield of 60.98%.
[0032] PXRD pattern of crystal Ⅱ (radiation source is CuKα 1 )Such as image 3 As shown, there are diffraction peaks at 2θ values of 11.88, 13.86, 17.26, 17.80, 18.16, 20.78, 23.32, 23.92, 25.60, 27.96, 28.96, 36.06, and the error range of 2θ values is ±0.2.
[0033] The DSC spectrum of crystal Ⅱ is Figure 4 , It has an endothermic peak at 62.74±5.0℃.
Embodiment 3
[0034] Example 3 ɑ-lipoic acid crystal Ⅰ tablets
[0035] prescription:
[0036]
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