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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

Inactive Publication Date: 2014-06-25
NANJING REAL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The melting point of ɑ-lipoic acid is 58-61 ° C, poor thermal stability, easy to polymerize under aerobic conditions

Method used

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  • Polymorphic substance of alpha-lipoic acid as well as preparation method and application of polymorphic substance
  • Polymorphic substance of alpha-lipoic acid as well as preparation method and application of polymorphic substance
  • Polymorphic substance of alpha-lipoic acid as well as preparation method and application of polymorphic substance

Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to a polymorphic substance of alpha-lipoic acid as well as a preparation method and an application of the polymorphic substance. The polymorphic substance has novel spectral line characteristics in a powder X-ray diffraction spectrum. The polymorphic substance can be applied to medicine production, food additives and healthcare products.

Description

technical field [0001] The invention relates to a polymorph of α-lipoic acid, a preparation method and application of the polymorph. Background technique [0002] Polymorphism refers to the phenomenon that solid substances form solid states with different physical and chemical properties in two or more different spatial arrangements. Drug molecules often exist in different solid forms, including salts, polymorphs, co-crystals, amorphous, hydrates, and solvates. Different crystal forms of the same drug will have significant differences in terms of crystal structure, stability, dissolution, dissolution performance, manufacturability, and bioavailability, which will have an important impact on the efficacy and developability of the drug. In view of the importance of drug crystal forms, both FDA and SFDA have put forward clear regulations on this in drug declarations, requiring research on drug polymorphism and providing corresponding data. Therefore, the research and developm...

Claims

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Application Information

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IPC IPC(8): C07D339/04A61K31/385A61P3/10A23L1/30A23L33/10
CPCC07D339/04A23L33/10
Inventor 叶海晁阳包玉胜
Owner NANJING REAL PHARMA
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