Huperzine A polymorphism body, preparation method thereof, pharmaceutical composition comprising polymorphism body and application thereof
A technology for huperzine A and crystal form, which is applied in the field of preparation of huperzine A polymorph and its synthesis process research field, and can solve problems such as the raw material crystal form of huperzine A is not involved
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Embodiment 1
[0056] Example 1: Preparation of huperzine A crystal form I.
[0057] Mix 50 mg of huperzine A raw material (amorphous) with 1 ml of acetone, heat to 50° C. and keep stirring at 50° C. for 3 days, and filter to obtain a white solid. After evaporating the solvent at room temperature, the white solid was dried under reduced pressure with an oil pump for 12 hours to obtain a crystalline powder, which was determined by X-ray powder diffraction, showing that the obtained crystal form was Form I. The specific peak positions are shown in Table 1 below.
[0058] Table 1: X-ray powder diffraction data of Huperzine A crystal form I in Example 1 of the present invention
[0059]
[0060] Other tests were carried out on the obtained sample, and the obtained DSC thermal spectrum, infrared spectrum and Raman spectrum were as follows: Figure 1b , 1c , 1d shown.
Embodiment 2
[0061] Example 2: Preparation of huperzine A crystal form II.
[0062] Put 25 mg of huperzine A crystal form I in an oven at 125 degrees Celsius and heat for 2 hours to obtain a crystalline powder, which was determined by X-ray powder diffraction to show that the obtained crystal form was crystal form II. The specific peak positions are shown in Table 2 below.
[0063] Table 2: X-ray powder diffraction data of Huperzine A crystal form II in Example 2 of the present invention
[0064]
[0065]
[0066] Other tests were carried out on the obtained sample, and the obtained DSC thermal spectrum, infrared spectrum and Raman spectrum were as follows: Figure 2b , 2c , as shown in 2d.
Embodiment 3
[0067] Example 3: Preparation of huperzine A crystal form III.
[0068] Mix 50 mg of huperzine A crystalline form I with 1 ml of acetonitrile, heat to 50° C. and keep stirring at 50° C. for 2 days, and filter to obtain a white solid. After evaporating the solvent at room temperature, the white solid was placed in a vacuum drying oven at 100°C, and dried for 24 hours under vacuum with an oil pump to obtain a crystalline powder, which was determined by X-ray powder diffraction, showing that the obtained crystal form was crystal Type III. The specific peak positions are shown in Table 3 below.
[0069] Table 3: X-ray powder diffraction data of Huperzine A crystal form III in Example 3 of the present invention
[0070]
[0071] Other tests were carried out on the obtained sample, and the obtained DSC thermal spectrum, infrared spectrum and Raman spectrum were as follows: Figure 3b , 3c , 3d shown.
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