Crystal forms of bellidifolin as well as preparation method and pharmaceutical compositions of crystal forms
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A kind of technology of gentianone and daisy leaves, applied in the field of medicine
Inactive Publication Date: 2015-03-25
吕丽娟
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Problems solved by technology
But so far, there is no literature report on the characteristics of the daisy leaf gentianone crystal form and its preparation method
Method used
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Embodiment 1
[0052] Weigh 1.0g of daisy leaf gentianone, add 115mL of ethanol, heat to reflux until dissolved, filter while hot, remove the solvent from the solution under reduced pressure, collect samples, and vacuum dry at 30°C to obtain daisy leaf gentianone crystals Type I. Its powder X-ray diffraction pattern is shown in figure 1 , 2 , FTIR see image 3 . Infrared spectrum at 3438, 3104, 3017, 2986, 2950, 2848, 2381, 2349, 1872, 1657, 1632, 1613, 1594, 1563, 1497, 1433, 1399, 1356, 1314, 1267, 1244, 1208, 1185, 1158, 1094, 1049, 1032, 993, 960, 882, 835, 824, 806, 757, 698, 672, 634, 590, 520, 481, 460cm -1 There is an absorption peak. The main characteristic parameters of the powder X-ray diffraction patterns are shown in Table 1.
[0053] Table 1 Main characteristic parameters of powder X-ray diffraction pattern of daisy leaf gentianone form Ⅰ
[0054]
[0055] Example 2
Embodiment 2
[0057] Weigh 1.0g of daisy leaf gentianone, add 45mL of acetone, heat to 50°C, stir and dissolve, then filter while hot, remove the solvent from the solution under normal pressure, collect samples, and vacuum dry at 35°C to obtain daisy leaf gentianone Cholesterone crystal form I. Its powder X-ray diffraction and infrared spectrum detection results are consistent with the results of Example 1.
[0058] Example 3
Embodiment 3
[0060] Weigh 1.0 g of daisy leaf gentianone, add 20 mL of tetrahydrofuran, heat to 60°C, stir and dissolve, then filter while hot, remove the solvent from the solution under normal pressure, collect samples, and vacuum dry at 50°C to obtain daisy leaf gentianone Cholesterone crystal form I. Its powder X-ray diffraction and infrared spectrum detection results are consistent with the results of Example 1.
[0061] Example 4
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Abstract
The invention relates to crystal forms I, II, III and VI of bellidifolin as well as a preparation method and pharmaceutical compositions of the crystal forms. The preparation method comprises the following steps: heating and stirring or refluxing and dissolving in a solvent, filtering while a solution is hot, removing the solvent from the solution under normal pressure or reduced pressure, collecting samples and drying at 30-50 DEG C to obtain the crystal forms, wherein the volume of the solvent is 20-120 times of mass of the corresponding bellidifolin; and the solvent is one of methanol, ethanol, acetone, 2-butanone, ethyl acetate, acetonitrile, isopropanol, tetrahydrofuran and water. The crystal forms I, II, III and VI of bellidifolin have the advantages of high purity and good stability, and have important significance for depth research and comprehensive utilization of the compound; and the preparation method is simple and has good repeatability.
Description
technical field [0001] The present invention belongs to the technical field of medicine, and more specifically relates to the crystal forms I, II, III and IV of bellidifolin or 1,5,8-trihydroxy-3-methoxykoushanone , and its preparation method, its pharmaceutical composition and its use in the manufacture of antiarrhythmic drugs. Background technique [0002] Daisy leaf gentianone (bellidifolin), the chemical name is 1,5,8-trihydroxy-3-methoxykoushanone, which is obtained from plants of the genus Gentiana, Pseudogentiana and Swertia An isolated mountain ketone compound. Most of the ketone compounds have central nervous system excitation or inhibition, diuresis, cardiotonic, inhibition of monoamine oxidase, anti-inflammatory and anti-viral effects. Current studies have shown that gentianone from daisy leaf has a wide range of biological activities, such as hypoglycemic, antibacterial, antioxidative, antiarrhythmic, promoting nerve function recovery, and has protective effect...
Claims
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