Icariin H2 crystal form, preparation method of icariin H2 crystal form, medicine composition and application
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A technology of icariin and its composition, applied in the field of medicinal chemistry, can solve the problems of poor water solubility of icariin, poor oral absorption, and limitation of clinical application, and achieve good reproducibility, favorable absorption and utilization, and oral absorption high rate effect
Inactive Publication Date: 2015-07-29
ZHUCHENG HAOTIAN PHARMA
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Problems solved by technology
However, due to the poor water solubility of icariin and poor oral absorption, its clinical application is greatly limited.
At present, there is no report on the polymorphic form of icariin
Method used
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Embodiment 1
[0035] Take 30 mg of icariin in a bottle, add 5 mL of ethanol / water (volume ratio 1:1), dissolve it by ultrasonication, and dissolve it at 50°C for 1 hour, then filter it while it is hot to prevent it from becoming supersaturated, and then put it in Volatilize at 50°C, and the obtained solid is the crystal form of icariin H2.
Embodiment 2
[0037] Take 30mg of icariin in a bottle, add methanol / water (volume ratio 2:3) 3mL, place on a magnetic stirrer, suspend at room temperature for 3 days, discard the supernatant after centrifugation, and centrifuge The solid was evaporated to dryness to obtain icariin H2 crystal form.
Embodiment 3
[0039] Take 30 mg of icariin in a bottle, add 5 mL of dioxane / water (volume ratio 2:1) mixed solvent, ultrasonically dissolve it, and dissolve it at 50°C for 1 hour, then filter while it is hot to avoid excessive Saturated state, then volatilize at 50°C, the obtained solid is icariin H2 crystal form.
[0040] A kind of icariin H2 crystal form provided by the present invention, through X-ray powder diffraction (XRPD), thermogravimetric analysis (TG), differential scanning calorimetry (DSC), dynamic water adsorption (DVS), infrared ( IR) and Raman (Raman) and other solid-state methods for characterization.
[0041] Carry out X-ray powder diffraction analysis to the icariin H2 crystal form solid sample that embodiment 1 makes, it adopts the diffractometer of Bruker D8 advance type of German Bruker Instrument Co., Ltd., adopts Cu-Kα ray The voltage is 40 kV, the current is 40 mA, the scanning speed is 12 degrees per minute, the step size is 0.02 degrees, and each step takes 0.1 ...
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Abstract
The invention belongs to the technical field of medicine chemistry, and particularly relates to an icariin H2 crystal form, a preparation method of the icariin H2 crystal form, a medicine composition and an application. The crystal form is represented by virtue of an X-ray powder diffraction pattern. The preparation method comprises the following steps: dissolving icariin by utilizing mixed solvent, drying the icariin at the temperature of 50 DEG C, or suspending the icariin at the room temperature after the icariin is dissolved, drying the centrifuged solid. The medicine composition comprises the icariin H2 crystal form and a carrier acceptable on the medicine; the icariin H2 crystal form is applied in the medicine for preventing diseases of immune system, tumor tissue diseases, diseases of reproductive system, diseases of endocrine system, bone diseases, diseases of cardiovascular system and diseases of nerve and metal system. The preparation method of the icariin H2 crystal form is simple to operate, easy to control, high in crystal degree, good in repetition and good in stability.
Description
technical field [0001] The invention belongs to the technical field of medicinal chemistry, and in particular relates to a crystal form of icariin H2, a preparation method thereof, a pharmaceutical composition and application thereof. 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. In the field of pharmaceutical research, polymorphism includes multi-component crystal forms such as organic solvates and hydrates. [0003] Drug polymorphism widely exists in the drug development process and is an inherent characteristic of small organic molecules. Theoretically, small-molecule drugs can have an infinite number of crystal packing methods - polymorphic forms. Studies have shown that the number of drug polymorphic forms discovered is proportional to the time and resources invested in research. For example, Lipitor, the drug wit...
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