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A kind of Aconitin C crystal form and its preparation method and application
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A technology of scutellarin and crystal form, which is applied in the field of medicinal chemistry and achieves the effects of good thermal stability, stable properties and high purity
Active Publication Date: 2021-01-12
YUNNAN HAOPY PHARM LTD
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Embodiment 1
[0039] Embodiment 1, the preparation and identification of Aconitin C crystal form
[0040] Obtained by the gas-solid infiltration method, the specific preparation steps are: weigh 14.7 mg of aconitin and place it in a 3 ml vial, take another 20 ml vial and add 2 ml of DMF to it, place the 3 ml vial in a 20 ml vial After about 6 days, the solid was collected and subjected to XRPD, TGA / DSC and 1 HNMR test.
[0041] The XRPD results show that there are obvious characteristic absorption peaks at the diffraction angles (2θ angle) of 5.8±0.2, 6.3±0.2, 10.8±0.2, 11.8±0.2, 13.8±0.2, and 17.5±0.2. TGA / DSC results showed that when the sample was heated to 60°C, the weight loss was 8.5%; multiple endothermic signals appeared on the DSC curve. 1 HNMR results showed that 1.68 moles of DMF (16.02 wt%) were detected in the sample.
[0042] Identified as crystal form C, solvate.
[0043] Spectrum see respectively figure 1 The X-ray powder diffraction pattern of the C crystal form of aco...
Embodiment 2
[0044] Embodiment 2, the preparation of aconitin C crystal form
[0045]Obtained by the gas-solid infiltration method, the specific preparation steps are: weigh 14.7 mg of aconitin and place it in a 3 ml vial, take another 20 ml vial and add 2 ml of DMF to it, place the 3 ml vial in a 20 ml vial In the vial, leave it at room temperature after sealing, after 2 days, collect the solid and carry out XRPD test, the result is the same as figure 1 unanimous.
Embodiment 3
[0046] Embodiment 3, the preparation of aconitin C crystal form
[0047] Obtained by the gas-solid infiltration method, the specific preparation steps are: weigh 14.7 mg of aconitin and place it in a 3 ml vial, take another 20 ml vial and add 2 ml of DMF to it, place the 3 ml vial in a 20 ml vial In the vial, leave it at room temperature after sealing, after 20 days, collect the solid and carry out XRPD test, the result is consistent with figure 1 unanimous.
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Abstract
A bulleyaconitine A crystalline form C, and a preparation method therefor. An X-ray powder diffraction spectrum of the crystalline obtained by measurement using a Cu-Kα ray is as shown in fig. 1. The preparation method therefor comprises: using DMF as a solvent and obtaining by means of a gas-solid permeation method. The procedure of the preparation process is simple, and the obtained crystalline form is a solvate crystalline form, has high purity, and has good stability to light, humidity, and heat.
Description
technical field [0001] The invention relates to the field of medicinal chemistry, in particular to a C crystal form of aconitin and its preparation method and application. Background technique [0002] The chemical name of aconitin is (1α, 6α, 14α, 16β) tetrahydro-8,13,14-triol-20-ethyl-1,6,16-trimethoxy-4-methoxymethyl- 8-Acetoxy-14-(4'-p-methoxybenzyl)-aconitane. It is a diterpene diester alkaloid extracted and isolated from the root of Aconitum georgei Comber (Aconitum georgei Comber), a plant of the genus Ranunculaceae. It is named Crassicauline A. It was later renamed as Bulleaconitine A (T2), which belongs to known natural compounds in plant species, and its structural formula is as follows: [0003] [0004] At present, Aconitin preparations are widely used clinically for the treatment of rheumatoid arthritis (RA), osteoarthritis, myofibritis, neck and shoulder pain, low back pain, cancer pain and chronic pain caused by various causes. [0005] Drug polymorphism...
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