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Daisy leaf gentianone single crystal and its preparation method and application

A technology of gentianone and daisy leaf, which is applied in the field of medicine, can solve the problems that there are no literature reports on the preparation method of the crystalline form of daisy leaf gentianone, and achieve the effects of easy industrial production, short production cycle and high yield

Active Publication Date: 2017-02-15
TIANJIN AGRICULTURE COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • Daisy leaf gentianone single crystal and its preparation method and application
  • Daisy leaf gentianone single crystal and its preparation method and application
  • Daisy leaf gentianone single crystal and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 1.0g of daisy leaf gentianone, add 50mL of acetone, heat to 40°C, stir to dissolve, filter while hot, and naturally cool the filtrate to room temperature, place it in a constant temperature incubator at 4°C, and cultivate for 16 days , precipitated solid, filtered to obtain yellow transparent crystals. Take 100 mg of the crystals and carry out the powder X-ray diffraction test.

[0035] Test instrument: Rigaku D / max-2500 powder X-ray diffractometer. Test conditions: CuKα radiation, graphite monochromator, tube pressure 40kV, tube flow 200mA, 2q scan range 3-80°, scan rate 8° / min, step size 0.02°, the powder X-ray diffraction experimental pattern of the crystal is shown in figure 1 (a).

Embodiment 2

[0037]Among the yellow transparent crystals of daisy leaf gentianone described in Example 1, a single crystal with a size of 0.20 mm×0.18 mm×0.12 mm was selected for single crystal X-ray diffraction test.

[0038] Test instrument: Rigaku MicroMax-007 single crystal diffractometer, MoKα radiation.

[0039] The crystal structure was resolved by the direct method (Shelxs 97) on a microcomputer, and the final reliability factor R 1 =0.0403, wR 2 =0.1034(w=1 / s|F|2), S = 1.023. Finalize the stoichiometric formula as C 14 h 10 o 6 , the calculated molecular weight is 274.22, and the calculated crystal density is 1.642g / cm 3 . figure 2 is the projection diagram of the three-dimensional structure of the molecule shown, image 3 Shown is the molecular unit cell packing diagram. Table 1 shows the atomic coordinate parameters and equivalent temperature factors, and Table 2 shows the bond length and bond angle of bonded atoms.

[0040] According to the single crystal structure da...

Embodiment 3

[0153] Weigh 1.0g of daisy leaf gentianone, add 20mL of tetrahydrofuran, heat to 60°C, stir to dissolve, filter while hot, and naturally cool the filtrate to room temperature, place it in a constant temperature incubator at 20°C, and cultivate for 10 days , Precipitated solid, filtered to obtain yellow transparent crystals, and observed under a microscope, a single crystal of gentianone from daisy leaf was formed. The single crystal X-ray diffraction characterization results are: it belongs to the triclinic crystal system, the space group is P-1, and the unit cell parameters: a=7.0459(14) Å, b=7.4871(15) Å, c=10.634(2) Å, α=86.64(3)°, β=79.73(3)°, γ=85.00(3)°, unit cell volume V=549.35(19)Å 3 , the number of molecules in the unit cell Z=2, the calculated crystal density is 1.658g / cm 3 , powder X-ray diffraction experiment pattern see figure 1 (a).

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Abstract

The invention relates to bellidifolin single crystal and a preparation method thereof. The bellidifolin single crystal is represented by a single crystal X-ray diffraction spectrum and belongs to a triclinic system, the space group of the bellidifolin single crystal is P-1, the unit cell parameters of the bellidifolin single crystal are as follows: a is equal to 7.0602(14)angstrom, b is equal to 7.5236(15)angstrom, c is equal to 10.662(2)angstrom, alpha is equal to 86.65(3)angstrom, beta is equal to 79.84(3)angstrom and gamma is equal to 84.96(3)angstrom, the unit cell volume V is equal to 554.77(19)angstrom, and the number Z of molecules in a unit cell is 2. The bellidifolin single crystal is yellow transparent crystal at normal temperature and is prepared by dissolving a crude bellidifolin product in an appropriate solvent system by using a recrystallization method, and by further volatilizing a solvent slowly. The bellidifolin single crystal which is prepared by using the preparation method provided by the invention is good in form and high in purity, and the preparation method is simple to operate and good in reproducibility, so that great significance is achieved for further development of the compound.

Description

technical field [0001] The invention belongs to the technical field of medicine, and relates to a single crystal of gentianone daisyleaf, a preparation method thereof, and the application of a pharmaceutical composition containing it in the manufacture of antiarrhythmic drugs. Background technique [0002] Daisy leaf gentianone (bellidifolin), chemically named 1,5,8-trihydroxy-3-methoxykoushanone, is isolated from Gentiana, Pseudogentiana, Swertia and other plants A mouth mountain ketone compound obtained. 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 effects on brain damage, etc., which has attracted widespread attention...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/86A61K31/352A61P9/06
CPCC07D311/86
Inventor 吕丽娟李旻辉韩华锐李振华黄治强赵雅婵
Owner TIANJIN AGRICULTURE COLLEGE
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