Glycyrrhetinic acid crystal type C, preparation method and use thereof in pharmaceutical compositions or health-care products
A technology of glycyrrhetic acid and health care products, which is applied in the directions of drug combination, food preparation, steroids, etc.
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[0040] According to the preparation method of glycyrrhetinic acid crystal type C according to the present invention, it is characterized in that the glycyrrhetinic acid raw material is completely dissolved at a temperature of 15°C to 80°C using a single solvent of methanol, and then heated at an ambient temperature of 4°C to 80°C. Glycyrrhetinic acid crystal type C is obtained through the recrystallization preparation process under the condition of ambient humidity of 10%-75% and normal pressure or vacuum pressure.
[0041] According to the preparation method of glycyrrhetinic acid crystal type C according to the present invention, it is characterized in that after mixing any two or more of methanol, n-hexane, cyclohexane, and water, the mixture is mixed at a temperature of 15°C to 80°C. Glycyrrhetinic acid raw materials are completely dissolved, and glycyrrhetinic acid crystal type C is obtained through a recrystallization preparation process under the conditions of ambient te...
Embodiment 1
[0049] The preparation method of glycyrrhetinic acid crystal type C sample 1 :
[0050] The preparation method of crystal type C sample of glycyrrhetinic acid is characterized in that 20 ml of methanol solvent is used to completely dissolve 500 mg of glycyrrhetinic acid raw material at 25 ° C, and the solvent is removed under vacuum conditions at a temperature of 40 ° C to prepare glycyrrhetinic acid Acid crystal type C solid sample, its powder X-ray diffraction pattern and figure 1 unanimous.
[0051] The preparation method of the crystal type C sample of glycyrrhetinic acid 2 :
[0052] The preparation method of crystal type C sample of glycyrrhetinic acid is characterized by using a mixed solvent of 20ml of methanol and 20ml of n-hexane to completely dissolve 500mg of glycyrrhetinic acid raw material at a temperature of 40°C, then standing at 25°C to precipitate a solid, and then vacuum Filter and dry, prepare and obtain glycyrrhetinic acid crystal type C solid sampl...
Embodiment 2
[0058] Glycyrrhetinic acid crystal form C absorption characteristics and blood concentration characteristics in rats :
[0059] SD rats with a body weight of 230 ± 5g were reared under conventional feeding conditions, free to drink water, and after fasting for 12 hours, the glycyrrhetinic acid crystal type C solid prepared in Example 1 was administered by intragastric administration at 200 mg / kg, before administration. And 0.083, 0.25, 0.5, 1, 1.5, 2, 3, 4, 6, 8, 12, 24 (h) after administration, about 0.4ml of blood was collected from the orbit, centrifuged at 4,000rpm for 15min to prepare plasma. Take 150 μl of plasma, add 200 μl of methanol, vortex for 1 min, centrifuge at 13400 rpm for 15 min, absorb the supernatant layer, filter through a 0.45 μm microporous membrane, take 20 μl for HPLC detection, Aligent XDB-C18 (150×4.6mm, 5 μm), flow The phase is methanol:0.4% acetic acid aqueous solution=90:10, flow rate: 1ml / min, detection wavelength: 254nm.
[0060] From the resu...
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