Method for preparing myricetin/HP-beta-CD inclusion compound superfine granules through supercritical CO2 anti-solvent technique
An ultra-fine particle, anti-solvent technology, used in anti-toxic agents, anti-inflammatory agents, drug combinations, etc., to achieve green and efficient processes, reduce raw material losses, and overcome the effects of organic solvent residues
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[0040] Example 1: Single factor method to investigate the influence of various factors on the drug loading and recovery rate of myricetin / HP-β-CD inclusion compound ultrafine particles
[0041] Single factor experiment: CO 2 Effect of flow rate on the recovery rate and morphology of superfine particles of myricetin / HP-β-CD inclusion complex
[0042] Under the conditions of crystallization pressure 11MPa, crystallization temperature 40℃, myricetin mass concentration 6.0g / L, molar ratio of myricetin API to HP-β-CD 1:1, and solution volume flow rate of 1.0mL / min, the CO 2 When the flow rate is 2.0-2.5, 2.5-3.0, 3.0-3.5, 3.5-4.0, 4.0-4.5L / min, the influence on the morphology and recovery rate of myricetin inclusion compound. When the flow rate is less than or equal to 2.5L / min, the product is similar to the rotary evaporation product under the same conditions, showing a yellow transparent viscous solid attached to the bottom of the crystallization kettle; when the flow rate is 2.5-3.0 a...
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[0051] Example 2: Preparation of Myricetin / HP-β-CD Inclusion Compound Ultrafine Particles by Supercritical Antisolvent Method
[0052] The method for preparing superfine particles of myricetin / HP-β-CD inclusion compound by supercritical antisolvent method includes the following steps:
[0053] Step S1, dissolving myricetin crude drug and water-soluble carrier in an organic solvent to obtain a myricetin-carrier mixed solution;
[0054] Step S2, the CO 2 Pass into the crystallization kettle to adjust the temperature and pressure in the crystallization kettle;
[0055] Step S3, continue to access CO 2 , Maintaining the temperature and pressure in the crystallization kettle unchanged, while passing the myricetin-carrier mixed solution prepared in step S1 into the crystallization kettle;
[0056] Step S4, after the mixed solution has been introduced, continue to introduce CO 2 40min, release the pressure after exhausting the residual solvent; when the pressure in the crystallization kettle d...
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[0066] Example 3: In vitro dissolution test
[0067] A certain amount of myricetin crude drug, myricetin / HP-β-CD solid mixture and the myricetin / HP-β-CD inclusion compound ultrafine particles under a better process were measured and determined to be in 0.1% Tween 80 The dissolution rate of the solution clock, compare its dissolution performance, the result is as Picture 9 As shown, the analysis shows that the dissolution rate of myricetin / HP-β-CD inclusion compound ultrafine particles can reach 85.69% in 5 minutes and over 99% in 60 minutes, which proves that the dissolution of the drug has been significantly improved.
[0068] The in vitro dissolution results show that compared with the crude drug and solid mixture, the dissolution performance of myricetin / HP-β-CD inclusion compound ultrafine particles has been significantly improved. Specifically, myricetin / HP-β-CD inclusion compound The cumulative dissolution rate of ultrafine particles in 60 minutes can reach more than 99%, w...
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