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Method for improving bulk density and fluidity of curcumin crystal

A technology of curcumin and bulk density, which is applied in the field of improving the bulk density and fluidity of curcumin, which can solve the problems of introducing new impurities, high requirements for curcumin bulk density, increasing costs, etc., and achieve good fluidity

Pending Publication Date: 2021-12-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN107805193A has announced a kind of production method of preparing low-solubility residual curcumin crystals, obtained the low-solubility residual curcumin crystals by adding reagents such as additives and refined preparations, and the required time is about 12h, but this technique uses a large amount of organic solvents and surfactants, which not only increase the cost, but also risk the introduction of new impurities
[0006] Curcumin can be used as a raw material and directly filled into capsules for dietary supplements or pharmaceutical preparations. During the filling or tableting process, the fluidity and bulk density of curcumin are highly required. The current production process of curcumin is the product The bulk density is about 0.4g / mL, and the angle of repose is above 40°, which seriously affects the application of curcumin in pharmaceutical preparations and other fields

Method used

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  • Method for improving bulk density and fluidity of curcumin crystal
  • Method for improving bulk density and fluidity of curcumin crystal
  • Method for improving bulk density and fluidity of curcumin crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Weigh 11g of curcumin crude powder raw material, dissolve it in 100g1,4-dioxane at 55°C with stirring, cool to 41°C at a cooling rate of 1°C / h, then heat up to 48°C, Crystallization for 2 hours; cooling and returning to temperature, and finally maintaining the temperature at 43°C, growing crystals for 2h; filtering, and then desolvating in a vacuum oven at 60°C for 12h, and performing characterization after the desolventization is complete.

[0047] figure 1Obtain the scanning electron micrograph (model is TM3000, Hitachi, Japan) of the 1,4-dioxane solvate of curcumin for embodiment 1, by figure 1 It can be seen that the crystal habit of the product is rod-shaped.

[0048] figure 2 Obtain the scanning electron micrograph (model is TM3000, Hitachi, Japan) of the curcumin product after the desolvation for embodiment 1, by figure 2 It can be seen that the crystal habit of the product is rod-shaped.

[0049] image 3 Be the scanning electron micrograph (model TM3000,...

Embodiment 2

[0055] Weigh curcumin crude product powder raw material 11g, be dissolved in 100g1,4-dioxane under the condition of 60 ℃ of band agitation, be cooled to 43 ℃ with the cooling rate of 2 ℃ / h, then be warming up to 48 ℃, raise Crystallization for 1 hour; cooling and returning to temperature, and finally maintaining the temperature at 46°C, growing the crystal for 1 hour; filtering, and then desolvating in a vacuum oven at 65°C for 12 hours, and performing characterization after the desolventization is complete.

[0056] Using the same detection method as in Example 1, it can be seen that the crystal habit of the obtained product is rod-shaped, and it is a stable 1 crystal form, with a bulk density of 0.7g / mL, an angle of repose of 35°, a purity of 99.7%, and a dissolved residue of 39ppm .

Embodiment 3

[0058] Weigh curcumin crude product powder raw material 10g, be dissolved in 50g1,4-dioxane under the condition of 60 ℃ of band stirring, be cooled to 52 ℃ with the cooling rate of 1.5 ℃ / h, then be warming up to 57 ℃, raise Crystallization for 1.5 hours; cooling and returning to temperature, and finally maintaining the temperature at 54°C, growing crystals for 1.5h; filtering, and then desolvating in a vacuum oven at 60°C for 12 hours, and then performing characterization after the desolventization is complete.

[0059] Using the same detection method as in Example 1, it can be seen that the crystal habit of the obtained product is rod-shaped, and it is a stable 1 crystal form, with a bulk density of 0.69g / mL, an angle of repose of 32°, a purity of 99.8%, and a dissolved residue of 27ppm .

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Abstract

The invention provides a method for improving bulk density and fluidity of curcumin crystal, and the method comprises the following steps: carrying out primary cooling on a 1,4-dioxane solution of curcumin until crystals are separated out, then carrying out heating, carrying out primary crystal growing, then carrying out secondary cooling, and carrying out secondary crystal growing to obtain the curcumin crystal. The curcumin product obtained by the method is rod-shaped in crystal habit and good in fluidity, the bulk density of the product reaches 0.5 g / mL or above, and the purity of the product reaches 99% or above.

Description

technical field [0001] The invention belongs to the technical field of medicine crystallization, and relates to a method for improving bulk density and fluidity of curcumin. Background technique [0002] Curcumin (Curcumin) was first extracted from turmeric rhizome in 1870 as a natural hydrophobic polyphenolic compound. It exists as keto-enol tautomers with the chemical names (E,E)-1,7-bis(4-hydroxy-3-methoxyphenyl)-1,6-heptadiene- 3,5-diketone and (E,E)-1,7-bis(4-hydroxy-3-methoxyphenyl)-1,6-heptadien-3-one-5-enol. [0003] Curcumin is an orange-yellow crystalline powder, which has been used as a natural pigment for food dyeing and food additives for a long time. With the deepening of research, curcumin was found not only as an acid-base indicator (pH 7.8 (yellow)-9.2 (red-brown)), but also has obvious inhibitory and preventive effects on diseases such as cancer, senile dementia and inflammation. . In addition, curcumin can also be used as antiseptic, beauty product, st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/255C07C45/81A23L33/105
CPCC07C45/81A23L33/105A23V2002/00C07C49/255A23V2250/2112
Inventor 龚俊波万旭兴曹越超吴送姑张韶男刘剑侯宝红
Owner TIANJIN UNIV