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CN-121974961-A - Preparation technology for improving mobility of rebaudioside M crystals

CN121974961ACN 121974961 ACN121974961 ACN 121974961ACN-121974961-A

Abstract

The invention relates to the technical field of rebaudioside M crystals, in particular to a preparation process for improving the fluidity of rebaudioside M crystals, which comprises the following steps of (1) taking a rebaudioside M raw material, adding a first solvent, heating and stirring to obtain a phase I solution for standby, (2) taking a second solvent with the density larger than that of the phase I solution as a phase II solution, taking a third solvent with the density smaller than that of the phase II solution as a phase III solution, (3) adding the phase III solution in the step (2) into the phase II solution, then adding the phase I solution in the step (1) after controlling the temperature, standing at constant temperature in a closed state until white flaky crystals appear in the interior of the phase I solution and at the interface of the phase I solution and the phase II and phase III mixed solution, and separating, leaching and drying to obtain the rebaudioside M crystals. By adopting the preparation process, the rebaudioside M crystal with high fluidity and high dissolution rate can be obtained.

Inventors

  • ZHU LIPING
  • DU GUOYING
  • ZANG PENGFEI
  • HE DONGSHENG

Assignees

  • 东台市浩瑞生物科技有限公司

Dates

Publication Date
20260505
Application Date
20251231

Claims (8)

  1. 1. A preparation process for improving the fluidity of rebaudioside M crystals, which is characterized by comprising the following steps: (1) Taking a rebaudioside M raw material, adding a first solvent, heating and stirring to obtain a phase I solution for later use; (2) Taking a second solvent with density higher than that of the phase I solution as a phase II solution, and taking a third solvent with density lower than that of the phase II solution as a phase III solution; (3) Adding the phase III solution in the step (2) into the phase II solution, adding the phase I solution in the step (1) after controlling the temperature, standing at constant temperature under a closed state until white flaky crystals appear in the interior of the phase I solution and at the interface of the phase I solution and the mixed solution of the phase II and the phase III, separating, leaching and drying to obtain the rebaudioside M crystals.
  2. 2. The preparation process for improving the fluidity of rebaudioside M crystals according to claim 1, wherein the first solvent in step (1) is 60-80% by volume of aqueous methanol solution or 50-70% by volume of aqueous ethanol solution, and the rebaudioside M raw material and the first solvent are added according to a ratio of 1:5-15 of feed liquid.
  3. 3. The process for preparing a rebaudioside M crystal with improved flowability according to claim 1, wherein the heating in step (1) is to 50-75 ℃.
  4. 4. The preparation process for improving the fluidity of rebaudioside M crystals according to claim 1, wherein the second solvent in the step (2) is one or more of dichloromethane, 1, 2-dichloroethane and chloroform, and the third solvent is one or more of ethyl acetate, methyl tert-butyl ether and isopropyl acetate.
  5. 5. The process for preparing a rebaudioside M crystal according to claim 1, wherein the phase II solution and the phase III solution in the step (3) are added in a volume ratio of 1-2:1.
  6. 6. The preparation process for improving the fluidity of rebaudioside M crystals according to claim 1, wherein the phase I solution and the phase III solution in the step (3) are added in a volume ratio of 1:2-3, and the phase I solution is added under the condition that the temperature is controlled to be 40-65 ℃.
  7. 7. The process for preparing the rebaudioside M crystal with improved fluidity according to claim 1, wherein the standing treatment is carried out for 5-15 days at a constant temperature of 10-25 ℃ in the step (3).
  8. 8. The process for preparing a rebaudioside M crystal according to claim 1, wherein the crystal is washed with n-hexane or petroleum ether in step (3).

Description

Preparation technology for improving mobility of rebaudioside M crystals Technical Field The invention relates to the technical field of rebaudioside M crystals, in particular to a preparation process for improving the fluidity of rebaudioside M crystals. Background Rebaudioside M (rebaudioside M) is one of the most organoleptic components of steviol glycosides. However, the high-purity rebaudioside M has two intrinsic physical defects that firstly, the most stable thermodynamic crystal form is extremely slow in dissolution dynamics and low in apparent solubility, and secondly, a spray drying process which is commonly adopted for obtaining a solid form leads to a hollow, fluffy amorphous or microcrystalline product, and the product has extremely low bulk density, extremely poor fluidity and apparent hydrophobicity and cannot meet the accurate and automatic dry-method batching requirements of the modern food industry. The prior art improves the above properties mainly by physical mixing (addition of flow aids), pelletization or eutectic/salt formation. All the methods introduce inactive components, change the chemical composition of the product, have limitations in the trend of cleaning labels, and fail to radically change the crystalline properties of rebaudioside M itself. Therefore, in view of the above problems, it is necessary to develop a preparation process for improving the fluidity of rebaudioside M crystals. Disclosure of Invention Aiming at the defects of the prior art, the invention provides a preparation process for improving the fluidity of the rebaudioside M crystal, and the preparation process can be used for obtaining the rebaudioside M crystal product with low repose angle and high dissolution rate. In order to solve the technical problems, the technical scheme of the invention is as follows: A preparation process for improving the flowability of rebaudioside M crystals, the preparation process comprising the steps of: (1) Taking a rebaudioside M raw material, adding a first solvent, heating and stirring to obtain a phase I solution for later use; (2) Taking a second solvent with density higher than that of the phase I solution as a phase II solution, and taking a third solvent with density lower than that of the phase II solution as a phase III solution; (3) Adding the phase III solution in the step (2) into the phase II solution, adding the phase I solution in the step (1) after controlling the temperature, standing at constant temperature under a closed state until white flaky crystals appear in the interior of the phase I solution and at the interface of the phase I solution and the mixed solution of the phase II and the phase III, separating, leaching and drying to obtain the rebaudioside M crystals. As an improved technical scheme, in the step (1), the first solvent is 60-80% by volume of methanol aqueous solution or 50-70% by volume of ethanol aqueous solution, and the rebaudioside M raw material and the first solvent are added according to the ratio of 1:5-15 of feed liquid. As an improved technical scheme, the step (1) is heated to 50-75 ℃. As an improved technical scheme, the second solvent in the step (2) is one or more of dichloromethane, 1, 2-dichloroethane and chloroform, and the third solvent is one or more of ethyl acetate, methyl tertiary butyl ether and isopropyl acetate. As a modified embodiment, the phase II solution and the phase III solution in step (3) are added in a volume ratio of 1-2:1. As an improved technical scheme, the phase I solution and the phase III solution in the step (3) are added according to the volume ratio of 1:2-3, and the phase I solution is added under the condition that the temperature is controlled to be 40-65 ℃. As an improved technical scheme, the method is characterized in that in the step (3), standing treatment is carried out for 5-15 days at the constant temperature of 10-25 ℃. As an improved technical scheme, the crystal is washed by adopting normal hexane or petroleum ether in the step (3). After the technical scheme is adopted, the invention has the beneficial effects that: The invention abandons the traditional cooling crystallization or rapid mixing precipitation method, controls the supersaturation degree by diffusion, and is characterized in that a dynamic environment generated by controlling the supersaturation degree by solvent interface diffusion is created. The direct mixing rate of good solvent (phase I) with heavy antisolvent (phase II) is greatly retarded by the presence of a well-designed three-phase density gradient system, particularly the intermediate buffer phase (phase III). The method ensures that the reduction process of the solubility of the rebaudioside M is extremely slow and uniform, effectively inhibits explosive nucleation, provides thermodynamic and kinetic conditions for anisotropic, ordered and compact growth of crystals, and is the root cause for obtaining regular crystal habit and high-density crystals. By