Rebaudioside D Crystallization with Selective Supersaturation

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Solution Overview

Problem

Existing methods for producing rebaudioside D-containing crystallized products face challenges in achieving high purity and yield ratios due to the higher content of rebaudioside A compared to rebaudioside D in stevia plant extracts, leading to entrainment of rebaudioside D in rebaudioside A crystallization.

Innovation Solution

A method involving the use of a roughly purified stevia plant extract with a total steviol glycoside content of 50 to 95% by mass, adjusting the solvent supersaturation levels for rebaudioside A and D, and controlled cooling to precipitate rebaudioside D, using methanol or ethanol as solvents, and optionally seed crystals to enhance crystallization.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If conventional crystallization methods are used to purify rebaudioside D, then rebaudioside A is preferentially crystallized due to its higher content, but rebaudioside D becomes entrained and cannot be effectively separated

Engineering Contradiction:
Improvepurity of rebaudioside DVSAvoidyield ratio of rebaudioside D
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention changes the crystallization parameters by controlling the degree of supersaturation of rebaudioside D to be 10 or more while keeping rebaudioside A at 18 or less, and by adjusting cooling rates and temperatures. This selective parameter control enables rebaudioside D to crystallize preferentially despite its lower concentration, resolving the contradiction between purity and yield

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention performs preliminary purification of the stevia extract to concentrate rebaudioside D and remove impurities before crystallization. This preliminary action creates optimal conditions for subsequent selective crystallization, enabling high purity and high yield of rebaudioside D by preparing the material in advance

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If multiple consecutive crystallization steps are performed to improve purity, then the purification effectiveness increases, but the production time and process complexity increase significantly

Engineering Contradiction:
Improvepurity of rebaudioside DVSAvoidproduction time
Core Design Contradiction:
Manufacturing precisionVSLoss of time

Solution Approach 1:

The invention performs comprehensive preliminary purification including extraction, concentration, and impurity removal before the crystallization step. This preliminary action ensures that a single crystallization step under controlled conditions achieves high purity, eliminating the need for multiple consecutive crystallization cycles and thereby reducing production time

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention optimizes crystallization parameters including supersaturation degree, cooling rate, and temperature to maximize purity in a single crystallization step. By carefully controlling these parameters, the process achieves high purification effectiveness without requiring multiple repeated steps, thus reducing overall production time

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method achieves a rebaudioside D-containing crystallized product with high purity and yield ratios, overcoming the limitations of conventional methods by directly crystallizing rebaudioside D from a roughly purified product.

Implementation Method 1

adjusting the solvent supersaturation levels for rebaudioside A and D

Methodology Applied
Scientific EffectSupersaturation: Supersaturation

Implementation Method 2

cooling the solution for crystallization with stirring, to precipitate rebaudioside D

Methodology Applied
Scientific EffectCrystallization: Crystallisation

Data Source

PatentEP4052771B1Method for manufacturing rebaudioside-d-containing crystallized product
Publication Date: 2025.10.22 SUNTORY HLDG LTD
  • EP4052771B1 patent drawingFigure 1
  • EP4052771B1 patent drawingFigure 2~3
  • EP4052771B1 patent drawingFigure 4~5

AI summary

There is demand for a novel method for manufacturing a RebD crystallized product. The present invention provides a method for manufacturing a RebD-containing crystallized product, including: a step for mixing a stevia plant-derived crude product having a total steviol glycoside content of 50-95 mass%, and containing at least RebA and RebD, into a solvent containing methanol or ethanol so that the supersaturation of RebD at 10°C is at least 10 and the supersaturation of RebA at 10°C does not exceed 18, and adjusting a crystallization solution; and a step for cooling the crystallization solution under stirring and causing RebD to precipitate.