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A crystal form x of rebaudioside e, its preparation method and use

A crystal form and crystal technology, which is applied in the preparation of sugar derivatives, organic chemical methods, chemical instruments and methods, etc., can solve the problems of rare reports on the crystal structure and crystallization method of rebaudioside E, difficulty in obtaining crystals in large quantities, and low solubility and other problems, to achieve the effect of high crystallinity, easy operation and simple process

Active Publication Date: 2022-03-04
DONGTAI HIRYE BIOTECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the crystal structure and crystallization method of rebaudioside E are rarely reported.
[0006] Usually, when crystallization is carried out using the method of concentration after dissolution, it is difficult to obtain crystals in large quantities if the solubility of the target substance in the solvent is too low
For rebaudioside E, when the inventors prepared crystals from rebaudioside E powder with a purity of 95% obtained by spray drying, the inventors found that the solubility of rebaudioside E in water at 25°C was only 0.034% (ie 0.34mg / mL), the highest solubility at room temperature in aqueous ethanol is only about 0.38% (ie 3.8mg / mL), and the solubility in 95% aqueous ethanol at 65°C is less than 1% (ie 10mg / mL) (see attached Figure 5 , 6 ); Too low solubility makes it difficult to obtain a large amount of crystals of rebaudioside E by concentrating after dissolving

Method used

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  • A crystal form x of rebaudioside e, its preparation method and use
  • A crystal form x of rebaudioside e, its preparation method and use
  • A crystal form x of rebaudioside e, its preparation method and use

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Effect test

Embodiment 1

[0037] Dissolve 1 g of rubusoside with a purity of 95% in 100 mL of 90% aqueous ethanol and heat to 70°C. 65 g of rebaudioside E with a purity of 95% was slowly added to the above solution, and stirred at 70° C. to obtain a suspension solution. Then filter while hot to obtain supernatant and filter residue respectively. The supernatant was stirred at a speed of 20 rpm and cooled to 4°C at a speed of 2°C / min, and a white solid was precipitated. Collect the separated white solid by suction filtration, wash the crystal with 90% ethanol aqueous solution at 10°C, and then dry the crystal in vacuum at 30°C to obtain 30g of rebaudioside E crystal with crystal form X. The polarized light micrograph is as follows: Figure 4 as shown in a.

Embodiment 2

[0039] Dissolve 2 g of rubusoside with a purity of 95% in 100 mL of 90% aqueous methanol and heat to 58°C. 55 g of rebaudioside E with a purity of 90% was slowly added to the above solution, and a suspension solution was obtained after stirring. Then filter while hot to obtain supernatant and filter residue respectively. The supernatant was stirred at a speed of 50 rpm and cooled to 10° C. at a speed of 3° C. / min, and a white solid was precipitated. The precipitated white solid was collected by filtration, the crystal was washed with 90% methanol aqueous solution at 10°C, and then evaporated and dried at 50°C to obtain 35 g of rebaudioside E crystal with crystal form X.

Embodiment 3

[0045] 3 g of rubusoside with a purity of 75% was dissolved in 100 mL of 95% aqueous ethanol and heated to 70°C. 80 g of rebaudioside E with a purity of 80% was slowly added to the above solution, and a suspension solution was obtained after stirring. Then filter while hot to obtain supernatant and filter residue respectively. The supernatant was stirred at a speed of 40 rpm and cooled to 0° C. at a speed of 1° C. / min, and a white solid was precipitated. Collect the precipitated white solid by filtration, wash the white solid with 95% ethanol aqueous solution at 25°C, and then vacuum-dry the crystal at 30°C to obtain rebaudioside E crystal with crystal form X.

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Abstract

The invention discloses a crystal form X of rebaudioside E, a preparation method and application thereof, and belongs to the field of chemical pharmacy. The technology provided by the present invention can. The present invention utilizes low-carbon alcohol water as a solvent, utilizes rubus glycoside to solubilize, and crystallizes to obtain rebaudioside E crystals whose crystal form is X, and overcomes the low solubility of rebaudioside E in alcohol-water solvents, so that Difficulty in obtaining crystals in large quantities with high efficiency. Using technical means such as XRD, DSC, TGA and polarized light microscopy to characterize the rebaudioside E crystal with crystal form X, it was found that the rebaudioside E crystal with crystal form X had high crystallinity, stable Good sex and other advantages. The preparation method involved in the invention is simple, easy to operate, good in reproducibility, and can stably obtain target crystals in batches.

Description

technical field [0001] The invention relates to a crystal form X of rebaudioside E, a preparation method and application thereof, and belongs to the field of chemical pharmacy. Background technique [0002] As a high-power sweetener, steviol glycoside is not only widely used in beverages, soy sauce, various marine foods, kimchi, candy and baked goods, but also has medicinal activity. It has hypoglycemic, anti-tumor, anti-inflammatory and Dental caries, antihypertensive, anti-inflammatory and antioxidant activities. Stevioside is non-fermentable, does not affect the coagulation and viscosity of food, is not prone to mildew, does not cause Maillard reaction during processing, and cannot be used by microorganisms, thereby prolonging the shelf life of stevia products and making it easy to store and transport. [0003] Rebaudioside E is an isomer of rebaudioside A, which has similar polarity and is not easy to separate. Due to the low content of rebaudioside E in stevia rebaudi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/256C07H1/06A23L2/60
CPCC07H15/256C07H1/06A23L2/60A23V2002/00C07B2200/13A23V2200/16A23V2250/24
Inventor 夏咏梅王婉洁程双武沈洁胡学一樊晔刘湘
Owner DONGTAI HIRYE BIOTECH CO LTD
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