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Method for separating and purifying rebaudioside C

A technology for separation and purification of glycosides, applied in the field of food additive production, which can solve problems such as short service life, high cost, and loss, and achieve the effects of simple process, convenient operation, and low cost

Active Publication Date: 2018-09-14
SEPAX TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, on the one hand, steviol glycosides are used as raw materials, and a certain amount of valuable RA must be lost during the preparation process; on the other hand, silica gel fillers are used, and the service life is short; After the industrial scale-up of the mixed reagent of methyl chloride and ethanol, the solvent recovery is difficult and the cost is high, and the whole method is not suitable for industrial scale-up production

Method used

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  • Method for separating and purifying rebaudioside C

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] (1) Take 1200g of mother liquor sugar in batch 1, its RC content is 10.0%, add appropriate amount of water to make it 200mg / mL, load the sample with a pump, and flow through a 30cm×50cm chromatographic column (built-in filler Stevia-AX-2) , was eluted with 60% methanol, and the RC component was collected by HPLC detection, concentrated by nanofiltration membrane, and dried to obtain 344 g of dried RC component; wherein the purity of RC was 32%.

[0057] (2) Take the dried RC component obtained in step (1), add 2752 mL of ethanol-acetone-water (10%:70%:20%), dissolve at 70°C, stir and crystallize for 12 hours, filter and dry to obtain primary crystals 136g; the purity of RC is 60%.

[0058] (3) Add 2800 mL of ethanol-methanol-water (10%: 40%: 50%) to the primary crystal obtained in step (2) for secondary recrystallization test, the dissolution temperature is 30°C, let stand for 36h, filter and dry , 78 g of secondary crystals were obtained; the RC purity was 95.7%.

Embodiment 2

[0060] (1) Take 700g of mother liquor sugar in batch 2, whose RC content is 25.1%, add appropriate amount of water to make it 10mg / mL, load the sample with a pump, and flow through a 30cm×50cm chromatographic column (built-in filler Stevia-AX-2) , eluted with 50% methanol, detected and collected RC components by HPLC, concentrated by nanofiltration membrane, and dried to obtain 326 g of dry matter of RC components; wherein the purity of RC was 50%.

[0061] (2) Take the dried RC component obtained in step (1), add 3260 mL of ethanol-acetone-water (30%: 40%: 30%), dissolve at 30°C, stir and crystallize for 36 hours, filter, and dry to obtain primary crystals 144g; the purity of RC is 80%.

[0062] (3) Take the primary crystal obtained in step (2) and add 1160 mL of ethanol-methanol-water (25%: 30%: 45%) for secondary recrystallization test, the dissolution temperature is 70°C, let stand for 12h, filter and dry , 108 g of secondary crystals were obtained; the RC purity was 97.5...

Embodiment 3

[0064] (1) Take 1300g of mother liquor sugar of batch 3, its RC content is 15.4%, add appropriate amount of water to make it 100mg / mL, load the sample with a pump, and flow through a 30cm×50cm chromatographic column (built-in filler Stevia-AX-2) , was eluted with 55% methanol, detected by HPLC to collect RC components, concentrated by nanofiltration membrane, and dried to obtain 442 g of dry matter of RC components; wherein the purity of RC was 41%.

[0065] (2) Take the dried RC component obtained in step (1), add 3575mL ethanol-acetone-water (20%: 60%: 20%), dissolve at 50°C, stir and crystallize for 24h, filter and dry to obtain primary crystals 185g; RC purity 72%.

[0066] (3) Add 1852 mL of ethanol-methanol-water (25%: 40%: 35%) to the primary crystal obtained in step (2) for secondary recrystallization test, the dissolution temperature is 60°C, let stand for 24h, filter and dry , 133.2 g of secondary crystals were obtained; the RC purity was 96.2%.

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Abstract

The invention provides a method for separating and purifying rebaudioside C. The method includes steps of a), mixing stevioside mother liquor sugar and water with each other, preparing mother liquor sugar solution, loading samples by the aid of pumps, allowing the samples to flow through chromatographic columns filled with fillers, carrying out elution by the aid of methanol aqueous solution, detecting and collecting rebaudioside C components by means of HPLC (high-performance liquid chromatography), concentrating the rebaudioside C components by the aid of nano-filtration membranes and dryingthe rebaudioside C components to obtain rebaudioside C component dried substances; b), dissolving the rebaudioside C component dried substances, which are obtained at the step a), by the aid of ethylalcohol-acetone-water, carrying out primary crystallization and further carrying out filtering and drying to obtain primarily crystallized crystals; c), dissolving the primarily crystallized crystals, which are obtained at the step b), by the aid of ethyl alcohol-methanol-water, carrying out secondary crystallization, and further carrying out still standing, filtering and drying to obtain rebaudioside C finished products. Silica gel is used as a matrix for the fillers, and octadecyl silane and divinyl benzene are bonded on the silica gel. The method has the advantages that the high-purity rebaudioside C can be prepared by the aid of the method, and the method is high in yield; rebaudioside A can be recycled, the fillers are long in service life, and solvents are easy to recycle.

Description

technical field [0001] The invention relates to the technical field of food additive production, and more specifically, relates to a method for separating and purifying rebaudioside C. Background technique [0002] Steviol glycoside is a kind of glycoside extracted from Stevia rebaudiana, and its sweet components mainly include rebaudioside A (hereinafter referred to as RA), stevioside (ST), rebaudioside C (hereinafter referred to as RC), lysoside Baudioside D (RD), rebaudioside M (RM), rebaudioside F (RF), dulcoside (DA), etc. As a new type of natural sweetener, steviol glycoside is 150-300 times sweeter than sucrose. It has high sweetness, low calorie, no metabolism in the human body, no residue, no side effects, safety and reliability. Its application scope is expanding day by day, and it has been hailed as a new type of sugar source plant internationally, and it is the best natural sweetener. [0003] As a steviol glycoside, RA has a high content, high sweetness (450 t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/256C07H1/08
CPCC07H1/08C07H15/256
Inventor 王艺黄学英
Owner SEPAX TECH
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