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A kind of refining purification method of plant source ceramide extract

A technology for the purification and purification of ceramides, which is applied in the separation/purification of carboxylic acid amides, plant raw materials, active ingredients of amides, etc. It can solve the problems of consuming a large amount of solvents, product loss, and low extraction efficiency, so as to improve product purity and separation efficiency. , Reduce the effect of product loss

Active Publication Date: 2020-11-06
SHENZHEN SANYE BIOLOGY TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] Therefore, in the face of the disadvantages brought by the ceramide purification method in which the prior art adopts extraction and one or more silica gel column chromatography (specifically, for example: the extraction efficiency is low due to the hydrophilic and lipophilic characteristics of ceramide and A large amount of loss is caused; and although two or more column chromatography purifications can improve the purity to more than 90%, in addition to more product losses caused by multiple chromatography, it also brings long purification time, consume a large amount of solvents and low separation efficiency, and are not suitable for industrialized production), it is necessary to provide a separation and purification method suitable for crude ceramide extracts of plant sources such as konjac, to overcome the defects of the prior art

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0089] Preparation of surface carboxyl-modified polymer magnetic microspheres A

[0090] 1) Preparation of Magnetic Polyvinyl Alcohol / Polyglycidyl Methacrylate Composite Microspheres

[0091] Heat and dissolve 40g polyvinyl alcohol in 400mL water, add 4g nano-ferroferric oxide magnetic particles and 5g polyglycidyl methacrylate under boiling water bath conditions, stir mechanically for 0.5h to mix well, add 600mL liquid paraffin when the temperature is lowered to 60°C and 200g Tween 80, stirred for 4h; then added 10mL of 2mol / L hydrochloric acid solution and 40mL of 30wt% glutaraldehyde solution, stirred and reacted for 30min, centrifuged to separate the microspheres, washed 2-3 times with absolute ethanol, and then The magnetic polyvinyl alcohol / polyglycidyl methacrylate composite base microspheres with a particle size range of 1-5 μm are obtained by vacuum drying.

[0092] 2) Surface carboxyl modification: ultrasonically disperse 50 g of the polyvinyl alcohol / polyglycidyl m...

preparation example 2

[0094] Preparation of surface amino-modified polymer magnetic microspheres B

[0095] 1) Weigh 10 g of mesoporous silica microspheres with a particle size of about 0.1 μm, ultrasonically disperse them in 310 g of deionized water, and stir to form a suspension evenly; weigh ferrous chloride and ferric chloride with a molar ratio of 1:2 Dissolve 25g of mixed raw materials in 50ml of deionized water, stir evenly, add it to the silica particle suspension, and then slowly add 1g of PVP dropwise under stirring; turn on the mechanical stirring, and heat it in a water bath at 75°C. Add 30g of concentrated ammonia water (30wt%) in batches, and continue stirring for 2 hours after the addition is complete; after the reaction is completed, cool to room temperature, centrifuge or magnetically separate the microspheres, wash the microspheres with deionized water, and dry them in vacuum to obtain surface-coated mesoporous carbon dioxide. Magnetic microspheres of silica.

[0096] 2) Disperse...

Embodiment 1

[0098] The method for refining and purifying konjac ceramide crude product comprises the following steps:

[0099] 1) Take 10g of crude konjac ceramide with a purity of about 75% (the raw material crude product in this example is obtained from konjac flour by supercritical carbon dioxide fluid extraction and molecular distillation, and extracted according to the extraction method of patent 201710999197.8) with 50% volume Dissolve the concentration of ethanol to 2wt%, add 18g of sodium chloride, adjust the pH to 5.5-6 with hydrochloric acid, stir for 0.5h, evaporate and concentrate to make it reach a saturated state. When the ceramide solution begins to precipitate solids, stop heating, cool down to room temperature, and stand at 1-3°C for 12 hours to cool down and crystallize to obtain a salt-forming solid; filter to obtain a solid, combine the filtrate with the next batch of raw materials, and recycle. After drying the filter cake, heat and stir it with 350ml of 60% ethanol s...

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Abstract

The present invention relates to a method for refining and purifying the crude product of plant source ceramide extract, adopting the refining and purifying process of salting out-primary polymer magnetic microsphere separation-secondary polymer magnetic microsphere separation-crystallization, which overcomes the existing The purification method can only obtain the defect of low-purity ceramide, and can provide high-purity ceramide with a purity of 99% or higher, so that it can be directly used in the fields of cosmetics and medicines. The purification method of the present invention adopts the means of combining secondary crystallization and specific magnetic polymer microsphere adsorption, can significantly improve product purity, effectively reduce product loss, and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of purification and separation of plant extracts, and in particular relates to a method for combined purification and purification of plant-derived crude ceramides. Background technique [0002] Ceramides are a kind of sphingosine substances formed by condensation of sphingosine and long-chain fatty acids through amide bonds. The molecular formula usually has amide groups, polyhydroxyl groups and long-chain alkyl chains of different lengths, so it has Hydrophilic and lipophilic amphiphilic properties. Ceramides have barrier, moisturizing, whitening, anti-aging, anti-tumor effects, and are widely used in the fields of medicine, food and cosmetics. Ceramides can be divided into two types: natural and chemically synthesized. Natural ceramides are usually derived from plant-based extractions, animal-derived extractions, and fermented bacteria. Cosmetics applications are mainly natural ceramide products. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C231/24C07C233/18C07C235/08A61K31/164A61P35/00A61P39/06A61K36/888A61K8/42A61K8/9794A61Q19/02A61Q19/08A61Q19/00
CPCA61K8/42A61K8/9794A61K31/164A61K36/888A61P35/00A61P39/06A61Q19/00A61Q19/02A61Q19/08C07C231/24C07C233/18C07C233/20C07C235/08
Inventor 池江南
Owner SHENZHEN SANYE BIOLOGY TECH
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