CN103768121B - A kind of method extracting sinapic acid choline ester. extract from Semen Raphani - Google Patents
A kind of method extracting sinapic acid choline ester. extract from Semen Raphani Download PDFInfo
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- CN103768121B CN103768121B CN201410049670.2A CN201410049670A CN103768121B CN 103768121 B CN103768121 B CN 103768121B CN 201410049670 A CN201410049670 A CN 201410049670A CN 103768121 B CN103768121 B CN 103768121B
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Abstract
The invention provides a kind of method extracting sinapic acid choline ester. extract from Semen Raphani, comprise the operation such as the extraction after the parch of Semen Raphani raw material, defat and defat, post separation; The inventive method safety is controlled, simple and practical, and the purity of the sinapic acid choline ester. extract using the inventive method to prepare is higher.
Description
Technical field
The present invention relates to a kind of method extracting sinapic acid choline ester. extract from Semen Raphani, belong to technical field of Chinese medicine.
Background technology
Chinese medicine is a complicated system, and in Herba indigoferae Pseudotinctoriae, different drug action composition coexists integrally.The process of preparing Chinese medicine can affect amount or the matter of its inherent composition.Through the systematic study to Chinese medicine raw product, on the basis of understanding processing excipient, utilize modern means of science and technology, carry out separation and purification to different active component, component, make the effective enrichment of active ingredient, resource is fully utilized.Can reduce at dosage, under quality controllable prerequisite, improve the scientific and technological content of Chinese medicine, realize the optimization of Chinese medicine decoction pieces effect, also can carry out the exploitation of new effect to the part of separation and purification, for original new drug development provides technical support.
Semen Raphani is traditional Chinese medical science common medicine, the fatty oil wherein containing 30%-40%, and enter decoct use by Chinese medicine tradition and only have fried less than 5%, all the other are then discarded with medicinal residues.Containing the erucic acid of more than 30% in Semen Raphani fatty oil.Erucic acid is edible unfavorable to human body for a long time, be one of restrictive standards of edible oil, but it is important industrial chemicals, has very high industrial utility value.Sinapic acid choline ester. content " Chinese Pharmacopoeia " version in 2010 in Semen Raphani must not specify lower than 0.4%.Research proves, sinapic acid choline ester. has the multiple pharmacological effect such as blood pressure lowering, blood fat reducing, radioprotective, antiinflammatory, diarrhea, anticancer, androgen antagonist.Above-mentioned effect and the traditional Chinese medical science use Semen Raphani to be used for the de-swelling that helps digestion, and lowering the adverse-rising QI to resolve phlegm does not have inevitable contact.From Semen Raphani, obtain the sinapic acid choline ester. extract that content is high, can be research and development is that the new drug of main pharmacodynamics composition provides technical support with sinapic acid choline ester..The problems such as synthetic cost is high, and side effect is obvious can be avoided simultaneously.From Semen Raphani, extract sinapic acid choline ester. extract, the pharmacological action of other compositions can be given prominence to better, and be conducive to high erucic acid fatty oil in Semen Raphani, sulfur methods of glycosides deep development and comprehensive utilization.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of method extracting sinapic acid choline ester. extract from Semen Raphani.
On the basis of specification Semen Raphani stir-frying-technology, obtained the Semen Raphani fatty oil part of raw material about 75% by physics defat, the polish that can be high erucic acid fatty oil is supplied raw materials, and Semen Raphani resource is fully utilized.
Extraction and purification process is optimized to the part after defat, obtains the sinapic acid choline ester. extract of content more than 20%, be enriched nearly 40 times compared with the sinapic acid choline ester. content in Semen Raphani raw material.Invention has also carried out certain research to the method for quality control of sinapic acid choline ester. extract and drug effect.
In Semen Raphani, the preparation technology of sinapic acid choline ester. extract is as follows:
1. the parch of Semen Raphani and defat
Get Semen Raphani, only make; During parch, be preheated to dispensing when cooking bottom temperature reaches 200-250 DEG C, Quick uniform stir-fries 1-1.5min, heaves, easily peels, when having cracker and peculiar fragrance, take out, dry in the air cool to quality; Be ground into 10 order powder, 90 DEG C are dried 1-2h, make powder temperature evenly reach 90 DEG C, grease press supplies room temperature control 95 DEG C ± 3 DEG C, be fed into pumping chamber, grease press adopts gradual pressurization, after fatty oil overflows, and dwell, until oil spill go out speed significantly slow down time, continue to be forced into oil spill again to go out, when so repeatedly reaching 75% ± 3% of fatty oil content in raw material to oil yield, stop force feed; The another device of fatty oil is preserved, and medicine cake extracts for further after pulverizing; Fatty oil can be used as the accurately machined raw material of high erucic acid fatty oil;
2. the preparation of defat Semen Raphani (parched) sinapic acid choline ester. extract
Semen Raphani (parched) medicine cake after physics defat is broken into coarse powder, soaks 0.5h, heating and refluxing extraction three times, and amount of water is followed successively by 8 times of spice, 6 times, 6 times, extraction time is respectively 1.0h, 0.5h, 0.5h, filters, merging filtrate, be evaporated to 1g/ml, add 95% ethanol, limit edged rapid stirring, make concentration of alcohol be 80%, leave standstill 24h, filter, filtrate reduced in volume, reclaims ethanol to without alcohol taste, and adjusting pH with ammonia is 8 as load solution;
HPD722 type macroporous resin, wet method dress post, gets the load solution of 2 times of column volume pH8 with 3BVh
-1flow velocity loading, absorption 4h, with 3BV distilled water with 4BVh
-1flow velocity eluting, merge eluent, another device is preserved.Use 50% ethanol of the pH4 of 5BV with 4BVh again
-1flow velocity eluting, collect ethanol elution, reclaim ethanol; In 75 DEG C, under-0.08-0.09Mpa condition, concentrating under reduced pressure obtains extractum, and extractum is again with 70 DEG C, and pressure-0.09Mpa, vacuum drying not higher than 5.0%, obtains Semen Raphani (parched) sinapic acid choline ester. extract to water content.
Beneficial effect of the present invention is as follows:
1, the Semen Raphani stir-frying-technology that optimizes of the present invention, under the prerequisite not affecting sinapic acid choline ester. content and extraction, the activity of sulfur glycosides catabolic enzyme in effective deactivation Semen Raphani can be ensured, improve the content of glucoraphenin and other thioglycoside in Semen Raphani (parched) Aqueous extracts to greatest extent, parch temperature improperly can be avoided again the destruction of the thioglycoside such as glucoraphenin in Semen Raphani.The content of the total sulfur glycosides composition based on glucoraphenin in Semen Raphani (parched) can be significantly improved.
2, the Semen Raphani (parched) physics degreasing process that optimizes of the present invention, does not use organic solvent.Effectively overcome organic solvent defat inflammable and explosive, there is the difficult problem that organic solvent is residual in product, be convenient to commercial production.Can ensure that again in skimming processes, glucoraphenin is not destroyed, and make sinapic acid choline ester. obtain effective enrichment.This technique had both effectively obtained Semen Raphani (parched) fatty oil position, for fine chemical industry provides high erucic acid fatty oil raw material, made Semen Raphani (parched) resource obtain comprehensive utilization, improve its added value.Again for sinapic acid choline ester. extract extraction and isolation in Semen Raphani (parched) decreases interference.
3, the defat Semen Raphani (parched) extraction and purification process that optimizes of the present invention, simple and practical, is convenient to promote.Extraction ratio and the rate of transform of sinapic acid choline ester. is ensure that by minimum solvent amount.
4, sinapic acid choline ester. extract separation preparation in the defat Semen Raphani (parched) extracting solution that optimizes of the present invention, from different resinous type, optimization macroporous adsorptive resins model, the key parameter such as kind and pH value, elution speed, effluent volume of the pH value of loading medicinal liquid, adsorption time, eluent, ensure that yield and the purity of sinapic acid choline ester. extract.Make in extract that sinapic acid choline ester. content is higher than 23%, comparatively Semen Raphani raw material improves nearly 60 times.Simple and practical, be convenient to promote.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
1. the parch of Semen Raphani and defat
Get Semen Raphani, only make.During parch, be preheated to dispensing when cooking bottom temperature reaches 200-250 DEG C, Quick uniform stir-fries 1-1.5min, heaves, easily peels, when having cracker and peculiar fragrance, take out, dry in the air cool to quality; Be ground into 10 order powder, 90 DEG C are dried 1-2h, make powder temperature evenly reach 90 DEG C, grease press supplies room temperature control 95 DEG C ± 3 DEG C, is fed into pumping chamber, after grease press adopts gradual pressurization that fatty oil is overflowed, dwell, until oil spill go out speed significantly slow down time, then continue to be forced into oil spill and go out, when so repeatedly reaching 75% ± 3% of fatty oil content in raw material to oil yield, stop force feed; The another device of fatty oil is preserved, and medicine cake extracts for further after pulverizing;
Sinapic acid choline ester. content before Semen Raphani defat: 0.80%; Glucoraphenin content after defat: 1.08%;
2. the preparation of defat Semen Raphani (parched) sinapic acid choline ester. extract
Semen Raphani (parched) medicine cake after physics defat is broken into coarse powder, soaks 0.5h, heating and refluxing extraction three times, and amount of water is followed successively by 8 times of spice, 6 times, 6 times, extraction time is respectively 1.0h, 0.5h, 0.5h, filter, merging filtrate, is evaporated to 1g/ml, adds 95% ethanol, limit edged rapid stirring, makes concentration of alcohol be 80%, leaves standstill 24h, filter, filtrate reduced in volume reclaims ethanol to without alcohol taste, and adjusting pH with ammonia is 8 as load solution.
HPD722 type macroporous resin, wet method dress post, gets the medicinal liquid of 2 times of column volume pH8 with 3BVh
-1flow velocity loading, absorption 4h, with 3BV distilled water with 4BVh
-1flow velocity eluting, merge eluent, another device is preserved; Use 50% ethanol of the pH4 of 5BV with 4BVh again
-1flow velocity eluting, collect ethanol elution, reclaim ethanol; In 75 DEG C, under-0.08-0.09Mpa condition, concentrating under reduced pressure obtains extractum, and extractum is again with 70 DEG C, and pressure-0.09Mpa, vacuum drying not higher than 5.0%, obtains Semen Raphani (parched) sinapic acid choline ester. extract position to water content.
Sinapic acid choline ester. content in sinapic acid choline ester. extract: 23.07%.
in described Semen Raphani test sample, the assay method of sinapic acid choline ester. is as follows:
According to " Chinese Pharmacopoeia " version annex VI D high effective liquid chromatography for measuring in 2010.
chromatographic condition and system suitabilitytake octadecylsilane chemically bonded silica as filler; With acetonitrile-0.1% acetum (15:85) for mobile phase; Determined wavelength is 326nm.Number of theoretical plate calculates should be not less than 5000 by sinapic acid choline ester. peak.
the preparation of reference substance solutionget Sinapine Thiocyanate reference substance appropriate, accurately weighed, put in brown measuring bottle, add pure water and make the solution of every 1ml containing 40 μ g, to obtain final product.
the preparation of need testing solutionget sinapic acid choline ester. extract powder 0.05g, accurately weighed, distilled water dissolves, ultrasonic 20min, and adding distil water is settled to 100ml, gets and crosses 0.45 μm of microporous filter membrane in right amount.
algoscopyaccurate absorption reference substance solution and each 20 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
Note: have sinapic acid choline ester. to contain survey method in " pharmacopeia ", but use phenyl silane base key to close silicagel column, expensive, this method uses common C18 post, convenient and practical.
Claims (2)
1. from Semen Raphani, extract a method for sinapic acid choline ester. extract, it is characterized in that, comprise the following steps:
1) parch of Semen Raphani and defat
Get Semen Raphani, only make; During parch, be preheated to dispensing when cooking bottom temperature reaches 200-250 DEG C, Quick uniform stir-fries 1-1.5min, heaves, easily peels, when having cracker and fragrance, take out, dry in the air cool to quality; Be ground into 10 order powder, 90 DEG C are dried 1-2h, make powder temperature evenly reach 90 DEG C, grease press supplies room temperature control 95 DEG C ± 3 DEG C, be fed into pumping chamber, grease press adopts gradual pressurization, after fatty oil overflows, and dwell, until oil spill go out speed significantly slow down time, continue to be forced into oil spill again to go out, when so repeatedly reaching 75% ± 3% of fatty oil content in raw material to oil yield, stop force feed; The another device of fatty oil is preserved, and medicine cake extracts for further after pulverizing;
2) preparation of defat Semen Raphani (parched) sinapic acid choline ester. extract
Semen Raphani (parched) medicine cake after physics defat is broken into coarse powder, soaks 0.5h, heating and refluxing extraction three times, and amount of water is followed successively by 8 times of spice, 6 times, 6 times, extraction time is respectively 1.0h, 0.5h, 0.5h, filters, merging filtrate, be evaporated to 1g/ml, add 95% ethanol, limit edged rapid stirring, make concentration of alcohol be 80%, leave standstill 24h, filter, filtrate reduced in volume, reclaims ethanol to without alcohol taste, and adjusting pH with ammonia is 8 as load solution;
HPD722 type macroporous resin, wet method dress post, gets the load solution of 2 times of column volume pH8 with 3BVh
-1flow velocity loading, absorption 4h, with 3BV distilled water with 4BVh
-1flow velocity eluting, merge eluent, another device is preserved; Use 50% ethanol of the pH4 of 5BV with 4BVh again
-1flow velocity eluting, collect ethanol elution, reclaim ethanol; In 75 DEG C, under-0.08-0.09Mpa condition, concentrating under reduced pressure obtains extractum, and extractum is again with 70 DEG C, and pressure-0.09Mpa, vacuum drying not higher than 5.0%, obtains Semen Raphani (parched) sinapic acid choline ester. extract to water content.
2. method according to claim 1, is characterized in that, in described Semen Raphani (parched) sinapic acid choline ester. extract, the content of sinapic acid choline ester. is greater than 23%.
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| CN102068424A (en) * | 2011-01-14 | 2011-05-25 | 哈尔滨工业大学 | Brain atrophy treating medicament prepared from active ingredient of radish seed |
| CN103316088A (en) * | 2013-07-04 | 2013-09-25 | 石强 | Natural pharmaceutical composition |
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| CN102068424A (en) * | 2011-01-14 | 2011-05-25 | 哈尔滨工业大学 | Brain atrophy treating medicament prepared from active ingredient of radish seed |
| CN103316088A (en) * | 2013-07-04 | 2013-09-25 | 石强 | Natural pharmaceutical composition |
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