CN101037459A - Isolation and purification method of amygdalin from loquat core - Google Patents
Isolation and purification method of amygdalin from loquat core Download PDFInfo
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Abstract
The invention provides a method for separating the purified amygdalin from the loquat nucleus, comprising: extracting the amygdalin from the loquat nucleus to produce a concrete with a hydrophilic organic water solution; fully dissolving the concrete by ethanol, filtering, depressed dealcoholization of the filtrate, cryogenic crystallization to produce the coarse amygdalin; fully dissolving the amygdalin, filtering, cryogenic recrystallization, washing by ethanol-aether, getting a amygdalin white crystal with a purity not less than 98.7%. The invention purifies the amygdalin from the loquat nucleus which solves the problem that the amygdalin as an original medicine is hydrolyzed by acid and enzyme so as to reduce the curative effect and has a broad extension.
Description
Technical field
The present invention relates to a kind of green chemical industry preparation method who from the plant kernel, extracts active pharmaceutical ingredients, more specifically relate to a kind of from Radix Eriobotryae the method for separation and purification amygdaloside.
Background technology
Amygdaloside (Amygdalin, C
20H
27O
11) be the amygdalate effective constituent of traditional Chinese medicine, extensively be present in the kernel of multiple rosaceous plants such as apricot, peach, Lee, loquat, apple, hawthorn, especially content is more in Semen Armeniacae Amarum, is about 2～3%.
Effects such as amygdaloside has tangible cough-relieving, relievings asthma, analgesia, anti-inflammatory, antitumor, digestion promoting, the tradition tcm clinical practice often is used as medicine with the former medicine of Semen Armeniacae Amarum, but often owing to store and boil in the process, the effective component amygdaloside is easily by acid and enzyme institute catalytic hydrolysis, the Alpha-hydroxy benzyl cyanide aglycon that obtains is very unstable, easily decompose generation phenyl aldehyde and prussic acid, thereby reduced the curative effect of the former medicine of Semen Armeniacae Amarum.
The aromatic series cyanogen glycosides that amygdaloside is made up of phenyl aldehyde, prussic acid and glucose, easily become prunasin (prunasin) and almond cyanogen (mandelonitrile) by synaptase (amygdalase), prunase glucose glycoside enzymic hydrolysiss such as (prunase), latter's instability is met heat and is easily decomposed generation phenyl aldehyde and prussic acid.An amount of prussic acid can produce certain restraining effect to respiratory centre, make respiratory movement be tending towards quiet and reach cough-relieving, relieving asthma, analgesia, antiphlogistic effect.But a large amount of oral Semen Armeniacae Amarums or amygdaloside all easily produce intoxicating phenomenon, its mechanism of action mainly is that oral amygdaloside can be hydrolyzed into prussic acid and phenyl aldehyde by enteric microorganism in vivo, excessive hydrocyanic acid can react with the active centre ferric iron of Terminal oxidase in the cell mitochondrial, the activity of inhibitory enzyme, thus cause the histocyte respiration inhibition and cause death.
Amygdaloside dissolves in ethanol, methyl alcohol, acetone and the water isopolarity solvent, and during normal temperature, solubleness is about 8～10% in the water, is dissolved in fat-soluble organic solvents such as ether, normal hexane hardly.The solubleness of amygdaloside in cold ethanol is very little, and solubleness is very big in hot ethanol and boiling water.The trihydrate of high purity amygdaloside is the crystallization of rhombic prism shape, 200 ℃ of fusing points, about 220 ℃ of no hydrate fusing point.
Loquat is large special product fruit of China subtropical zone for Rosaceae loquat belongs to [Eriobotrya japonica (Thunb.) Lindl.] plant.China is topmost in the world loquat producing country, cultivated area and output account for the whole world 2/3, its main producing region is the Putian, Fujian, Zhe Jiangtang is dwelt and mountain, Dongting Lake, Jiangsu, 354 of existing loquat Cultivars, and main high-yield variety be red No. 3 and No. 4, city etc. too of No. 6, clock, liberation clock, length early.
The loquat of Fujian Province's Putian City is " three Daxing assumed name fruits ", is important " name, excellent, the spy " fruit in Fujian Province.160,000 mu of the existing planting loquat areas in the whole city, account for global planting loquat area 1/6,1/4 and the Fujian Province in the whole nation 1/2.The planting loquat area in Putian City Chang Tai town, Fujian Province reaches 70,000 mu, be chosen as " the famous-brand and high-quality base of subtropical crop " by the Ministry of Agriculture, and being awarded the title in " Chinese loquat first township ", the loquat of production is awarded " green food ", " Fujian Province's famous brand agricultural-food " and titles such as " country of origin marked products ".
The kernel part of loquat karyonide loquat, peaberry account for fresh fruit heavy 10%, wherein amygdaloside content is about 1.64%.As the seeds that " mountain area forestry comprehensive exploitation " project is given priority to, loquat is one of the fastest economic tree of development in recent years.At present, annual national loquat fresh fruit output has reached 16～200,000 tons, has number all to give up and do not add utilization with ten thousand tons Radix Eriobotryae, has not only polluted environment, has also wasted valuable resource.
Summary of the invention
The object of the present invention is to provide a kind of from Radix Eriobotryae the method for separation and purification amygdaloside, this preparation method directly adopts hydrophilic organic solvent separation and purification amygdaloside from Radix Eriobotryae, not only technology is simple, extraction efficiency is high, easy suitability for industrialized production, and amygdaloside purity height, the production cost of preparation are low.
Of the present invention a kind of from Radix Eriobotryae the method steps of separation and purification amygdaloside be:
(1) preparation of amygdaloside crude extract medicinal extract: with the Radix Eriobotryae is raw material, adopt 30～65% the hydrophilic organic solvent aqueous solution of 10～20 times of Radix Eriobotryae dry weights (W/W), extract 1～3 time under 50～80 ℃ of conditions, each 1～3 hour, united extraction liquid, filter, filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration;
(2) separation of amygdaloside crude product: in amygdaloside crude extract medicinal extract, add ethanol and make ethanol final concentration 〉=80% in the system, fully dissolve amygdaloside under 60～80 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product;
(3) amygdaloside crystalline purifying: under 50～75 ℃ of conditions, fully dissolve the amygdaloside crude product with dehydrated alcohol, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under the room temperature condition, remove impurity with dehydrated alcohol and anhydrous diethyl ether wash crystallization, get the amygdaloside white crystal.
Remarkable advantage of the present invention is:
One: the present invention adopts one or more mixed solvents in methyl alcohol, ethanol, acetone, propyl alcohol or the Virahol as hydrophilic organic solvent separation and purification amygdaloside from Radix Eriobotryae, advantage 1: the solubility property of hydrophilic organic solvents such as methyl alcohol, ethanol is good, penetrativity to the Radix Eriobotryae vegetable cell is strong, easier being penetrated in the Radix Eriobotryae internal organizational structure improved the dissolution rate and the extraction efficiency of amygdalin in eriobotrya japonia nut active pharmaceutical ingredients greatly; Advantage 2: adopt the hydrophilic organic solvents such as methyl alcohol, ethanol of heat to extract, can avoid that amygdaloside is become phenyl aldehyde and prussic acid by acid in the leaching process with enzymatic hydrolysis, thereby improved the extraction efficiency and the yield of medicinal ingredients amygdaloside greatly; Advantage 3: hydrophilic organic solvents such as the methyl alcohol of heat, ethanol are very big to the solubleness of amygdalin in eriobotrya japonia nut, and less to the solubleness of impurity such as protein, polysaccharide, are easy to obtain high purity amygdaloside product, obviously increase the competitiveness of product in market.
Two: the present invention preferentially selects for use methyl alcohol or acetone as the advantage of hydrophilic solvent to be: though the extraction effect of hydrophilic organic solvents such as methyl alcohol, ethanol, acetone, propyl alcohol or Virahol is suitable, but for other hydrophilic organic solvent, the boiling point of methyl alcohol or acetone is lower, energy consumption is littler during solvent recuperation, the rate of recovery is higher, can significantly reduce the preparation cost of product.
Three: made full use of the notable difference of impurity component solubleness in the hydrophilic organic solvent aqueous solution such as amygdalin in eriobotrya japonia nut activeconstituents and protein, polysaccharide, really reached the high efficiency separation of amygdalin in eriobotrya japonia nut active pharmaceutical ingredients and impurity component.
Four: made full use of the solubleness of amygdaloside in cold ethanol very little, in hot ethanol solubleness very big, be dissolved in the characteristics of fat-soluble organic solvents such as ether hardly, do not adopt column chromatography technology, and directly adopt hydrophilic organic solvent separation and purification amygdaloside from Radix Eriobotryae, not only raw material is cheap and easy to get, simple efficient, the amplification production easily of preparation technology, and amygdaloside purity height, the production cost of preparation are low.
Five: the separation and purification amygdaloside is used as medicine from Radix Eriobotryae, solved when using the former medicine of Semen Armeniacae Amarum to be used as medicine for a long time, the effective component amygdaloside is easily by acid and enzymic hydrolysis and the drawback that lessens the curative effect, " three height ", " three is little " and advantages such as " three just " with modern Chinese herbal medicine product, energy adapts to and satisfies modern Chinese medicine clinical application demand, meets the modernization of Chinese medicine and international industry policy that country advocates.
Embodiment
Implement separation and purification amygdaloside from Radix Eriobotryae according to the described method steps of content of the present invention.
Wherein, used hydrophilic organic solvent can be one or more mixed solvents in methyl alcohol, ethanol, acetone, propyl alcohol or the Virahol, preferentially selects methyl alcohol or acetone for use.
Amygdaloside white crystal purity 〉=98.7% of final separation and purification.
The physical and chemical parameter measuring method of each prepared product of the present invention is as follows:
The amygdaloside assay: adopting high performance liquid chromatography, is contrast with amygdaloside standard substance (available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute).Chromatographic condition: chromatographic column is selected Waters Nova-Pak C for use
18Post (Φ 3.9 * 15mm, 4 μ m), pre-column C
18(3.9mm * 15mm), UV-detector, moving phase are methyl alcohol: 0.01% phosphate aqueous solution (20: 80), and flow velocity 1.0mL/min, 34 ℃ of column temperatures detect wavelength 215nm, sample size 20 μ L.After measured, the used middle amygdaloside content of Putian product Radix Eriobotryae dry powder (water content 2.3%) of experiment is 16.8～22.3g/kg.
The amygdaloside fusing point test: take from system amygdaloside white crystal, drying, porphyrize, the kapillary of packing into adopt the YRT-3 melting point detector to measure its fusing point, are contrast with the amygdaloside standard substance.After measured, the melting range of self-control amygdaloside white crystal is 212.3～218.6 ℃.200 ℃ of the trihydrate fusing points of amygdaloside standard substance, 220 ℃ of no hydrate fusing points.
Preparation method's of the present invention embodiment is presented below:
Embodiment 1
Producing Radix Eriobotryae with the Putian, Fujian is raw material, with fresh Radix Eriobotryae washing, drying, pulverizing, mistake 10～30 mesh sieves, get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extractor, 48% methyl alcohol-acetone (1: 1) aqueous solution with 10 times of weight of Radix Eriobotryae powder (W/W), under 63 ℃ of conditions, extract 3 times, each 2 hours, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make that the ethanol final concentration is 81% in the system, fully dissolve amygdaloside under 80 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 50 ℃ of conditions, dehydrated alcohol with 12 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 10 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (1: 2) wash crystallization of 6 times of amounts (W/W) 1 time.After measured, amygdaloside white crystal purity is 99.4%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 62.6%.
Embodiment 2
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 30% methanol aqueous solution with 20 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 2 times, each 3 hours, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 88% in the system, fully dissolve amygdaloside under 75 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 68 ℃ of conditions, dehydrated alcohol with 5 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 25 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (7: 3) wash crystallization of 5 times of amounts (W/W) 1 time.After measured, amygdaloside white crystal purity is 98.8%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 61.3%.
Embodiment 3
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 65% methanol aqueous solution with 17 times of weight of Radix Eriobotryae powder (W/W), refluxing extraction is 1 hour under 80 ℃ of conditions, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add dehydrated alcohol, make ethanol final concentration 90% in the system, fully dissolve amygdaloside under 60 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 75 ℃ of conditions, dehydrated alcohol with 3 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 30 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (9: 1) wash crystallization of 3 times of amounts (W/W) 3 times.After measured, amygdaloside white crystal purity is 99.8%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 62.3%.
Embodiment 4
Producing Radix Eriobotryae with the Putian, Fujian is raw material, with fresh Radix Eriobotryae washing, drying, squeezing de-oiling, pulverizing, mistake 10～30 mesh sieves, get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extractor, with 65% aqueous ethanolic solution of 20 times of weight of Radix Eriobotryae powder (W/W), under 80 ℃ of conditions, extracted 1 hour, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 80% in the system, fully dissolve amygdaloside under 80 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 55 ℃ of conditions, dehydrated alcohol with 10 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 12 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (1: 4) wash crystallization of 5 times of amounts (W/W) 2 times.After measured, amygdaloside white crystal purity is 99.3%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 61.3%.
Embodiment 5
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 42% ethanol-Virahol (2: 1) aqueous solution with 15 times of weight of Radix Eriobotryae powder (W/W), under 78 ℃ of conditions, extract 2 times, each 2 hours, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 84% in the system, fully dissolve amygdaloside under 72 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 70 ℃ of conditions, dehydrated alcohol with 4 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 20 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (3: 1) wash crystallization of 3 times of amounts (W/W) 2 times.After measured, amygdaloside white crystal purity is 99.6%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 62.0%.
Embodiment 6
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 30% aqueous ethanolic solution with 10 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 88% in the system, fully dissolve amygdaloside under 60 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 75 ℃ of conditions, dehydrated alcohol with 4 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 25 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (4: 1) wash crystallization of 2 times of amounts (W/W) 3 times.After measured, amygdaloside white crystal purity is 98.7%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 60.9%.
Embodiment 7
Producing Radix Eriobotryae with the Putian, Fujian is raw material, with fresh Radix Eriobotryae washing, drying, 6# solvent deoiling, pulverizing, mistake 10～30 mesh sieves, get the Radix Eriobotryae powder, 3.0kg Radix Eriobotryae powder is put into extractor, 30% aqueous acetone solution with 14 times of weight of Radix Eriobotryae powder (W/W), under 50 ℃ of conditions, extract 3 times, each 3 hours, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 81% in the system, fully dissolve amygdaloside under 80 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 58 ℃ of conditions, dehydrated alcohol with 8 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 13 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (1: 3) wash crystallization of 2 times of amounts (W/W) 3 times.After measured, amygdaloside white crystal purity is 99.5%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 61.6%.
Embodiment 8
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 65% aqueous acetone solution with 10 times of weight of Radix Eriobotryae powder (W/W), refluxing extraction is 2 times under 80 ℃ of conditions, each 1 hour, united extraction liquid, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add 95% ethanol, make ethanol final concentration 86% in the system, fully dissolve amygdaloside under 78 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 65 ℃ of conditions, dehydrated alcohol with 5 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 24 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (3: 1) wash crystallization of 3 times of amounts (W/W) 2 times.After measured, amygdaloside white crystal purity is 99.2%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 61.9%.
Embodiment 9
10～30 order Radix Eriobotryae powder 2.5kg are put into extractor, 60% methyl alcohol-ethanol (2: 5) aqueous solution with 20 times of weight of Radix Eriobotryae powder (W/W), refluxing extraction is 2 hours under 75 ℃ of conditions, filter, filtrate through filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration.
In medicinal extract, add dehydrated alcohol, make ethanol final concentration 92% in the system, fully dissolve amygdaloside under 60 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product.
Under 75 ℃ of conditions, dehydrated alcohol with 4 times of amounts (W/W) fully dissolves the amygdaloside crude product, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under 18 ℃ of conditions, with dehydrated alcohol-anhydrous diethyl ether (1: 3) wash crystallization of 3 times of amounts (W/W) 2 times.After measured, amygdaloside white crystal purity is 99.8%, and the rate of recovery of amygdalin in eriobotrya japonia nut is 62.8%.
More than the part embodiment of the present invention of Chan Shuing is intended to describe in detail preparation method of the present invention, but is not limited thereto.
The present invention is the separation and purification amygdaloside from the waste Radix Eriobotryae of the large characteristic fruit loquat of China, not only raw material is cheap and easy to get, simple efficient, the amplification production easily of preparation technology, and when having solved the former medicine of clinical for a long time use Semen Armeniacae Amarum and being used as medicine, the difficult problem that the effective component amygdaloside is caused curative effect to descend by sour and enzymic hydrolysis easily has bigger dissemination.
Claims (4)
1. the method for a separation and purification amygdaloside from Radix Eriobotryae, it is characterized in that: method steps is:
(1) preparation of amygdaloside crude extract medicinal extract: with the Radix Eriobotryae is raw material, adopt 30～65% the hydrophilic organic solvent aqueous solution of 10～20 times of Radix Eriobotryae dry weights (W/W), extract 1～3 time under 50～80 ℃ of conditions, each 1～3 hour, united extraction liquid, filter, filtrate-0.06～-0.09MPa, 50～65 ℃ of conditions under, become amygdaloside crude extract medicinal extract through decompression and solvent recovery, vacuum concentration;
(2) separation of amygdaloside crude product: in amygdaloside crude extract medicinal extract, add ethanol and make ethanol final concentration 〉=80% in the system, fully dissolve amygdaloside under 60～80 ℃ of conditions, filter, filtrate-0.06～-0.09MPa, 50～75 ℃ of conditions under, through decompression recycling ethanol to begin to separate out amygdaloside, 4～10 ℃ of refrigeration, leave standstill growing the grain, filter beige amygdaloside crude product;
(3) amygdaloside crystalline purifying: under 50～75 ℃ of conditions, fully dissolve the amygdaloside crude product with dehydrated alcohol, filter, filtrate slowly cooling to begins to separate out amygdaloside, 4～10 ℃ of refrigeration, leaves standstill growing the grain, filtration, under the room temperature condition, remove impurity with dehydrated alcohol and anhydrous diethyl ether wash crystallization, get the amygdaloside white crystal.
2. according to claim 1 a kind of from Radix Eriobotryae the method for separation and purification amygdaloside, it is characterized in that: hydrophilic organic solvent is one or more mixed solvents in methyl alcohol, ethanol, acetone, propyl alcohol or the Virahol.
3. according to claim 2 a kind of from Radix Eriobotryae the method for separation and purification amygdaloside, it is characterized in that: described hydrophilic organic solvent is preferentially selected methyl alcohol or acetone for use.
4. according to claim 1 a kind of from Radix Eriobotryae the method for separation and purification amygdaloside, it is characterized in that: described amygdaloside white crystal purity 〉=98.7%.
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| CN104163837A (en) * | 2014-08-14 | 2014-11-26 | 合肥工业大学 | Method for extracting amygdalin from loquat cores by adopting supercritical CO2 extraction |
| CN106117279A (en) * | 2016-06-20 | 2016-11-16 | 福建师范大学 | Polyphenol and the continuous extraction method of amygdaloside in a kind of loquat nut |
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| CN107926989A (en) * | 2017-12-13 | 2018-04-20 | 潍坊科技学院 | For preventing the biological sterilization agent of leaf muld of tomato |
| CN108178776A (en) * | 2017-12-22 | 2018-06-19 | 江南大学 | A kind of preparation of amarogentin enriched products |
| CN109045048A (en) * | 2018-08-24 | 2018-12-21 | 浙江中医药大学附属第医院 | A kind of amarogentin is preparing the application in knee osteoarthritis anti-inflammatory drug |
| CN109260282A (en) * | 2018-03-19 | 2019-01-25 | 株式会社世普劳统 | Cosmeceutical, plant extracts and its preparation method and application |
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2007
- 2007-03-30 CN CNB2007100087607A patent/CN100475828C/en not_active Expired - Fee Related
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| CN104163837A (en) * | 2014-08-14 | 2014-11-26 | 合肥工业大学 | Method for extracting amygdalin from loquat cores by adopting supercritical CO2 extraction |
| CN106117279A (en) * | 2016-06-20 | 2016-11-16 | 福建师范大学 | Polyphenol and the continuous extraction method of amygdaloside in a kind of loquat nut |
| CN106117279B (en) * | 2016-06-20 | 2019-02-15 | 福建师范大学 | The continuous extraction method of polyphenol and amarogentin in a kind of loquat nut |
| CN107573391A (en) * | 2017-09-29 | 2018-01-12 | 武汉华士特工业生物技术开发有限公司 | A kind of method that loquat kernel oil and amarogentin are extracted from loquat nut |
| CN107926989A (en) * | 2017-12-13 | 2018-04-20 | 潍坊科技学院 | For preventing the biological sterilization agent of leaf muld of tomato |
| CN107926989B (en) * | 2017-12-13 | 2020-09-25 | 潍坊科技学院 | Biological sterilizing agent for preventing and treating tomato leaf mold |
| CN108178776A (en) * | 2017-12-22 | 2018-06-19 | 江南大学 | A kind of preparation of amarogentin enriched products |
| CN109260282A (en) * | 2018-03-19 | 2019-01-25 | 株式会社世普劳统 | Cosmeceutical, plant extracts and its preparation method and application |
| CN109045048A (en) * | 2018-08-24 | 2018-12-21 | 浙江中医药大学附属第医院 | A kind of amarogentin is preparing the application in knee osteoarthritis anti-inflammatory drug |
| CN109045048B (en) * | 2018-08-24 | 2021-08-24 | 浙江中医药大学附属第一医院 | Application of amygdalin in preparation of knee osteoarthritis anti-inflammatory drug |
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