CN102219721A - Extraction method for concentrate containing beta-cryptoxanthin, concentrate obtained by the method, and usage of the obtained concentrate - Google Patents
Extraction method for concentrate containing beta-cryptoxanthin, concentrate obtained by the method, and usage of the obtained concentrate Download PDFInfo
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Abstract
The invention relates to a method for extracting concentrate containing beta-cryptoxanthin from persistent calyx of Physalis alkekengi L. var. franchetii (Masters)Makino, the concentrate containing beta-cryptoxanthin obtained by the method, and the usage of the concentrate. The method comprises the steps of pretreatment, enzyme treatment, extraction, saponification, condensation and purification of raw materials. According to the method provided in the invention, the technical defect in the prior art that extraction efficiency of beta-cryptoxanthin is low is overcome; a beta-cryptoxanthin product with great value is obtained; and the content of beta-cryptoxanthin in the product provided in the invention is far more than the content of beta-cryptoxanthin in the product obtained in the prior art, thereby enabling a good prospect for the application of beta-cryptoxanthin products. The raw materials used in the method are easily available, the extraction process is simple, the content of beta-cryptoxanthin in the obtained product is high, and comprehensive cost for the extraction is controllable; therefore, the method is suitable for industrial production and can be used for lengthening manufacturing chain.
Description
[technical field]
The invention belongs to from the technical field of extracted form natural plant effective constituent.More specifically, the present invention relates to a kind ofly extract the method for the enriched material contain beta-cryptoxanthin, also relate to the enriched material that contains beta-cryptoxanthin that adopts aforesaid method to obtain, also relate to the purposes of the described enriched material that contains beta-cryptoxanthin from Calyx Physalis.
[background technology]
Wintercherry (Physalis alkekengi L.var.franchetii (Masters) Makino) is a kind of per nnial herb of Solanaceae (Solanaceae) Physalis (Physalis), has another name called " red Miss ", " foreign Miss ", " red lantern ", " Franchet Groundcherry Calyx and Fruit " etc.The wintercherry fruit is spherical berry, and outside place calyx is roomy, is the bird-caging cryptomere, in the most of area of China distribution is arranged all.The root of wintercherry and herb all can be used as medicine, have heat-clearing, detoxifcation, diuresis, step-down, cardiac stimulant, antibacterial, function such as make eye bright.Cure mainly that heat is coughed, pharyngalgia, hoarsen, the acute flat diseases such as body inflammation, dysuria and oedema of choosing.Contain abundant beta-cryptoxanthin in the calyx of wintercherry fruit place, mainly the form with fatty acid ester exists; Its fatty acid ester is following formula chemical structure (R=is fatty acid-based):
(β-Cryptoxanthin) is a kind of carotenoid (Carotenoid) to beta-cryptoxanthin, chemical name is (3R)-β, β-Hu Luobusu-3-alcohol, its molecule is made up of central conjugated polyene chain and terminal six-ring, and have single hydroxyl on one of them terminal six-ring, so molecule is asymmetric.Because the existence of central conjugated polyene chain makes whole molecule have the nonsaturation of height, can form (E/Z) isomer in theory multiple how much, and is wherein the most stable with following formula alltrans isomer:
The form that beta-cryptoxanthin is monomer or beta-cryptoxanthin ester usually is present in the flower or fruit tissue of high plants such as orange, red pepper, pawpaw, pumpkin, wintercherry, persimmon, loquat.Generally speaking, the plant that contains beta-cryptoxanthin often contains other carotenoid such as xenthophylls, zeaxanthin simultaneously, because these structural carotenoids are very close with chemical property, so they are separated very difficulty fully.WO 2004/029275 discloses a kind of method of utilizing composite fungus agent to produce zeaxanthin and beta-cryptoxanthin, and beta-cryptoxanthin content is 2.1-3.5mg/L in this specification sheets the 12nd table.CN 1388830A discloses the microbe preparation method of multiple carotenoid, in culturing process by being controlled in the culturing process concentration by the dissolved oxygen of the liquid substratum of control, change the ratio of the carotinoid compounds (astaxanthin, ADX, β-Hu Luobusu, myoxanthin, canthaxanthin, zeaxanthin, beta-cryptoxanthin, 3-hydroxyl myoxanthin, adonirubin etc.) that generates like this, embodiment 3 table 7 data declarations content of beta-cryptoxanthin in culture is 0.1mg/L.Just because of this, in the market only by several beta-cryptoxanthin products, the beta-cryptoxanthin product sold of Cotion company for example, its beta-cryptoxanthin content only is 0.2%, and its application is very restricted.Therefore, be necessary to study a kind of can be from natural phant more high-level efficiency extract and the production technique of separating beta-cryptoxanthin.On the prior art basis, the inventor has finished from extract the method for beta-cryptoxanthin from Calyx Physalis finally through lot of experiments.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of method of extracting the enriched material that contains beta-cryptoxanthin from Calyx Physalis.
Another object of the present invention provides a kind of enriched material that contains beta-cryptoxanthin.
Another object of the present invention provides a kind of purposes that contains the enriched material of beta-cryptoxanthin.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of method of extracting the enriched material that contains beta-cryptoxanthin from Calyx Physalis.The step of this method is as follows:
A, raw materials pretreatment
Under the temperature 30-50 ℃ of condition with lucifuge, Calyx Physalis is dried to its water-content below 10%, is ground into the Calyx Physalis powder again in Calyx Physalis weight;
B, enzyme are handled
(1) gets 800-1400 weight parts water and water temperature transferred to 20～50 ℃, add 0.5-2.0 weight part cellulase and 0.1-0.4 weight part polygalacturonase then, again with mineral acid or mineral alkali pH regulator to 4～7 with its solution, activate 20-60min down for 20～50 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 8～300 weight parts is sprayed onto the 8-60 weight part by steps A) in the Calyx Physalis powder that obtains, stir again, compacting, sealing, at 20～50 ℃ of following lucifuges insulation 4～96h of temperature, obtain a kind of enzyme and handle the Calyx Physalis powder;
(3) described enzyme is handled the Calyx Physalis powder and is dried to its water content counts 10～13% with enzyme processing Calyx Physalis grain weight amount under lucifuge and temperature 30-50 ℃ condition;
C, extraction
Taking by weighing the 8-12 weight part at step B) the dry enzyme that obtains handles the Calyx Physalis powder, under 2～50 ℃ of conditions of temperature, use 30-80 weight part organic solvent to carry out refluxing extraction 30～90min, separation and Extraction liquid then, leftover materials repeat to extract 3～6 times again, united extraction liquid;
The extracting solution that merges pressure-0.06～-carry out vacuum concentration under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain a kind of enriched material;
D, saponification
It is to dissolve in 1: 10～1: 4 according to the volume ratio of normal hexane and described united extraction liquid that described enriched material uses normal hexane, the enriched material solution that obtains carries out saponification reaction 0.5～12h with 20～50% alkaline ethanol solutions again under 4～50 ℃ of volume ratio 6: 1～12: 1, temperature, lucifuge and the stirring condition of described enriched material solution and described alkaline ethanol solution, obtain a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use organic acid or mineral acid that the pH value of described saponification liquor is adjusted to 4～7; Then pressure-0.06～-be concentrated under the condition of 20～40 ℃ of 0.09MPa and temperature dried; The condensed cream acetic acid ethyl dissolution that obtains, its solution carries out silica gel column chromatography to be separated, with normal hexane as the eluent wash-out, collection contains the wash-out part of beta-cryptoxanthin, again pressure-0.06～-carry out concentrating under reduced pressure under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain containing the enriched material of beta-cryptoxanthin.
A preferred embodiment of the invention, described Calyx Physalis can use Root of Franchet Groundcherry, wintercherry leaf or wintercherry herb to replace.
According to another kind of preferred implementation of the present invention, the granularity of described Calyx Physalis powder is the 20-100 order.
According to another kind of preferred implementation of the present invention, at step B) mineral acid that uses is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; Mineral alkali is selected from sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or saleratus.
According to another kind of preferred implementation of the present invention, the enzyme work 〉=4000IU/g of described cellulase, the enzyme work 〉=5000IU/g of described polygalacturonase.
According to another kind of preferred implementation of the present invention, step C) organic solvent that uses is selected from normal hexane, ethyl acetate, No. six solvent oils or sherwood oil.
According to another kind of preferred implementation of the present invention, described alkaline ethanol solution is sodium hydroxide ethanolic soln or potassium hydroxide-ethanol solution.
According to another kind of preferred implementation of the present invention, step e) organic acid that uses is selected from citric acid, oxysuccinic acid or succsinic acid, and mineral acid is phosphoric acid or hydrochloric acid.
The invention still further relates to the enriched material that adopts described method to obtain, it is characterized in that it contains in the beta-cryptoxanthin of enriched material weight more than 10%.
The invention still further relates to the purposes of described enriched material in preparation foodstuff additive, functional foodstuff, medicine and fodder additives.
Below the present invention will be described in more detail.
The present invention relates to a kind of method of extracting the enriched material that contains beta-cryptoxanthin from Calyx Physalis.The step of this method is as follows:
A, raw materials pretreatment
Under the temperature 30-50 ℃ of condition with lucifuge, Calyx Physalis is dried to its water-content below 10%, is ground into the Calyx Physalis powder again in Calyx Physalis weight;
In the present invention, except described Calyx Physalis, can also use Root of Franchet Groundcherry, wintercherry leaf or wintercherry herb.
Described Calyx Physalis and Root of Franchet Groundcherry, wintercherry leaf or wintercherry herb all need to carry out drying and pulverize pre-treatment.
In the present invention, when drying, can use that normally used drying plant carries out drying in the Chinese medicinal materials processing technology, for example the GZX-9146MBE type digital display air dry oven produced of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. carries out drying.
In the present invention, described pulverizing is to use in the Chinese medicinal materials processing technology normally used disintegrating apparatus that Calyx Physalis is carried out high speed shear and pulverizes, and is crushed to the 20-100 order.
Among the present invention, employed pulverizer can be the normally used pulverizer of selling in the market in the Chinese medicinal materials processing technology, for example the food masher produced of the new friendly machinofacture in Jiangyin City company limited.Typically use pulverizer raw material pulverizing is arrived certain particle size, sieve with steel then, collect the following Calyx Physalis powder of 20-100 order.
In the present invention, described lucifuge should be appreciated that it is to allow pending Calyx Physalis be under the airtight and not unglazed environment.
B, enzyme are handled
(1) gets 800-1400 weight parts water and water temperature transferred to 20～50 ℃, add 0.5-2.0 weight part cellulase and 0.1-0.4 weight part polygalacturonase then, again with mineral acid or mineral alkali pH regulator to 4～7 with its solution, activate 20-60min down for 20～50 ℃ in temperature, so obtain a kind of enzyme treatment solution.
Cellulase (EC 3.2.1.4) is a kind of important enzyme product, is a kind of prozyme, mainly is made up of circumscribed beta-glucanase, inscribe beta-glucanase and beta-glucosidase etc.Usually, cellulase is divided into three classes: C1 enzyme, Cx enzyme and β Polyglucosidase.The C1 enzyme is the enzyme that Mierocrystalline cellulose is worked at first, destroys the crystalline texture of cellulose chain.The Cx enzyme is Mierocrystalline cellulose, the decomposition β-1 that acts on through the C1 enzyme activation, the cellulase of 4-glycosidic link.The β Polyglucosidase can be decomposed into glucose with cellobiose, procellose and other low molecule cellodextrins.
In the present invention, described cellulase for example is Pangbo Bioengineering Co Ltd, Nanning's production of cellulose enzyme.
According to the present invention, if the enzyme work of described cellulase is lower than 4000IU/g, then can be not high because of enzyme activity, and need to use a large amount of cellulases to guarantee that the raw material cell wall broken wall is abundant, therefore, the enzyme work of described cellulase should be higher than 4000IU/g, in view of the enzyme of the cellulase of selling on the market is lived, the enzyme work of described cellulase is 4000～10000IU/g, preferably 5000～9000IU/g, more preferably 6000～8000IU/g.
Wherein, enzyme work is defined as 1 gram enzyme powder or 1ml enzyme liquid under 40 ℃ of conditions with pH4.6, and it is 1 enzyme work unit that 1 hour decomposing soluble starch produces the enzyme amount of 1mg glucose.
Polygalacturonase is a multienzyme complex of decompose pectin, generally includes protopectinase, pectinesterase lytic enzyme, pectinesterase.Combined action by them is decomposed pectin substance fully.Natural pectin substance changes into the pectin of water dissolvable under the protopectinase effect; Pectin is generated pectic acid by pectin methyl esters lytic enzyme catalytic elimination methyl esters group; Pectic acid generates galacturonic acid through pectic acid hydrolase and the degraded of pectate lyase class.In the present invention, described polygalacturonase for example is that Pangbo Bioengineering Co Ltd, Nanning produces polygalacturonase.
According to the present invention, if the enzyme work of described polygalacturonase is lower than 5000IU/g, then can be not high because of enzyme activity, and need to use a large amount of polygalacturonases to guarantee that the whole hydrolysis of the pectin that raw material is contained are better discharged to guarantee target compound, therefore, the enzyme work of described polygalacturonase should be higher than 5000IU/g; In view of the enzyme work of the polygalacturonase of selling on the market, therefore the enzyme work of described polygalacturonase is 5000～12000IU/g, preferably 6000～10000IU/g, more preferably 8000～9000IU/g.
Preferably, with 800-1400 weight parts water dissolving 0.8-1.8 weight part cellulase and 0.2-0.4 weight part polygalacturonase; More preferably, with 800-1400 weight parts water dissolving 1.0-1.6 weight part cellulase and 0.2-0.3 weight part polygalacturonase.
In this step, the mineral acid of use is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid, preferably is selected from hydrochloric acid, sulfuric acid or phosphoric acid; More preferably be selected from hydrochloric acid or phosphoric acid.
In this step, the mineral alkali that uses is selected from sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or saleratus, preferably be selected from sodium hydroxide, potassium hydroxide, yellow soda ash, sodium bicarbonate or saleratus, more preferably be selected from sodium hydroxide, yellow soda ash, sodium bicarbonate or saleratus.
In this step, cellulase and polygalacturonase are common enzyme in the plant materials, it can guarantee that the pH scope of enzyme activity is 4～7, in order in reaction process, to guarantee the maximum vigor of enzyme, the pH of reaction solution can not be too high, can not be low excessively, therefore, need be with mineral acid or mineral alkali pH regulator to 4～7 with its enzyme solution.Too high or too low pH can make enzyme suffer irreversible breaking because of the stability that influences enzyme, thereby influences reaction effect.
(2) the described enzyme treatment solution of 8～300 weight parts is sprayed onto the 8-60 weight part by steps A) in the Calyx Physalis powder that obtains, stir again, compacting, sealing, at 20～50 ℃ of following lucifuges insulation 4～96h of temperature, obtain a kind of enzyme and handle the Calyx Physalis powder.
Among the present invention, use common mechanical stirrer or whipping device with described enzyme treatment solution with by steps A) the Calyx Physalis powder mixing that obtains, use compact machine equipment that the density of mixing mixture is improved then, seal with plastic material again, so that can reach the lucifuge effect.In the present invention, employed heat-preserving equipment can be the thermostat water bath that often uses in experimentation, as the DZKW-C type electronic thermostatic water-bath of Beijing Bo Lian medical apparatus corporation, Ltd production.
In this step, preferably use described enzyme treatment solution of 50～250 weight parts and 15-50 weight part by steps A) the Calyx Physalis powder that obtains.More preferably use described enzyme treatment solution of 100～180 weight parts and 25-40 weight part by steps A) the Calyx Physalis powder that obtains.
In this step, preferably, the mixture of described enzyme treatment solution and Calyx Physalis powder is at 25～45 ℃ of following lucifuge insulation 10～85h of temperature.More preferably, the mixture of described enzyme treatment solution and Calyx Physalis powder is at 30～40 ℃ of following lucifuge insulation 20～75h of temperature.
(3) described enzyme is handled the Calyx Physalis powder and is dried to its water content counts 10～13% with enzyme processing Calyx Physalis grain weight amount under lucifuge and temperature 30-50 ℃ condition.The GZX-9146MBE type digital display air dry oven that for example uses medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. to produce carries out drying.
C, extraction
Taking by weighing the 8-12 weight part at step B) the dry enzyme that obtains handles the Calyx Physalis powder, under 2～50 ℃ of conditions of temperature, use 30-80 weight part organic solvent to carry out refluxing extraction 30～90min, separation and Extraction liquid then, leftover materials repeat to extract 3～6 times again, united extraction liquid.
Preferably, taking by weighing the 8-12 weight part at step B) the dry enzyme that obtains handles the Calyx Physalis powder, uses 35-70 weight part organic solvent to carry out refluxing extraction 40～80min under 10～40 ℃ of conditions of temperature.
Described organic solvent is selected from normal hexane, ethyl acetate, No. six solvent oils or sherwood oil.Wherein No. six solvent oils are colourless transparent liquid, are the mixtures of various lower paraffin hydrocarbonss.Product fraction scope is wide than industrial hexane, has the similar character of industrial hexane.Can be miscible with the most liquid fats except that Viscotrol C, the solubilized lower fatty acid meets standard GB 1669-96.Sherwood oil (BP:60～90 ℃) is an oils, is the mixture of low relative molecular mass alkanes.Normal hexane and ethyl acetate are the solvents that very generally uses in the chemical technology field.They all are product solds in the market.
United extraction liquid pressure-0.06～-carry out vacuum concentration under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain a kind of enriched material;
Among the present invention, used extraction and concentrating unit for example are by the Shanghai RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces that shakes, capacity is 10L, and vacuum pump is SHZ-D (III) the type circulation ability of swimming vacuum pump of being produced by Yuhua Instrument Co., Ltd., Gongyi City.
D, saponification
It is to dissolve in 1: 10～1: 4 according to the volume ratio of normal hexane and described united extraction liquid that described enriched material uses normal hexane, the enriched material solution that obtains carries out saponification reaction 0.5～12h with 20～50% alkaline ethanol solutions again under 4～50 ℃ of volume ratio 6: 1～12: 1, temperature, lucifuge and the stirring condition of described enriched material solution and described alkaline ethanol solution, obtain a kind of saponification liquor.
20～50% alkaline ethanol solutions are prepared according to ordinary method with potassium hydroxide and sodium hydroxide.
According to the present invention, if the volume ratio of normal hexane and described united extraction liquid less than 1: 10, then can be, and medicinal extract can not be dissolved fully owing to the normal hexane consumption is less; If the volume ratio of normal hexane and described united extraction liquid is greater than 1: 4, volume that then can augmenting response liquid, and cause trouble in the processing.In the present invention, the volume ratio of described normal hexane and described united extraction liquid is preferably 1: 8～1: 4.More preferably, the volume ratio of described normal hexane and described united extraction liquid is 1: 6～1: 4.
According to the present invention, if the volume ratio of described enriched material solution and described alkaline ethanol solution greater than 12: 1, then can cause saponification reaction insufficient because of alkali lye with quantity not sufficient, residual saponification beta-cryptoxanthin ester completely not in a large number in the reaction solution; If the volume ratio of described enriched material solution and described alkaline ethanol solution was less than 6: 1, the waste of acid also can cause the monomeric degraded of beta-cryptoxanthin because reaction solution keeps long high alkalinity condition in the time of then can causing the waste of alkali lye and subsequent adjustment pH because the alkali lye consumption is too big.
According to the present invention, if the saponification reaction time less than 0.5h, then can be owing to the reaction times causes reaction abundant inadequately inadequately; If the saponification reaction time then can be owing to long high alkalinity condition causes the monomeric degraded of beta-cryptoxanthin greater than 12h.
Therefore, the volume ratio of described enriched material solution and described alkaline ethanol solution preferably 8: 1～12: 1,10～45 ℃ of temperature, saponification reaction 1.0～10h.More preferably, the volume ratio of described enriched material solution and described alkaline ethanol solution is 8: 1～10: 1,20～40 ℃ of temperature, saponification reaction 2.0～8h.
Described lucifuge is as previously described.
In the present invention, used whipping device is the magnetic stirring apparatus with heating function, as the DF-101S type digital display automatic constant-temperature agitator of being produced by the prosperous training plant and instrument in Shanghai company limited.
E, concentrated and purifying
Under stirring condition, use organic acid or mineral acid that the pH value of described saponification liquor is adjusted to 4～7; Then pressure-0.06～-be concentrated under the condition of 20～40 ℃ of 0.09MPa and temperature dried; The condensed cream acetic acid ethyl dissolution that obtains, its solution carries out silica gel column chromatography to be separated, with normal hexane as the eluent wash-out, collection contains the wash-out part of beta-cryptoxanthin, again pressure-0.06～-carry out concentrating under reduced pressure under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain containing the enriched material of beta-cryptoxanthin.
Of the present invention concentrate with purification step in, described organic acid is selected from citric acid, oxysuccinic acid or succsinic acid, preferably citric acid or oxysuccinic acid.Described mineral acid is phosphoric acid or hydrochloric acid.
According to the present invention, the pH value of described saponification liquor is less than 4, and then formed soap can precipitate and separates out in the saponification reaction process, and carries a large amount of beta-cryptoxanthins secretly, thereby causes the loss of beta-cryptoxanthin; The pH value of described saponification liquor is greater than 7, then can owing to saponification liquor under the meta-alkalescence condition, cause the degraded of beta-cryptoxanthin.Therefore, the pH value of described saponification liquor selects 4～7 for use, and preferably 4.5～6.5; 5.0-6.0 more preferably.
The condensed cream acetic acid ethyl dissolution that obtains, its solution adopt silica gel column chromatography to separate.
The silica gel column chromatography preparation: use normal hexane activation silica gel for chromatography, adopt the wet method filling, post bed length-to-diameter ratio is 3: 1～6: 1, uses normal hexane balance chromatographic column.The silica gel that uses is the silica gel of selling in the market, the G type silica gel produced of subsidiary factory of Haiyang Chemical Plant, Qingdao for example, and the chromatography column of use is the glass chromatography column of customization, and for example column internal diameter is 2.0cm, and the post height is 32cm.
The dress sample: the ratio according to sample to be separated (being the solution of acetic acid ethyl dissolution) volume and column volume is 1: 20, with dropper sample to be separated is joined the chromatography column surface slowly along post jamb, notes not destroying post bed surface.
Adsorption conditions: under standard atmosphere pressure, lower valve is opened, sample to be separated is being immersed in the silicagel column slowly because the normal hexane in the post slowly flows out;
Desorption condition: as eluent, under standard atmosphere pressure, allow under the eluent spontaneous current with 100% normal hexane. carry out wash-out, collect the wash-out part that contains beta-cryptoxanthin;
The wash-out part of collecting again pressure-0.06～-carry out concentrating under reduced pressure under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain containing the enriched material of beta-cryptoxanthin.The concentrating under reduced pressure equipment that uses is equipment as previously described.
The enriched material that obtains adopts conventional H PLC method to detect the content of beta-cryptoxanthin.
The invention still further relates to the enriched material that adopts described method to obtain, it is characterized in that it contains in the beta-cryptoxanthin of enriched material weight more than 10%.The beta-cryptoxanthin content of product of the present invention is higher than prior art or content that currently available products reached far away.
Described enriched material also contains other carotenoid and a certain amount of oil-soluble impuritieses such as a small amount of zeaxanthin, xenthophylls except beta-cryptoxanthin.
The invention still further relates to the purposes of described enriched material in preparation foodstuff additive, functional foodstuff, medicine and fodder additives.
Be noted that and use and add the enriched material that the present invention contains beta-cryptoxanthin according to the relevant regulations of foodstuff additive, functional foodstuff, medicine and fodder additives.
[beneficial effect]
The invention has the beneficial effects as follows:
At present, the wintercherry aboundresources of China mainly concentrates on products such as production wintercherry preserved fruit, wintercherry health care drink and wintercherry wine, and perhaps Calyx Physalis is sold at a low price as medicinal raw material or direct discard processing, causes the significant wastage of resource.Adopt method of the present invention not only to solve and extract the inefficient technological deficiency of beta-cryptoxanthin in the prior art, but also obtain costly beta-cryptoxanthin product, the beta-cryptoxanthin content of product of the present invention is higher than prior art or content that currently available products reached far away, therefore, the application for the beta-cryptoxanthin product provides good prospect.Raw material of the present invention easily obtains, and extraction process is simple, products obtained therefrom content height, and comprehensive cost is controlled, is suitable for suitability for industrialized production and prolongs industrial chain.
[embodiment]
Embodiment 1: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The GZX-9146MBE type air dry oven that places medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. to produce the Calyx Physalis of collecting is dried to water content＜10% under 45 ℃ of temperature, take by weighing the dry place of 1kg calyx, is crushed to≤20 orders through high speed shear.Take by weighing 100g place calyx powder, place the 1000mL graduated cylinder, its volume is 454mL, and its tap density is 0.22g/mL as calculated.
B, enzyme are handled
(1) gets 1000ml water and water temperature transferred to 35 ℃, add the cellulase of 1.0g Pangbo Bioengineering Co Ltd, Nanning production and the polygalacturonase that 0.2g Pangbo Bioengineering Co Ltd, Nanning produces then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 5.0 with its solution, activate 30min down for 25 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 80 grams is sprayed onto 30g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, spray the enzyme treatment solution on one side, stir again, compacting, seal with preservative film, lucifuge insulation 65h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 25 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 10.0% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 45 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 10g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, join in the 10L Rotary Evaporators, under 20 ℃ of conditions of temperature, use the 40g normal hexane to carry out refluxing extraction 30min, then separation and Extraction liquid, leftover materials repeat to extract 3 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 35 ℃ of pressure-0.09MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Take by weighing 40g KOH in the 500mL beaker, under stirring state, slowly add 100mL water and make it whole dissolvings, to wherein adding 95% ethanol 100mL, obtain the 20%KOH ethanolic soln then.
It is to dissolve at 1: 5 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 35 ℃ of volume ratio 6: 1, temperature, lucifuge and the stirring velocity 60rpm/min of described enriched material solution and 20%KOH ethanolic soln, carry out saponification reaction 2.0h, the pH value is 10.0 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 7.0; After leaving standstill 30min, get the upper strata reaction solution, under the condition of 35 ℃ of pressure-0.09MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, and its solution carries out silica gel column chromatography to be separated.
Get silica gel for chromatography, the adding normal hexane also stirs, and adorns post behind the ultrasonic degas 10min, post height of bed 12cm, and post bed diameter is 2.0cm, column volume is about 37mL, with normal hexane balance chromatography column.Get sample 2mL to be separated, slowly join in the silicagel column uniformly with dropper along post jamb, open lower valve, after treating that sample immerses silicagel column fully, use the normal hexane wash-out repeatedly, collection contains the wash-out part of beta-cryptoxanthin, re-use the Shanghai RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces that shakes, under the condition of 20 ℃ of pressure-0.09MPa and temperature, carry out concentrating under reduced pressure, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.87%.
Embodiment 2: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The Calyx Physalis of collecting is placed the GZX-9146MBE type air dry oven of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. production, under 35 ℃ of temperature, be dried to water content＜10%, take by weighing the dry place of 1kg calyx, be crushed to≤20 orders through high speed shear, adopting similarly to Example 1 mode to measure its tap density is 0.22g/mL.
B, enzyme are handled
(1) gets 800ml water and water temperature transferred to 50 ℃, add 2.0g cellulase and 0.1g polygalacturonase similarly to Example 1 similarly to Example 1 then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 4.0 with its solution, activate 60min down for 40 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 8 grams is sprayed onto 8g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, Yi Bian spray the enzyme treatment solution, stir again, compacting, seal with preservative film, lucifuge insulation 4h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 40 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 11.2% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 35 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 12g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, joins in the 10L Rotary Evaporators, uses the 20g normal hexane to carry out refluxing extraction 90min under 2 ℃ of conditions of temperature, separation and Extraction liquid then, leftover materials repeat to extract 2 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 40 ℃ of pressure-0.08MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Prepare the 50%KOH ethanolic soln according to mode similarly to Example 1.
It is to dissolve at 1: 4 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 4 ℃ of volume ratio 12: 1, temperature, lucifuge and the stirring velocity 60rpm/min of described enriched material solution and 50%KOH ethanolic soln, carry out saponification reaction 12.0h, the pH value is 10.2 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 4.0; After leaving standstill 35min, get the upper strata reaction solution, under the condition of 40 ℃ of pressure-0.08MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, its sample separates according to carrying out silica gel column chromatography with the same manner of embodiment 1, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.85%.
Embodiment 3: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The Calyx Physalis of collecting is placed the GZX-9146MBE type air dry oven of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. production, under 30 ℃ of temperature, be dried to water content＜10%, take by weighing the dry place of 1kg calyx, be crushed to≤20 orders through high speed shear, adopting similarly to Example 1 mode to measure its tap density is 0.21g/mL.
B, enzyme are handled
(1) gets 1400ml water and water temperature transferred to 20 ℃, add 0.5g cellulase and 0.3g polygalacturonase similarly to Example 1 similarly to Example 1 then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 7.0 with its solution, activate 20min down for 20 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 150g is sprayed onto 50g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, spray the enzyme treatment solution on one side, stir again, compacting, seal with preservative film, lucifuge insulation 96h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 20 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 12.2% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 30 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 8g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, joins in the 10L Rotary Evaporators, uses the 68g normal hexane to carry out refluxing extraction 40min under 45 ℃ of conditions of temperature, separation and Extraction liquid then, leftover materials repeat to extract 4 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 30 ℃ of pressure-0.06MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Prepare the 40%NaOH ethanolic soln according to mode similarly to Example 1.
It is to dissolve at 1: 6 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 50 ℃ of volume ratio 10: 1, temperature, lucifuge and the stirring velocity 65rpm/min of described enriched material solution and 40%KOH ethanolic soln, carry out saponification reaction 0.5h, the pH value is 10.4 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 6.0; After leaving standstill 30min, get the upper strata reaction solution, under the condition of 30 ℃ of pressure-0.06MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, its sample separates according to carrying out silica gel column chromatography with the same manner of embodiment 1, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.76%.
Embodiment 4: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The Calyx Physalis of collecting is placed the GZX-9146MBE type air dry oven of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. production, under 40 ℃ of temperature, be dried to water content＜10%, take by weighing the dry place of 1kg calyx, be crushed to≤20 orders through high speed shear, adopting similarly to Example 1 mode to measure its tap density is 0.22g/mL.
B, enzyme are handled
(1) gets 1200ml water and water temperature transferred to 40 ℃, add 1.5g cellulase and 0.4g polygalacturonase similarly to Example 1 similarly to Example 1 then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 6.0 with its solution, activate 40min down for 50 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 200g is sprayed onto 60g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, spray the enzyme treatment solution on one side, stir again, compacting, seal with preservative film, lucifuge insulation 80h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 50 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 12.9% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 40 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 9g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, joins in the 10L Rotary Evaporators, uses the 30g normal hexane to carry out refluxing extraction 68min under 50 ℃ of conditions of temperature, separation and Extraction liquid then, leftover materials repeat to extract 6 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 20 ℃ of pressure-0.09MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Prepare the 30%KOH ethanolic soln according to mode similarly to Example 1.
It is to dissolve at 1: 7 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 15 ℃ of volume ratio 8: 1, temperature, lucifuge and the stirring velocity 68rpm/min of described enriched material solution and 30%KOH ethanolic soln, carry out saponification reaction 8h, the pH value is 10.3 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 5.0; After leaving standstill 30min, get the upper strata reaction solution, under the condition of 20 ℃ of pressure-0.09MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, its sample separates according to carrying out silica gel column chromatography with the same manner of embodiment 1, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.65%.
Embodiment 5: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The Calyx Physalis of collecting is placed the GZX-9146MBE type air dry oven of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. production, under 50 ℃ of temperature, be dried to water content＜10%, take by weighing the dry place of 1kg calyx, be crushed to≤20 orders through high speed shear, adopting similarly to Example 1 mode to measure its tap density is 0.21g/mL.
B, enzyme are handled
(1) gets 900ml water and water temperature transferred to 25 ℃, add 0.8g cellulase and 0.15g polygalacturonase similarly to Example 1 similarly to Example 1 then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 5.5 with its solution, activate 50min down for 30 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 300g is sprayed onto 40g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, spray the enzyme treatment solution on one side, stir again, compacting, seal with preservative film, lucifuge insulation 45h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 30 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 10.8% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 50 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 11g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, join in the 10L Rotary Evaporators, under 12 ℃ of conditions of temperature, use the 80g normal hexane to carry out refluxing extraction 60min, then separation and Extraction liquid, leftover materials repeat to extract 5 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 25 ℃ of pressure-0.08MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Prepare the 35%NaOH ethanolic soln according to mode similarly to Example 1.
It is to dissolve at 1: 8 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 40 ℃ of volume ratio 9: 1, temperature, lucifuge and the stirring velocity 60rpm/min of described enriched material solution and 35%KOH ethanolic soln, carry out saponification reaction 4h, the pH value is 10.5 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 4.5; After leaving standstill 30min, get the upper strata reaction solution, under the condition of 25 ℃ of pressure-0.08MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, its sample separates according to carrying out silica gel column chromatography with the same manner of embodiment 1, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.87%.
Embodiment 6: the present invention contains the preparation of the enriched material of beta-cryptoxanthin
Implementation step is as follows:
A, raw materials pretreatment
The Calyx Physalis of collecting is placed the GZX-9146MBE type air dry oven of medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. production, under 48 ℃ of temperature, be dried to water content＜10%, take by weighing the dry place of 1kg calyx, be crushed to≤20 orders through high speed shear, adopting similarly to Example 1 mode to measure its tap density is 0.20g/mL.
B, enzyme are handled
(1) gets 1100ml water and water temperature transferred to 30 ℃, add 1.8g cellulase and 0.35g polygalacturonase similarly to Example 1 similarly to Example 1 then, again with hydrochloric acid or sodium hydroxide dilute aqueous soln pH regulator to 6.5 with its solution, activate 45min down for 45 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 250g is sprayed onto 18g by steps A) in the Calyx Physalis powder that obtains, on one side to adding material, spray the enzyme treatment solution on one side, stir again, compacting, seal with preservative film, lucifuge insulation 20h obtains a kind of enzyme and handles the Calyx Physalis powder in the thermostat water bath of 45 ℃ of temperature;
(3) described enzyme is handled the Calyx Physalis powder and is evenly placed the stainless steel pallet, is dried to its water content and counts 11.8% with enzyme processing Calyx Physalis grain weight amount in the GZX-9146MBE type digital display air dry oven that medical apparatus and instruments factory of Shanghai Boxun Industrial Co., Ltd. produces under the condition of 48 ℃ of lucifuge and temperature;
C, extraction
Taking by weighing 10.5g at step B) the dry enzyme that obtains handles the Calyx Physalis powder, join in the 10L Rotary Evaporators, under 32 ℃ of conditions of temperature, use the 55g normal hexane to carry out refluxing extraction 75min, then separation and Extraction liquid, leftover materials repeat to extract 3 times again, united extraction liquid;
Use Shanghai to shake RE-5210A type Rotary Evaporators that prompt experimental installation company limited produces, united extraction liquid carries out vacuum concentration under the condition of 28 ℃ of pressure-0.06MPa and temperature, obtain a kind of orange enriched material;
D, saponification
Prepare the 45%KOH ethanolic soln according to mode similarly to Example 1.
It is to dissolve at 1: 10 according to the volume ratio of normal hexane and described united extraction liquid that described orange enriched material uses normal hexane, obtains enriched material solution and installs in the triangular flask.
The triangular flask that fills enriched material solution is placed on the magnetic stirring apparatus, under the condition of 25 ℃ of volume ratio 7: 1, temperature, lucifuge and the stirring velocity 64rpm/min of described enriched material solution and 45%KOH ethanolic soln, carry out saponification reaction 6.0h, the pH value is 10.1 during reaction terminating, obtains a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use phosphoric acid that the pH value of described saponification liquor is adjusted to 5.5; After leaving standstill 30min, get the upper strata reaction solution, under the condition of 28 ℃ of pressure-0.06MPa and temperature, be concentrated into dried then; The condensed cream that obtains obtains sample to be separated with acetic acid ethyl dissolution, its solution separates according to carrying out silica gel column chromatography with the same manner of embodiment 1, obtain containing the enriched material of beta-cryptoxanthin, adopting conventional H PLC method to detect its beta-cryptoxanthin content is 10.64%.
Claims (10)
1. one kind is extracted the method for the enriched material contain beta-cryptoxanthin from Calyx Physalis, it is characterized in that the step of this method is as follows:
A, raw materials pretreatment
Under the temperature 30-50 ℃ of condition with lucifuge, Calyx Physalis is dried to its water-content below 10%, is ground into the Calyx Physalis powder again in Calyx Physalis weight;
B, enzyme are handled
(1) gets 800-1400 weight parts water and water temperature transferred to 20～50 ℃, add 0.5-2.0 weight part cellulase and 0.1-0.4 weight part polygalacturonase then, again with mineral acid or mineral alkali pH regulator to 4～7 with its solution, activate 20-60min down for 20～50 ℃ in temperature, so obtain a kind of enzyme treatment solution;
(2) the described enzyme treatment solution of 8～300 weight parts is sprayed onto the 8-60 weight part by steps A) in the Calyx Physalis powder that obtains, stir again, compacting, sealing, at 20～50 ℃ of following lucifuges insulation 4～96h of temperature, obtain a kind of enzyme and handle the Calyx Physalis powder;
(3) described enzyme is handled the Calyx Physalis powder and is dried to its water content counts 10～13% with enzyme processing Calyx Physalis grain weight amount under lucifuge and temperature 30-50 ℃ condition;
C, extraction
Taking by weighing the 8-12 weight part at step B) the dry enzyme that obtains handles the Calyx Physalis powder, under 2～50 ℃ of conditions of temperature, use 30-80 weight part organic solvent to carry out refluxing extraction 30～90min, separation and Extraction liquid then, leftover materials repeat to extract 3～6 times again, united extraction liquid;
The extracting solution that merges pressure-0.06～-carry out vacuum concentration under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain a kind of enriched material;
D, saponification
It is to dissolve in 1: 10～1: 4 according to the volume ratio of normal hexane and described united extraction liquid that described enriched material uses normal hexane, the enriched material solution that obtains carries out saponification reaction 0.5～12h with 20～50% alkaline ethanol solutions again under 4～50 ℃ of volume ratio 6: 1～12: 1, temperature, lucifuge and the stirring condition of described enriched material solution and described alkaline ethanol solution, obtain a kind of saponification liquor;
E, concentrated and purifying
Under stirring condition, use organic acid or mineral acid that the pH value of described saponification liquor is adjusted to 4～7; Then pressure-0.06～-be concentrated under the condition of 20～40 ℃ of 0.09MPa and temperature dried; The condensed cream acetic acid ethyl dissolution that obtains, its solution carries out silica gel column chromatography to be separated, with normal hexane as the eluent wash-out, collection contains the wash-out part of beta-cryptoxanthin, again pressure-0.06～-carry out concentrating under reduced pressure under the condition of 20～40 ℃ of 0.09MPa and temperature, obtain containing the enriched material of beta-cryptoxanthin.
2. preparation method according to claim 1 is characterized in that described Calyx Physalis replaces with Root of Franchet Groundcherry, wintercherry leaf or wintercherry herb.
3. method according to claim 1, the granularity that it is characterized in that described Calyx Physalis powder is less than the 20-100 order.
4. method according to claim 1 is characterized in that at step B) mineral acid that uses is selected from hydrochloric acid, sulfuric acid, nitric acid or phosphoric acid; Mineral alkali is selected from sodium hydroxide, potassium hydroxide, yellow soda ash, salt of wormwood, sodium bicarbonate or saleratus.
5. preparation method according to claim 1 is characterized in that the enzyme work 〉=4000IU/g of described cellulase, the enzyme work 〉=5000IU/g of described polygalacturonase.
6. method according to claim 1 is characterized in that step C) organic solvent that uses is selected from normal hexane, ethyl acetate, No. six solvent oils or sherwood oil.
7. method according to claim 1 is characterized in that described alkaline ethanol solution is sodium hydroxide ethanolic soln or potassium hydroxide-ethanol solution.
8. method according to claim 1 is characterized in that step e) organic acid that uses is selected from citric acid, oxysuccinic acid or succsinic acid, and mineral acid is phosphoric acid or hydrochloric acid.
9. the enriched material that obtains according to the described method of arbitrary claim among the claim 1-8 is characterized in that it contains in the beta-cryptoxanthin of enriched material weight more than 10%.
10. according to the purposes of the described enriched material of claim 9 in preparation foodstuff additive, functional foodstuff, medicine and fodder additives.
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| WO2014115037A3 (en) * | 2013-01-24 | 2014-12-31 | Omniactive Health Technologies Ltd. | Beta-cryptoxanthin from plant source and a process for its preparation |
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| CN103664724A (en) * | 2012-09-12 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for extracting zeaxanthine from physalis alkekengi and fruits through one-pot method |
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| CN104906112A (en) * | 2015-05-20 | 2015-09-16 | 杨克西 | Compound for promoting protein synthesis and preparing method and application thereof |
| CN112773844A (en) * | 2019-11-09 | 2021-05-11 | 佛山市善玺化妆品股份有限公司 | Novel medium for promoting protein synthesis and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN102219721B (en) | 2013-08-07 |
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