CN104004048A - High-utilization-rate extraction and processing method of wrinkled papaya - Google Patents
High-utilization-rate extraction and processing method of wrinkled papaya Download PDFInfo
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- CN104004048A CN104004048A CN201410228898.8A CN201410228898A CN104004048A CN 104004048 A CN104004048 A CN 104004048A CN 201410228898 A CN201410228898 A CN 201410228898A CN 104004048 A CN104004048 A CN 104004048A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
Abstract
The invention discloses a high-utilization-rate extraction and processing method of wrinkled papaya. The method comprises the following steps: cutting fresh wrinkled papaya fruits, juicing, extracting SOD (superoxide dismutase) and papaya juice from separated papaya puree, and preparing oleanolic acid and animal feeds by using residual peels and fruit residues. In the whole process, all parts of the winkled papaya are utilized as much as possible, harmful organic solvents are introduced as less as possible, and wastes are generated as less as possible. Therefore, the method has the characteristics of high utilization rate and ecological environmental protection property, the technical support is provided for full utilization of the value of the wrinkled papaya, the economic value is brought to planters as much as possible, and the promotional value and the prospect are very high.
Description
Technical field
The present invention relates to a kind of Zou's skin pawpaw high utilization rate and extract and complete processing, belong to vegetables and fruits deep processing technology method research field.
Background technology
Cockle pawpaw (Chaenomeles speciosa (Sweet) Nakai) is a kind of medicinal and edible plant, is rich in multiple bioactive ingredients.China is cockle pawpaw country of origin, and it is mainly distributed in the ground such as East China, Central China and southwest.
In cockle pawpaw, be rich in the bioactive ingredients of multiple needed by human body, as organic acid, pentacyclic triterpene, flavonoid, saponins, phenols, superoxide-dismutase, volatile oil, vitamins, trace element etc.Wherein organic acid, flavonoid and superoxide-dismutase, because having higher medical and anti-oxidant activity, are worth larger.
In cockle pawpaw, organic acid and tannin composition are higher, and fruit texture is hard, fiber is more, vascular bundle is flourishing, mouthfeel is sour and astringent, should not directly eat, so its processing technology seems particularly important in the utilization of Zou's skin pawpaw.
The current processing for this Zou's skin pawpaw also, in comparing the primary stage, is mainly used as the exploitation of the aspects such as the prepared slices of Chinese crude drugs (drying by direct slicing), Sucus Chaenomelis, papaya ester and pawpaw can.And directly abandoning of having for materials such as a large amount of discarded pawpaw skins and slags, being used for of having made compost or dried as feed.And above simple processing is for containing this kind of enriching organic acid, superoxide-dismutase, it is too low that its utility value and utilization ratio just seem.
Summary of the invention
The object of the invention is to overcome the deficiency that above-mentioned prior art exists, provide a kind of Zou's skin pawpaw high utilization rate to extract and working method.Method of the present invention is on the basis of existing extractive technique, carry out combination, optimization and the lifting of various extractive techniques, by the evaluation to Zou's skin pawpaw effective constituent, formulated the technical matters route that utilizes as much as possible its various piece, this technological line is by the introducing organic solvent the least possible or use on the basis of harmless solvent, its effective constituent/component of acquisition as much as possible, at utmost improves its economic use value.Selected Zou's skin pawpaw effective constituent/component of extracting is respectively superoxide-dismutase (SOD enzyme), Oleanolic Acid and pawpaw juice, and residual residue is used for preparing animal-feed.
The object of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of Zou's skin pawpaw high utilization rate and extract and working method, described method comprises the steps:
A, Zou's skin pawpaw are crushed to pasty state after mixing with water, and conventional filtration, carries out centrifugation to filtrate;
B, supernatant liquor filter through 0.22 μ m aperture filtering membrane;
C, filtered solution are 50,000 ultra-filtration membrane packet filterings through molecular weight cut-off;
D, filtered solution are 5,000 ultra-filtration membrane packet filterings through molecular weight cut-off;
E, trapped fluid carry out SOD enzyme precipitation by acetone method, and throw out, through frozen drying, obtains SOD enzyme;
F, the trapped fluid of the filtered solution of described 5,000 ultra-filtration membrane packet filterings and 50,000 ultra-filtration membrane packet filterings is merged, obtain pawpaw juice raw material;
G, the throw out of the filter residue of described conventional filtration and centrifugation gained is carried out to dehydrated alcohol lixiviate, filtration under ultrasonic wave is auxiliary; Cleaner liquid is removed after ethanol to obtain Oleanolic Acid crude product, the residue animal-feed of drying, pulverize, sieve and to obtain.
In above-mentioned steps, by conventional filtration method, remove robust fibre; 0.22 μ m aperture filtering membrane filtration removal bacterium and macromolecular particle material, molecular weight cut-off are that the ultrafiltration membrance filter bag of 50,000 ultra-filtration membrane packet filterings removal part foreign proteins, molecular weight cut-off 5,000 filters removal inorganics and ion.Technical process of the present invention reduces use link and the usage quantity of harmful organic solvent as far as possible, and produced simultaneously product as much as possible improves the use value of Zou's skin pawpaw.The raw material that the SOD enzyme product making can be further used as other products is used; In addition, because Zou's skin pawpaw fresh fruit shreds and first the supernatant liquor that carries out after conventional filtration adopted 0.22 μ m filter membrane, bacterium and macrobead thing have been removed, and after ultra-filtration process in without any the introducing of solvent and other pollutents, therefore, by described 5, the filtered solution of 000 ultra-filtration membrane packet filtering and 50, the trapped fluid of 000 ultra-filtration membrane packet filtering merges in clean environment, and the pawpaw juice raw material making can be used as the raw material of exploitation drink of Chinese flowering quince juice, papaya ester and other interpolation Sucus Chaenomelis liquid products.
Preferably, in steps A, it is that 30～50g is block that Zou's skin pawpaw fresh fruit is cut into weight, then mixes with the water of twice quality; After being crushed to pasty state, also comprise lixiviate 1h, the step stirring with the speed of 50～100 revs/min in leaching process.The object of lixiviate is to urge the stripping into enzyme.
Preferably, described conventional filtration is specially: after 8 layers of hospital gauze that stack through 45 ° of intersections filter, obtain coarse filtration liquid, then carry out decompress filter with quick filter paper, obtain crude enzyme liquid; Described centrifugation is specially: described crude enzyme liquid is heated rapidly to 60 ℃ and keep 20min, stops heating, static to after room temperature with the centrifugal 15min of 5000r/min speed.
Preferably, step C carries out ultrafiltration with the speed of 300ml/min.Ultrafiltration object is to remove molecular weight and hands over large foreign protein, sees through the raw material that liquid further extracts as SOD enzyme, and trapped fluid is retained as the raw material of Sucus Chaenomelis liquid product, this step trapped fluid: see through liquid=1: 9.
Preferably, step D carries out ultrafiltration with the speed of 200ml/min.Ultrafiltration object is to remove small molecules inorganics and ion, and trapped fluid is SOD enzyme concentrated solution, gives over to Sucus Chaenomelis series products raw material, this step trapped fluid: see through liquid=2: 1 and see through liquid.
Preferably, in step e, acetone is pre-chilled to 4 ℃, mix with described trapped fluid to be placed in-20 ℃ of refrigerator-freezers and spend the night, then under 4 ℃ of conditions, centrifugal under 12000r/min speed, get precipitation part, use washing with acetone three times, the precipitation finally obtaining is that 45 ℃, resolution temperature are that 60 ℃ of frozen drying methods obtain dry SOD enzyme powder by operating pressure 50Pa, sublimation temperature again; The volume ratio of described trapped fluid and acetone is 1: 1.SOD enzyme lyophilized powder-20 ℃ that make save backup.
Preferably, in step G, described dehydrated alcohol lixiviate is carried out under 60 ℃ of ultrasonic wave are auxiliary, and extraction time is 20min, and solid-liquid ratio is 1: 20.
Preferably, in step G, described removal ethanol is specially: by 60 ℃ of rotation method of enrichment, remove ethanol.
Lixiviate finishes, and 8 layers of hospital gauze that material is stacked by 45 ° of intersections filter, and obtain coarse filtration liquid, then by quick filter paper level, carry out decompress filter, obtain clear liquor.Clear liquor adopts the means of rotary evaporation to remove ethanol, obtain brown viscous liquid, add subsequently the distilled water of 10 times of weight of material to carry out twice washing, after standing, by suction filtration, carry out solid-liquid separation, getting upper strata powder and be Oleanolic Acid crude product, is that 55 ℃, resolution temperature are that under 70 ℃ of conditions, moisture is further removed in vacuum-drying in operating pressure 50Pa, sublimation temperature subsequently.The filter residue of holding back can animal-feed raw material, its rich cellulose and polysaccharose substance.
Preferably, in step G, activated carbon decolorizing, the crystallizing process under low temperature that the Oleanolic Acid crude product obtaining after described removal ethanol is solvent through petroleum ether degreasing, the ethanol of take successively obtain Oleanolic Acid sterling.
Because Oleanolic Acid is insoluble in water, so it is mainly present among pomace and pericarp; The pericarp being trapped while carrying out conventional filtration after therefore the stripping and slicing of Zou's skin pawpaw fresh fruit being pulverized and pomace part are using the raw material as extracting Oleanolic Acid, by using harmless solvent dehydrated alcohol to carry out lixiviate 20min as solvent under 60 ℃ of ultrasonic wave are auxiliary, then by ordinary method, cross leaching clear liquid part, then obtain Oleanolic Acid sterling after removing ethanol by 60 ℃ of rotation method of enrichment.The activated carbon decolorizing, the crystallizing process under low temperature that by petroleum ether degreasing, the ethanol of take, are solvent more afterwards obtain Oleanolic Acid sterling.This technical process leaching process adopts ethanol as solvent, and a large amount of residues that produce can be recycled, rather than becomes rubbish increase environmental pollution and burden.Activated carbon decolorizing, the crystallizing process under low temperature that petroleum ether degreasing, the ethanol of take are solvent are specially: the crude product obtaining be take sherwood oil again as solvent, with apparatus,Soxhlet's, carries out degreasing, with obscure glass, detect when siphon pipe outflow solvent does not have fat substantially and stop, and degreasing completes.Under identical vacuum lyophilization condition, process and obtain Oleanolic Acid powder subsequently.And then by a small amount of 100% dissolve with ethanol for the Oleanolic Acid crude product after degreasing, reflux, progressively adds ethanol to make hot saturated solution, add gac to boiling after 0.5h decolour.Then carry out heat filtering fast transfer filtrate, after filtrate is cooling, crystallize out, and carry out recrystallization, obtain Oleanolic Acid sterling.
Preferably, in step G, described bake out temperature is 60 ℃; Described sieving as crossing 10～20 mesh sieves.
Because a large amount of residue producing in the filtration of lixiviate Oleanolic Acid only contains alcohol solvent, and ethanol is a kind of harmless solvent, so residue can be used as animal-feed raw material, uses.Its processing process is: residue first carries out drying treatment at 60 ℃, then dried filter residue is carried out to pulverizing again with pulverizer, and crosses 10-20 mesh sieve.Screened part is qualified part, and not screened part continue to be crushed to qualified.This animal-feed can directly be used, and the raw material that also can be used as formula feed is used.
Compared with prior art, the present invention has following beneficial effect: the present invention, in whole technological process, has considered economic benefit, ecological friendly and the sustainable developability of Zou's skin pawpaw of output in unit surface substantially.In technique invention, by various experiments, the active substance of Zou's skin pawpaw various piece is measured, according to measurement result, formulated best testing program simultaneously and to reach loss lowest energy, obtain the object of maximum useful output.In described method steps A., Zou's skin pawpaw+water carries out in crushing process, the common way of prior art is to add pH7.8 and above phosphoric acid buffer to increase the activity of enzyme, but all liquid part after extraction enzyme and residue part can not be re-used as the exploitation raw material of fruit juice and animal-feed, when having reduced its economic worth, environment has been caused to white elephant.At SOD enzyme, concentrate and purification phase simultaneously, the present invention has adopted the mode of membrane filtration but not ammonium sulfate+acetone precipitation mode, the raw material that makes a large amount of juices can be used as Nakai beverage is used, in total economic worth and be all greatly improved in ecological friendly.In the leaching process of Oleanolic Acid, security and Zou's skin pawpaw of considering alcohol solvent contain abundant fiber and trace element, and residue is by being processed into the form of animal-feed but not simply as land for growing field crops fertilizer, has further promoted its economic use value.Therefore in the present invention in the various piece of utilizing as much as possible Zou's skin pawpaw, simultaneously the least possible introducing harmful organic solvent, simultaneously the least possible generation waste; Therefore, method of the present invention has high utilization rate and eco-environmental prote, for making full use of of Zou's skin pawpaw value provides technical support, simultaneously also for grower brings economic worth as much as possible, has very high promotional value and prospect.
Accompanying drawing explanation
By reading the detailed description of non-limiting example being done with reference to the following drawings, it is more obvious that other features, objects and advantages of the present invention will become:
Fig. 1 is the schematic flow sheet of Zou's skin pawpaw high utilization rate extraction of the present invention and working method.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art further to understand the present invention, but not limit in any form the present invention.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
embodiment
The present embodiment relates to a kind of Zou's skin pawpaw high utilization rate effective constituent/component and extracts and working method; Zou's skin pawpaw fresh fruit is squeezed the juice after chopping, and the pawpaw magma after separation is used for extracting SOD enzyme and pawpaw juice, and remaining pericarp and pomace are partly used for preparing Oleanolic Acid and animal-feed.Condition of storage after pawpaw fresh fruit is plucked is to preserve in Cool Room 4℃, and preservation period is 2-3 month.Total technological line as shown in Figure 1, specifically comprises the steps:
A, 200g pawpaw is cleaned to stripping and slicing (fruit piece size is 30～50g/ piece), according to pawpaw: water=1: 2 weight ratios add tap water 400g, with stirrer, carry out homogenate subsequently, static 1 hour, then 8 layers of hospital gauze that stack by 45 ° of intersections filter, obtain coarse filtration liquid, then by quick filter paper level, carry out decompress filter, obtain crude enzyme liquid stand-by.This process obtains pomace 67g.
B, gained crude enzyme liquid are heated to 60 ℃ and keep 20min to carry out thermally denature, rear static to room temperature, centrifugal 15min under the speed of 5000r/min then, and supernatant liquor further extracts raw material as SOD enzyme, and supernatant liquor constant volume is to 550ml.
C, the supernatant liquor of 550ml is crossed to 0.22 μ m filter membrane, the ultra-filtration membrane bag that the speed of 300ml/min of take is afterwards 50,000 by molecular weight cut-off, seeing through the raw material that liquid further extracts as SOD enzyme is 490ml, trapped fluid is 50ml, loss 10ml.The ultra-filtration membrane bag that the speed molecular weight cut-off of 200ml/min of take is subsequently 5,000, trapped fluid is SOD enzyme concentrated solution, volume is 180ml.See through liquid 350ml.100% acetone of 4 ℃ of being cooled to that adds 180ml at the SOD of 180ml enzyme concentrated solution, and the mixed solution stirring is placed in-20 ℃ of refrigerator-freezers and is spent the night, then under 4 ℃ of conditions, centrifugal under 12000r/min speed, get precipitation part, with a small amount of washing with acetone three times, obtain the about 6.25ml of dense thick precipitation, the precipitation finally obtaining is that 45 ℃, resolution temperature are that 60 ℃ of frozen drying methods obtain the dry about 5.6g of SOD enzyme powder by operating pressure 50Pa, sublimation temperature.SOD enzyme lyophilized powder-20 ℃ that make save backup.
The liquid 350ml that sees through of the ultra-filtration membrane bag that the trapped fluid 50ml in D, the ultra-filtration membrane packet filtering that will be 50,000 at molecular weight cut-off and molecular weight cut-off are 5,000 merges, and the raw material of preserving as Sucus Chaenomelis series products at 4 ℃ is used.
E, the dehydrated alcohol of 1300ml will be added in 67g pomace, at 60 ℃ and be lixiviate 20 minutes under 59KHZ microwave-assisted by frequency, lixiviate finishes, 8 layers of hospital gauze that stack by 45 ° of intersections filter, get supernatant liquor and obtain the about 5.3g of Oleanolic Acid crude product after 60 ℃ of rotation method of enrichment are removed ethanol, to in the Oleanolic Acid crude product obtaining, add 50ml distilled water, carry out twice washing, after standing, suction filtration is got upper strata powder, carry out vacuum-drying Oleanolic Acid crude product powder, volatilization ethanol reclaims and reuses.Then add 50ml sherwood oil to carry out degreasing, rotary evaporation is removed sherwood oil, then add 50ml60 ℃ of hot dehydrated alcohol and add 50g gac to decolour, 60, filter rapidly to obtain clear liquid, clear liquid is carried out to low temperature crystallization and recrystallization, obtain Oleanolic Acid sterling, yield is about 1.63%, i.e. 1.09g.
F, the about 4g of precipitation filter residue producing during by the filter residue of about 61.7g in Oleanolic Acid leaching process and SOD enzyme thermally denature are dried in the lump, obtain approximately 13～16g of dry fruit slag, as animal-feed and animal-feed raw material, develop and utilize.
Above specific embodiments of the invention are described.It will be appreciated that, the present invention is not limited to above-mentioned specific implementations, and those skilled in the art can make various distortion or modification within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. Zou's skin pawpaw high utilization rate extracts and a working method, it is characterized in that, described method comprises the steps:
A, Zou's skin pawpaw are crushed to pasty state after mixing with water, and conventional filtration, carries out centrifugation to filtrate;
B, supernatant liquor filter through 0.22 μ m aperture filtering membrane;
C, filtered solution are 50,000 ultra-filtration membrane packet filterings through molecular weight cut-off;
D, filtered solution are 5,000 ultra-filtration membrane packet filterings through molecular weight cut-off;
E, trapped fluid carry out SOD enzyme precipitation by acetone method, and throw out, through frozen drying, obtains SOD enzyme;
F, the trapped fluid of the filtered solution of described 5,000 ultra-filtration membrane packet filterings and 50,000 ultra-filtration membrane packet filterings is merged, obtain pawpaw juice raw material;
G, the filter residue of described conventional filtration is carried out to dehydrated alcohol lixiviate, filtration under ultrasonic wave is auxiliary; Cleaner liquid is removed after ethanol to obtain Oleanolic Acid crude product, the residue animal-feed of drying, pulverize, sieve and to obtain.
2. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in steps A, it is that 30～50g is block that Zou's skin pawpaw fresh fruit is cut into weight, then mixes with the water of twice quality; After being crushed to pasty state, also comprise lixiviate 1h, the step stirring with the speed of 50～100 revs/min in leaching process.
3. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in steps A, described conventional filtration is specially: after 8 layers of hospital gauze that stack through 45 ° of intersections filter, obtain coarse filtration liquid, with quick filter paper, carry out decompress filter again, obtain crude enzyme liquid; Described centrifugation is specially: described crude enzyme liquid is heated rapidly to 60 ℃ and keep 20min, stops heating, static to after room temperature with the centrifugal 15min of 5000r/min speed.
4. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, step C carries out ultrafiltration with the speed of 300ml/min.
5. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, step D carries out ultrafiltration with the speed of 200ml/min.
6. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in step e, acetone is pre-chilled to 4 ℃, mixes to be placed in-20 ℃ of refrigerator-freezers to spend the night, with described trapped fluid then under 4 ℃ of conditions, centrifugal under 12000r/min speed, get precipitation part, then use washing with acetone three times, the precipitation finally obtaining is that 45 ℃, resolution temperature are that 60 ℃ of frozen drying methods obtain dry SOD enzyme powder by operating pressure 50Pa, sublimation temperature; The volume ratio of described trapped fluid and acetone is 1: 1.
7. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in step G, described dehydrated alcohol lixiviate is carried out under 60 ℃ of ultrasonic wave are auxiliary, and extraction time is 20min, and solid-liquid ratio is 1: 20.
8. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in step G, described removal ethanol is specially: by 60 ℃ of rotation method of enrichment, remove ethanol.
9. Zou's skin pawpaw high utilization rate as described in claim 1 or 8 extracts and working method, it is characterized in that, in step G, activated carbon decolorizing, the crystallizing process under low temperature that the Oleanolic Acid crude product obtaining after described removal ethanol is solvent through petroleum ether degreasing, the ethanol of take successively obtain Oleanolic Acid sterling.
10. Zou's skin pawpaw high utilization rate as claimed in claim 1 extracts and working method, it is characterized in that, in step G, described bake out temperature is 60 ℃; Described sieving as crossing 10～20 mesh sieves.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106721047A (en) * | 2016-11-25 | 2017-05-31 | 南宁学院 | A kind of method that edible fungi leftovers prepare multifunctional feed |
| CN109123046A (en) * | 2018-09-03 | 2019-01-04 | 吴建民 | A kind of SOD health sugar and preparation method thereof with adjusting total balance of the body |
| CN112058378A (en) * | 2020-08-24 | 2020-12-11 | 岳西县徽记农业开发有限公司 | Snakegourd peel juice microwave membrane separation and extraction equipment |
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| JP2006298812A (en) * | 2005-04-20 | 2006-11-02 | Mikimoto Pharmaceut Co Ltd | Antioxidant, skin lotion for anti-oxidization, elastase activity inhibitor and maillard reaction inhibitor |
| CN101962634A (en) * | 2010-09-15 | 2011-02-02 | 安徽农业大学 | Methods for extracting papain and superoxide dismutase (SOD) crude enzyme from comman floweringquince fruit |
| CN102229638A (en) * | 2011-04-26 | 2011-11-02 | 安徽农业大学 | Method for extracting oleanolic acid from chaenomeles fruit and preparing oleanolic acid standard |
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Patent Citations (3)
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| JP2006298812A (en) * | 2005-04-20 | 2006-11-02 | Mikimoto Pharmaceut Co Ltd | Antioxidant, skin lotion for anti-oxidization, elastase activity inhibitor and maillard reaction inhibitor |
| CN101962634A (en) * | 2010-09-15 | 2011-02-02 | 安徽农业大学 | Methods for extracting papain and superoxide dismutase (SOD) crude enzyme from comman floweringquince fruit |
| CN102229638A (en) * | 2011-04-26 | 2011-11-02 | 安徽农业大学 | Method for extracting oleanolic acid from chaenomeles fruit and preparing oleanolic acid standard |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106721047A (en) * | 2016-11-25 | 2017-05-31 | 南宁学院 | A kind of method that edible fungi leftovers prepare multifunctional feed |
| CN109123046A (en) * | 2018-09-03 | 2019-01-04 | 吴建民 | A kind of SOD health sugar and preparation method thereof with adjusting total balance of the body |
| CN112058378A (en) * | 2020-08-24 | 2020-12-11 | 岳西县徽记农业开发有限公司 | Snakegourd peel juice microwave membrane separation and extraction equipment |
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