CN104004048B - Cockle pawpaw high utilization rate extracts and working method - Google Patents
Cockle pawpaw high utilization rate extracts and working method Download PDFInfo
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Abstract
The invention discloses a kind of cockle pawpaw high utilization rate to extract and working method; Squeezed the juice after chopping by cockle pawpaw fresh fruit, the pawpaw magma after separation is used for extracting SOD enzyme and pawpaw juice, and remaining pericarp and pomace part are used for preparing Oleanolic Acid and animal-feed.In whole technological process of the present invention, utilize the various piece of cockle pawpaw as much as possible, 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 cockle pawpaw value provides technical support, simultaneously also for grower brings economic worth as much as possible, has very high promotional value and prospect.
Description
Technical field
The present invention relates to a kind of cockle pawpaw high utilization rate to extract and complete processing, belong to vegetables and fruits deep processing technology technique study 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.
The bioactive ingredients of multiple needed by human body is rich in, as organic acid, pentacyclic triterpene, flavonoid, saponins, phenols, superoxide-dismutase, volatile oil, vitamins, trace element etc. in cockle pawpaw.Wherein organic acid, flavonoid and superoxide-dismutase are because having higher medical and anti-oxidant activity, are worth larger.
In cockle pawpaw organic acid and tannin composition higher, and fruit texture is hard, fiber is more, vascular bundle is flourishing, mouthfeel is sour and astringent, should not directly eat, and therefore its processing technology seems particularly important in the utilization of cockle pawpaw.
The current processing for this cockle pawpaw is also in compares the primary stage, is mainly used as the exploitation of the aspects such as the prepared slices of Chinese crude drugs (being dried by direct slicing), Sucus Chaenomelis, papaya ester and pawpaw can.And directly abandoning that the materials such as a large amount of discarded pawpaw skins and slag are had, being used for of having is made compost or is dried as feed.And above simple processing is for containing this kind enriching organic acid, superoxide-dismutase, its utility value and utilization ratio just seem too low.
Summary of the invention
The object of the invention is to the deficiency overcoming the existence of above-mentioned prior art, provide a kind of cockle pawpaw high utilization rate to extract and working method.Method of the present invention is on the basis of existing extractive technique, carry out the combination of various extractive technique, optimization and lifting, by the qualification to cockle pawpaw effective constituent, formulate the technical matters route utilizing its various piece as much as possible, this technological line is by the least possible introducing organic solvent 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.The selected cockle pawpaw effective constituent/component extracted 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 cockle pawpaw high utilization rate to extract and working method, described method comprises the steps:
Be crushed to pasty state after A, cockle pawpaw mix with water, conventional filtration, centrifugation is carried out to filtrate;
B, supernatant liquor are through 0.22 μm of bore filter membrane filtration;
C, filtered solution are 50,000 ultra-filtration membrane packet filtering through molecular weight cut-off;
D, filtered solution are 5,000 ultra-filtration membrane packet filtering 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, by the filtered solution and 50 of described 5,000 ultra-filtration membrane packet filterings, the trapped fluid of 000 ultra-filtration membrane packet filtering merges, and obtains pawpaw juice raw material;
G, the throw out of the filter residue of described conventional filtration and centrifugation gained is carried out dehydrated alcohol lixiviate, filtration under ultrasonic assistant; Cleaner liquid obtains Oleanolic Acid crude product after removing ethanol, and residue is dried, pulverize, sieve to obtain animal-feed.
In above-mentioned steps, remove robust fibre by conventional filtration method; 0.22 μm of bore filter membrane filtration removal bacterium and macromolecular particle material, molecular weight cut-off are that part foreign protein is removed in 50,000 ultra-filtration membrane packet filtering, the ultrafiltration membrance filter bag of molecular weight cut-off 5,000 carries out filtration and removes 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 the product as much as possible simultaneously produced is to improve the use value of cockle pawpaw.The raw material that obtained SOD enzyme product can be further used as other products uses; In addition, because cockle pawpaw fresh fruit shreds and first supernatant liquor after carrying out conventional filtration adopted 0.22 μm of filter membrane, bacterium and macrobead thing are removed, and without any the introducing of solvent and other pollutents in ultra-filtration process afterwards, therefore, by described 5, the filtered solution and 50 of 000 ultra-filtration membrane packet filtering, the trapped fluid of 000 ultra-filtration membrane packet filtering merges in the environment of cleaning, and obtained pawpaw juice raw material 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 cockle pawpaw fresh fruit is cut into weight, then mixes with the water of twice quality; Also comprise lixiviate 1h after being crushed to pasty state, in leaching process, carry out the step stirred with the speed of 50 ~ 100 revs/min.The object of lixiviate is to urge the stripping into enzyme.
Preferably, described conventional filtration is specially: after 8 layers of hospital gauzes filtration that 45 ° of intersections stack, obtain coarse filtration liquid, then carry out decompress filter with fast grade filter paper, obtain crude enzyme liquid; Described centrifugation is specially: described crude enzyme liquid is heated rapidly to 60 DEG C and keeps 20min, stop heating, static after room temperature with 5000r/min centrifugation 15min.
Preferably, step C carries out ultrafiltration with the speed of 300ml/min.Ultrafiltration object is that removing molecular weight hands over large foreign protein, the raw material that permeate is extracted further as SOD enzyme, and trapped fluid is retained as the raw material of Sucus Chaenomelis liquid product, this step trapped fluid: permeate=1:9.
Preferably, step D carries out ultrafiltration with the speed of 200ml/min.Ultrafiltration object is removing small molecules inorganics and ion, and trapped fluid is SOD enzyme concentrated solution, and permeate gives over to Sucus Chaenomelis series products raw material, this step trapped fluid: permeate=2:1.
Preferably, in step e, acetone is pre-chilled to 4 DEG C, mix to be placed in-20 DEG C of refrigerator-freezers with described trapped fluid and spend the night, then under 4 DEG C of conditions, centrifugal under 12000r/min speed, get sediment fraction, use washing with acetone again three times, the precipitation finally obtained by operating pressure 50Pa, sublimation temperature be 45 DEG C, resolution temperature is that 60 DEG C of frozen drying methods obtain dry SOD enzyme powder; The volume ratio of described trapped fluid and acetone is 1:1.Obtained SOD enzyme lyophilized powder-20 DEG C saves backup.
Preferably, in step G, described dehydrated alcohol lixiviate is carried out under 60 DEG C of ultrasonic assistant, and extraction time is 20min, and solid-liquid ratio is 1:20.
Preferably, in step G, described removal ethanol is specially: remove ethanol by 60 DEG C of spin concentration methods.
Lixiviate terminates, and is filtered by material 8 layers of hospital gauze that 45 ° of intersections stack, obtains coarse filtration liquid, then carry out decompress filter by fast grade filter paper level, obtain clear liquor.Clear liquor adopts the means of rotary evaporation to remove ethanol, obtain brown viscous liquid, the distilled water adding weight of material 10 times subsequently carries out twice washing, solid-liquid separation is carried out by suction filtration after leaving standstill, get upper strata powder and be Oleanolic Acid crude product, subsequently operating pressure 50Pa, sublimation temperature be 55 DEG C, resolution temperature be 70 DEG C of conditions under vacuum-drying remove moisture further.The filter residue retained then can the raw material of animal-feed, its rich cellulose and polysaccharose substance.
Preferably, in step G, the Oleanolic Acid crude product obtained after described removal ethanol successively through petroleum ether degreasing, take ethanol as the activated carbon decolorizing of solvent, the crystallizing process under low temperature obtains Oleanolic Acid sterling.
Because Oleanolic Acid is insoluble in water, therefore it is mainly present among pomace and pericarp; The pericarp be trapped when carrying out conventional filtration after therefore the stripping and slicing of cockle pawpaw fresh fruit being pulverized and pomace part are using the raw material as extraction Oleanolic Acid, under 60 DEG C of ultrasonic assistant, lixiviate 20min is carried out as solvent by using harmless solvent dehydrated alcohol, then cross leaching supernatant fraction by ordinary method, then obtain Oleanolic Acid sterling after removing ethanol by 60 DEG C of spin concentration methods.Afterwards again by petroleum ether degreasing, take ethanol as the activated carbon decolorizing of solvent, the crystallizing process under low temperature obtains Oleanolic Acid sterling.This technical process leaching process adopts ethanol as solvent, and a large amount of residues of generation can be recycled, instead of becomes rubbish increase environmental pollution and burden.Petroleum ether degreasing, take ethanol as the activated carbon decolorizing of solvent, the crystallizing process under low temperature is specially: the crude product obtained is solvent again with sherwood oil, carries out degreasing with apparatus,Soxhlet's, and detect siphon pipe with obscure glass and flow out solvent and substantially do not have to stop during fat, degreasing completes.Under identical vacuum lyophilization condition, process obtains Oleanolic Acid powder subsequently.And then by a small amount of 100% dissolve with ethanol of the Oleanolic Acid crude product after degreasing, reflux, progressively adds ethanol and make hot saturated solution, after adding gac to boiling, 0.5h decolours.Then heat filtering is carried out and fast transfer filtrate, after filtrate cooling, crystallize out, and carry out recrystallization, obtain Oleanolic Acid sterling.
Preferably, in step G, described bake out temperature is 60 DEG C; Described sieve into cross 10 ~ 20 mesh sieves.
Because a large amount of residue produced in the filtration of lixiviate Oleanolic Acid is only containing alcohol solvent, and ethanol is a kind of harmless solvent, so residue can use as animal-feed raw material.Its processing process is: residue first carries out drying treatment at 60 DEG C, then dried filter residue pulverizer is carried out pulverizing again, 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 use, and also can use as the raw material of formula forage.
Compared with prior art, the present invention has following beneficial effect: the present invention, in whole technological process, considers the economic benefit of the cockle pawpaw of output in unit surface, ecological friendly and sustainable developability substantially.In art inventions, measured by the active substance of various experiment to cockle pawpaw various piece, formulate best testing program to reach the object that loss lowest energy obtains maximum useful output according to measurement result simultaneously.In described method steps A., cockle pawpaw+water carries out in crushing process, the usual way of prior art is add pH 7.8 and above phosphoric acid buffer to increase the activity of enzyme, but all liquid part after extraction enzyme and residue fraction can not be re-used as the exploitation raw material of fruit juice and animal-feed, while reducing its economic worth, white elephant is caused to environment.And purification phase concentrated at SOD enzyme simultaneously, present invention employs the mode of membrane filtration but not ammonium sulfate+acetone precipitation mode, a large amount of juices can be used as the raw material of Nakai beverage, on general economic value and in ecological friendly, be obtained for very large lifting.In the leaching process of Oleanolic Acid, consider that security and the cockle pawpaw of alcohol solvent contain abundant fiber and trace element, residue is form by being processed into animal-feed but not simply improves its economic use value further as land for growing field crops fertilizer.Therefore in the present invention in the various piece utilizing cockle pawpaw as much as possible, 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 cockle 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 done non-limiting example with reference to the following drawings, other features, objects and advantages of the present invention will become more obvious:
Fig. 1 is the schematic flow sheet of cockle pawpaw high utilization rate of the present invention extraction 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 and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment
The present embodiment relates to a kind of cockle pawpaw high utilization rate effective constituent/component and extracts and working method; Squeezed the juice after chopping by cockle pawpaw fresh fruit, the pawpaw magma after separation is used for extracting SOD enzyme and pawpaw juice, and remaining pericarp and pomace part are used for preparing Oleanolic Acid and animal-feed.Condition of storage after the harvesting of pawpaw fresh fruit is preserve in Cool Room 4 DEG C, and preservation period is 2-3 month.Total technological line as shown in Figure 1, specifically comprises the steps:
A, 200g pawpaw cleaned stripping and slicing (fruit piece size is 30 ~ 50g/ block), according to pawpaw: water=1:2 weight ratio adds tap water 400g, homogenate is carried out subsequently with stirrer, static 1 hour, then filter with 8 layers of hospital gauze that 45 ° of intersections stack, obtain coarse filtration liquid, then carry out decompress filter by fast grade filter paper level, obtain crude enzyme liquid stand-by.This process obtains pomace 67g.
B, gained crude enzyme liquid are heated to 60 DEG C and keep 20min to carry out thermally denature, and rear static to room temperature, then centrifugal 15min under the speed of 5000r/min, supernatant liquor extracts raw material further as SOD enzyme, and supernatant liquor constant volume is to 550ml.
C, the supernatant liquor of 550ml is crossed 0.22 μm of filter membrane, afterwards with the speed of 300ml/min by molecular weight cut-off for 50, the ultra-filtration membrane bag of 000, permeate is 490ml as the raw material that SOD enzyme extracts further, and trapped fluid is 50ml, loss 10ml.Subsequently with the speed molecular weight cut-off of 200ml/min for 5, the ultra-filtration membrane bag of 000, trapped fluid is SOD enzyme concentrated solution, and volume is 180ml.Permeate 350ml.100% acetone being cooled to 4 DEG C of 180ml is added at the SOD enzyme concentrated solution of 180ml, and the mixed solution stirred is placed in-20 DEG C of refrigerator-freezers spends the night, then under 4 DEG C of conditions, centrifugal under 12000r/min speed, get sediment fraction, with a small amount of washing with acetone three times, obtain dense thick precipitation about 6.25ml, the precipitation finally obtained by operating pressure 50Pa, sublimation temperature be 45 DEG C, resolution temperature is that 60 DEG C of frozen drying methods obtain dry SOD enzyme powder and are about 5.6g.Obtained SOD enzyme lyophilized powder-20 DEG C saves backup.
D, will merge at the permeate 350ml of molecular weight cut-off to be trapped fluid 50ml in the ultra-filtration membrane packet filtering of 50,000 and molecular weight cut-off the be ultra-filtration membrane bag of 5,000, the raw material preserved at 4 DEG C as Sucus Chaenomelis series products uses.
E, the dehydrated alcohol of 1300ml will be added in 67g pomace, lixiviate 20 minutes under being also 59KHZ microwave-assisted by frequency at 60 DEG C, lixiviate terminates, the 8 layers of hospital gauze stacked by 45 ° of intersections filter, get supernatant liquor after 60 DEG C of spin concentration methods remove ethanol, to obtain Oleanolic Acid crude product be about 5.3g, 50ml distilled water is added by the Oleanolic Acid crude product obtained, carry out twice washing, after leaving standstill, suction filtration gets upper strata powder, carry out vacuum-drying Oleanolic Acid crude powder, volatilization ethanol carries out recovery and reuses.Then add 50ml sherwood oil and carry out degreasing, rotary evaporation removes sherwood oil, then add 50ml60 DEG C of hot dehydrated alcohol and add 50g gac and decolour, clear liquid is obtained at 60 rapid filtration, clear liquid is carried out low temperature crystallization and recrystallization, obtain Oleanolic Acid sterling, yield is about 1.63%, i.e. 1.09g.
F, the precipitation filter residue produced is about 4g dries in the lump when the filter residue of about 61.7g in Oleanolic Acid leaching process and SOD enzyme thermally denature, obtain dry fruit slag about 13 ~ 16g, develop and utilize as animal-feed and animal-feed raw material.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. cockle pawpaw high utilization rate extracts and a working method, and it is characterized in that, described method comprises the steps:
Be crushed to pasty state after A, cockle pawpaw mix with water, conventional filtration, centrifugation is carried out to filtrate;
B, supernatant liquor are through 0.22 μm of bore filter membrane filtration;
C, filtered solution are 50,000 ultra-filtration membrane packet filtering through molecular weight cut-off;
D, filtered solution are 5,000 ultra-filtration membrane packet filtering 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, by the filtered solution and 50 of described 5,000 ultra-filtration membrane packet filterings, the trapped fluid of 000 ultra-filtration membrane packet filtering merges, and obtains pawpaw juice raw material;
G, the filter residue of described conventional filtration is carried out dehydrated alcohol lixiviate, filtration under ultrasonic assistant; Cleaner liquid obtains Oleanolic Acid crude product after removing ethanol, and residue is dried, pulverize, sieve to obtain animal-feed.
2. cockle 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 cockle pawpaw fresh fruit is cut into weight, then mixes with the water of twice quality; Also comprise lixiviate 1h after being crushed to pasty state, in leaching process, carry out the step stirred with the speed of 50 ~ 100 revs/min.
3. cockle 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 gauzes filtration that 45 ° of intersections stack, obtain coarse filtration liquid, carry out decompress filter with fast grade filter paper again, obtain crude enzyme liquid; Described centrifugation is specially: described crude enzyme liquid is heated rapidly to 60 DEG C and keeps 20min, stop heating, static after room temperature with 5000r/min centrifugation 15min.
4. cockle pawpaw high utilization rate as claimed in claim 1 extracts and working method, and it is characterized in that, step C carries out ultrafiltration with the speed of 300ml/min.
5. cockle pawpaw high utilization rate as claimed in claim 1 extracts and working method, and it is characterized in that, step D carries out ultrafiltration with the speed of 200ml/min.
6. cockle 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 DEG C, mixes to be placed in-20 DEG C of refrigerator-freezers spend the night, then under 4 DEG C of conditions with described trapped fluid, centrifugal under 12000r/min speed, get sediment fraction, then use washing with acetone three times, the precipitation finally obtained by operating pressure 50Pa, sublimation temperature be 45 DEG C, resolution temperature is that 60 DEG C of frozen drying methods obtain dry SOD enzyme powder; The volume ratio of described trapped fluid and acetone is 1:1.
7. cockle pawpaw high utilization rate as claimed in claim 1 extracts and working method, and it is characterized in that, in step G, described dehydrated alcohol lixiviate is carried out under 60 DEG C of ultrasonic assistant, and extraction time is 20min, and solid-liquid ratio is 1:20.
8. cockle pawpaw high utilization rate as claimed in claim 1 extracts and working method, and it is characterized in that, in step G, described removal ethanol is specially: remove ethanol by 60 DEG C of spin concentration methods.
9. the cockle pawpaw high utilization rate as described in claim 1 or 8 extracts and working method, it is characterized in that, in step G, the Oleanolic Acid crude product obtained after described removal ethanol successively through petroleum ether degreasing, take ethanol as the activated carbon decolorizing of solvent, the crystallizing process under low temperature obtains Oleanolic Acid sterling.
10. cockle pawpaw high utilization rate as claimed in claim 1 extracts and working method, and it is characterized in that, in step G, described bake out temperature is 60 DEG C; Described sieve into cross 10 ~ 20 mesh sieves.
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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 |
| CN112058378B (en) * | 2020-08-24 | 2021-11-26 | 安徽省徽岳记食品有限公司 | Snakegourd peel juice microwave membrane separation and extraction equipment |
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| 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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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
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| 宣木瓜叶中生物活性物质的定性鉴别及提取工艺;丁之恩等;《经济林研究》;20110630;第29卷(第2期);8-13 * |
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