CN1826949A - Novel method for preparing pectin by soybean seed coat - Google Patents
Novel method for preparing pectin by soybean seed coat Download PDFInfo
- Publication number
- CN1826949A CN1826949A CNA2005101044578A CN200510104457A CN1826949A CN 1826949 A CN1826949 A CN 1826949A CN A2005101044578 A CNA2005101044578 A CN A2005101044578A CN 200510104457 A CN200510104457 A CN 200510104457A CN 1826949 A CN1826949 A CN 1826949A
- Authority
- CN
- China
- Prior art keywords
- pectin
- seed coat
- soybean seed
- solvent
- value
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention relates to a method for preparing pectin, especially to a method taking soybean seed coat as essential raw material and extracting pectin through further process. The process comprise: (1) pretreating raw material: cleaning soybean seed coat, and washing it; (2) extracting pectin: extracting with complexing agent for one time and two times; (3) decolorizing: with activated carbon and cold-soda; (4) depositing pectin: regulating pH value to 1.5-3.5 with inorganic acid of 6 mol/l; (5)solid and liquid separation: deacidifying with filter-pressing; (6) solvent treating: employing solvent which pectin can not dissolve in but water can, to make the pectin deposit from condensing liquor, or extracting pectin by direct spraying extract; (7) recovering deposit: employing suction method and further washing with solvent; (8) getting product: drying and disintegrating. The invention is characterized in that: (1) the cost of raw material is low; (2) the pectin gpt from soybean seed coat will be new pectin besides the traditional pectin.
Description
One, technical field: the present invention relates to a kind of preparation pectin method, especially is primary raw material with the soybean peel, extracts the new method of pectin by deep processing.
Two, background technology: the major product of soybean processing industry is soya-bean oil and various soybean protein both at home and abroad at present.In the soybean processing process, at first to peel, take off selected and sorting preprocessings such as plumule, with quality and the yield of guaranteeing soya-bean oil and various soybean proteins.Soybean peel is the accessory substance of the amount maximum that produces in the soybean deep-processing process, accounts for 8～10% of soybean weight.Soybean peel nutritive value lower (crude protein content 11%, crude fiber content 36%, crude fat content 1%), be difficult for absorbing for animal digestion, add and contain a large amount of ANFs---phytic acid, even reluctantly as the feed of ruminants such as ox, sheep, value is not high yet.Pectin has good gelatification, emulsification, suction-operated, is widely used in fields such as the production of food, medicine, cosmetics and water treatment.
At present, the raw material that extract pectin both at home and abroad mainly are materials such as oranges and tangerines skin, pomace, megasse, the extraction process of pectin mainly is to utilize dilute acid soln that protopectin is hydrolyzed to water soluble pectin matter and transfers to aqueous phase, utilizes pectin to be insoluble to ethanol, acetone etc. and water miscible organic solvent again or produces the flocculation precipitating and extract when some ionizable metal salts exist.Its technological process is: pretreatment of raw material → acid solution hydrolysis → filtration → decolouring → de-ash → concentrate → precipitating → drying → pulverizing → standardization → finished product.Key in the process for producing pectin is extraction and separates two steps.
In recent years, abroad begin with the soybean peel is the research and development that raw material begins to extract pectin, the method of representative preparing pectin by soybean seed coat is: (1) pretreatment of raw material: soybean peel (through sieving and selection by winnowing) is a raw material, stirred 1 hour with 12 times of water of skin of beancurd weight, through flotation and washing, inclining showy part, uses after drip washing drains, with impurity such as removal silts.(2) soybean peel hydrolysis: take the acid heat hydrolysis, once extract the extracted twice method of putting forward with slag.Inorganic acid concentration represents that with mole with the solution dilution of 6 mol concentration, under the acidometer monitoring, fine adjustment stirs hydrolysis and lixiviate certain hour to specified pH value under certain bath raio again; And the variation of monitoring pH value in insulation reaction is extracted.(3) neutralization: the NaOH solution with 4 mol is adjusted the pH value, reduces acidity, in order to avoid remain in strong acidic environment for a long time, causes excessive hydrolysis, influences pectin yield and product quality.(4) Separation of Solid and Liquid: adopt suction method, carry out in Buchner funnel, vavuum pump provides negative pressure.(5) decolouring: active carbon adsorption decolouring.Solution is preheating to 82 ℃, and pH is transferred to 2.5, and 2～5% (weight per volume) of pressing solution add activated carbon, stirs insulation down and handles suction filtration deactivation carbon in the Buchner funnel 30 minutes.(6) concentrate: carried out normal pressure, decompression (65 ℃) and ultrafiltration respectively and concentrated.(7) solvent deposition: solvent deposition is one of method of effectively isolating pectin substance, and with methyl alcohol, ethanol and acetone, flocculation and effect of settling are similar.(8) recycling precipitate: adopt suction method, again through hydrous ethanol drip washing, dense ethanol dehydration impurity elimination.(9) product obtains: precipitation, crushed after being dried, cross 100 mesh standard sieves.It is the technical feasibility that raw material extracts pectin that this method has solved soybean peel from theory, but exists output efficiency low in the actual application, the problem that technique controlling difficulty is high.
Three, summary of the invention: purpose of the present invention is exactly the defective that exists at prior art, and a kind of novel method for preparing pectin by soybean seed coat is provided.This method is extracted pectin according to being to contain in the soybean peel with calcium ions and magnesium ions etc. to be the pectin substance of bonding state, thereby can not be water-soluble.Utilize complexing agent to compete and combine, make with the pectin of calcium ions and magnesium ions bonding state freely, become water-soluble state, thereby make pectin enter extract to reach the purpose of extracting pectin with calcium ions and magnesium ions.
Its technical scheme comprises:
(1) preparation of raw material and preliminary treatment: soybean peel need add 10-20 times of normal-temperature water through after selected, the impurity elimination, adjusts pH value to 11, stirs 20-40 minute water washing cleaning.
(2) soy pectin extracts: take network and agent once to extract method with extracted twice.The complexing agent consumption is 0.5%-2.0% by the concentration that is made into certain solution, and pH value 7.5-11.0 stirred 50-70 minute, and monitors the variation of pH value under 65 ℃～95 ℃ conditions of temperature.
(3) extracting liquid decoloration: active carbon adsorption decolouring and two kinds of methods of cold alkali aggregate expansion.
(4) pectin precipitation: adjust pH 1.5～4.5, heavy 15-25 minute of acid.
(5) Separation of Solid and Liquid: adopt filter press technique deacidification water.
(6) pickling after the press filtration: under pH value 1.5～4.5 conditions, pickling 10-25 minute.
(7) alcohol/ammonia solution washing: adopt concentration 40-60% organic alcohol solvent with pectin separate broken after, with ammoniacal liquor adjust pH 8.0-9.0, handled 30 minutes;
(8) sediment separate out reclaims: solvent is handled the pectin of gained and is used 60%, 70% and 95～98% aqueous solvent drip washing successively;
(9) product obtains: precipitation, crushed after being dried.
Extract the used complexing agent of soy pectin and comprise calgon, EDTA; The selection of organic alcohol solvent comprises several solvents such as methyl alcohol, ethanol (absolute ethyl alcohol and industrial alcohol), propyl alcohol, isopropyl alcohol, acetone, is advisable with food grade ethanol.
On the basis of such scheme, compare Journal of Sex Research and experiment with regard to the relevant technologies parameter, the following raising and the recovery rate and the product quality concrete measure that improve product proposed.
1, cleaning is to the influence of pectin quality.Cleaning helps improving the quality of products, and can effectively improve product color, reduces ash.
2, the skin of beancurd granularity is to the influence of pectin yield.Taking all factors into consideration the each side factor adopts the soybean peel raw material of not pulverizing directly to use.
3. extract of the influence of the used complexing agent kind of soy pectin: adopt multiple complexing agents such as calgon, EDTA to combine respectively with calcium, magnesium ion in the soybean peel to yield and product quality.Take all factors into consideration factor EDTA such as environmental protection, price, source, effect and certain advantage is arranged as complexing agent.Find also in the experiment that the pH value of suitably regulating extract can make the extraction yield increase.
In the extract complexing agent concentration to the influence of yield: network and agent solution with variable concentrations extract soy pectin, found that complexing agent concentration is lower than 0.2% in the solution, DeGrain, yield is on the low side, the complexing agent concentration height, yield is steady, but that concentration is higher than is 0.8% no longer in rising trend.
5. extract the influence of temperature: carried out 15 ℃ of room temperatures, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 95 ℃, 100 ℃ extraction pectin experiments down respectively to pectin yield, found that: temperature is low, yield is low, but be not the temperature height, yield is just corresponding high, 80 ℃～90 ℃ are extracted down, recovery rate is similar, and the yield of extracting under the condition more than 95 ℃ descends again on the contrary to some extent, and the pectin viscosity in aqueous solution of allotting also decreases.May be that the pectin that causes lixiviate to go out under stronger heat condition is further degraded, molecule diminishes, and is difficult to sedimentation.
6. bath raio is to the influence of pectin yield and product quality: other condition is fixed, extract experiment by 5: 1,10: 1,15: 1,20: 1,25: 1 condition of bath raio, found that: bath raio is 5: 1 o'clock, can not soak soybean peel fully, bath raio is 10: 1 above could immersions fully; It is low that bath raio is crossed low yield, the solvent deposition thing be cotton-shaped and thread, the too high yield of bath raio is also lower, and the viscosity of gained pectin solution is poor slightly.8: 1,15: 1 of more suitable bath raioes further relatively, the result with 10: 1～12: 1 for the suitableeest.
7. extraction time is to the influence of pectin yield: other condition is fixed, and extraction time is a variable, does series of experiments.The result is: the time is too short, and hydrolyzed pectin and lixiviate in the soybean peel are incomplete, and yield is obviously on the low side.Overlong time, the pectin in the skin of beancurd excessively is hydrolyzed into little molecule, add solvent after, be difficult to precipitation, yield also decreases, and the water-soluble viscosity of gained pectin is relatively poor.Extraction time conforms to trend with the result who extracts test with acid system with the relation of pectin yield.In 60 minutes, along with the increase of time, yield rises, and is advisable time expand (90 minutes) yield slightly decline on the contrary again with 60 minutes.
8. the relation of sour heavy pH value and pectin yield: other condition is fixed, and the heavy pH value of acid is a variable, does series of experiments.The result is: the heavy pH value of acid is low excessively, and the pectin precipitation in the soybean peel extract is incomplete, and pectin substance is all with fluid loss, and yield is obviously on the low side.With pH value 1.5～4.5 is good.
9. the relation of pickling pH value and pectin yield: get the acid of the isodose pectin after heavy, clean with the sour water of different pH values, comparison cleaning performance discovery pH is too high, and to have part pectin water-soluble, causes yield on the low side; PH is low excessively, and is unfavorable to equipment and technology.To clean better with the similar acidifying water of the heavy pH value of acid.
10. with the selection of the mixable organic solvent of water: pectin is insoluble to ethanol etc. and the mixable organic solvent of water.Relatively cross several solvents such as methyl alcohol, ethanol (absolute ethyl alcohol and industrial alcohol), propyl alcohol, isopropyl alcohol, acetone in the test, find that the sedimentation effect difference is little.Consider source, price, the difficulty or ease of recovery and the composite factors such as specification requirement that are used for the additive of food of toxicity, propyl alcohol and the isopropyl alcohol of methyl alcohol, still select for use the food grade ethanol of fermentation method production to be advisable.
According to the new extraction conditions that the laboratory is optimized, adopt the new technology route after improving to carry out amplification and repeated test, it is as shown in the table that continuous 7 crowdes of EDTA extract pectin method setting-out result of the test:
Annotate: all batches test is only through once extracting, if can reach 14～15% through pectin yield after the second extraction.
| Batch | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Sample heavy (gram) | 200 | 200 | 400 | 400 | 400 | 400 | 400 |
| Pectin heavy (gram) | 22.375 | 23.087 | 47.048 | 44.091 | 46.016 | 44.16 | 47.03 |
| Yield (%) | 11.19 | 11.54 | 11.76 | 11.02 | 11.50 | 11.04 | 11.76 |
The present invention extracts pectin and compares with the conventional method of extracting pectin from materials such as oranges and tangerines skin, pomace, megasse from soybean peel, have following advantage at least: (1), soybean peel are as the byproduct of soybean processing enterprise, and low price is collected easily; (2), soybean peel does not need further to process just can to store and transport; (3), the development trend of prediction low sugar, healthy food low in calories and functional food and the increase of the market demand, the natural low-ester pectin that obtains in the soybean peel (calcium gelation) will become traditional pectin (high-ester pectins such as citrus pectin, apple pectin, high sugared gelation) pectin new varieties in addition.Prove through laboratory and pilot experiment that from technical scheme of the present invention extraction and separating technology are rationally ripe more, have good application prospects.
Four, description of drawings: accompanying drawing is a process chart of the present invention.
Five, specific embodiment:
With reference to accompanying drawing, specific embodiments of the present invention comprises:
(1) preparation of raw material and preliminary treatment: soybean peel need add 15 times of normal-temperature water through after selected, the impurity elimination, adjusts pH value to 11, stirs 30 minutes water washing cleanings.
(2) soy pectin extracts: take network and agent once to extract method with extracted twice.Complexing agent is 1.0% with calgon or EDTA by the concentration that is made into certain solution, and pH value 9.5 stirred 60 minutes, and monitors the variation of pH value under 85 ℃ of conditions of temperature.
(3) extracting liquid decoloration: active carbon adsorption decolouring and two kinds of methods of cold alkali aggregate expansion.
(4) pectin precipitation: adjust pH 2.5, heavy 20 minutes of acid.
(5) Separation of Solid and Liquid: adopt filter press technique deacidification water.
(6) pickling after the press filtration: under pH value 2.5 conditions, pickling 15 minutes.
(7) carry out alcohol/ammonia solution washing after the press filtration once more: adopt concentration 50% alcohol solvent with the pectin post precipitation,, handled 30 minutes with ammoniacal liquor adjust pH 8.5;
(8) sediment separate out reclaims: the pectin of solvent deposition gained is used 60%, 70% and 95% aqueous solvent drip washing successively;
(9) product of Fen Liing obtains finished product after screw extrusion, drying, pulverizing, packing.
Claims (3)
1, a kind of novel method for preparing pectin by soybean seed coat is characterized in that comprising:
(1) preparation of raw material and preliminary treatment: soybean peel need add 10-20 times of normal-temperature water through after selected, the impurity elimination, adjusts pH value to 11, stirs 20-40 minute water washing cleaning;
(2) soy pectin extracts: take network and agent once to extract method with extracted twice; The complexing agent consumption is 0.5%-2.0% by the concentration that is made into certain solution, and pH value 7.5-11.0 stirred 40-70 minute, and monitors the variation of pH value under 65 ℃～95 ℃ conditions of temperature;
(3) Separation of Solid and Liquid: adopt suction method deacidification water;
(4) extracting liquid decoloration: active carbon adsorption decolouring and two kinds of methods of cold alkali aggregate expansion;
(5) pectin precipitation: adjust pH 1.5～3.5, heavy 15-25 minute of acid;
(6) pickling after the press filtration: under pH value 1.5～3.5 conditions, pickling 10-25 minute;
(7) alcohol/ammonia solution washing: adopt concentration 40-60% organic alcohol solvent with the pectin post precipitation, with ammoniacal liquor adjust pH 8.0-9.0,30 minutes time;
(8) sediment separate out reclaims: the pectin of solvent deposition gained is used 60%, 70% and 95～98% aqueous solvent drip washing successively;
(9) product obtains: precipitation, crushed after being dried.
2, novel method for preparing pectin by soybean seed coat according to claim 1 is characterized in that: extract the used complexing agent of soy pectin and comprise calgon, EDTA; The selection of organic alcohol solvent comprises several solvents such as methyl alcohol, ethanol, propyl alcohol, isopropyl alcohol, acetone.
3, novel method for preparing pectin by soybean seed coat according to claim 2 is characterized in that: the selection of organic alcohol solvent is advisable with food grade ethanol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101044578A CN100508781C (en) | 2005-10-25 | 2005-10-25 | Novel method for preparing pectin by soybean seed coat |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101044578A CN100508781C (en) | 2005-10-25 | 2005-10-25 | Novel method for preparing pectin by soybean seed coat |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1826949A true CN1826949A (en) | 2006-09-06 |
| CN100508781C CN100508781C (en) | 2009-07-08 |
Family
ID=36945648
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005101044578A Active CN100508781C (en) | 2005-10-25 | 2005-10-25 | Novel method for preparing pectin by soybean seed coat |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100508781C (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224573A (en) * | 2013-04-24 | 2013-07-31 | 上海交通大学 | Method for extracting pectin from skin of beancurd |
| CN105192504A (en) * | 2015-09-28 | 2015-12-30 | 渤海大学 | Method for manufacturing flat apricot jam by aid of soybean coat pectin used as gel |
| CN106317252A (en) * | 2016-08-22 | 2017-01-11 | 邵玉华 | Method for extracting pectin polysaccharides from soybean hulls |
| CN114947111A (en) * | 2022-07-16 | 2022-08-30 | 广东欧帝玛生物工程有限公司 | Method for preparing food gum by mixing soybean hulls and fish scales |
-
2005
- 2005-10-25 CN CNB2005101044578A patent/CN100508781C/en active Active
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103224573A (en) * | 2013-04-24 | 2013-07-31 | 上海交通大学 | Method for extracting pectin from skin of beancurd |
| CN103224573B (en) * | 2013-04-24 | 2016-01-13 | 上海交通大学 | The method of pectin is extracted in skin of beancurd |
| CN105192504A (en) * | 2015-09-28 | 2015-12-30 | 渤海大学 | Method for manufacturing flat apricot jam by aid of soybean coat pectin used as gel |
| CN105192504B (en) * | 2015-09-28 | 2019-01-25 | 渤海大学 | Using soybean peel pectin as the preparation method of the flat apricot jam of gelling agent |
| CN106317252A (en) * | 2016-08-22 | 2017-01-11 | 邵玉华 | Method for extracting pectin polysaccharides from soybean hulls |
| CN114947111A (en) * | 2022-07-16 | 2022-08-30 | 广东欧帝玛生物工程有限公司 | Method for preparing food gum by mixing soybean hulls and fish scales |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100508781C (en) | 2009-07-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP2209816B1 (en) | Process for the preparation of purified beta-(1,3)-d-glucans | |
| CN101851300B (en) | Process for extracting chondroitin sulfate | |
| CN100422217C (en) | Process for preparing pectin and heavy metallic ion adsorber by soybean peel combined production | |
| CN111793145A (en) | Process for improving quality and yield of sodium chondroitin sulfate co-produced collagen peptide | |
| CN101037485A (en) | Pectin extraction method | |
| CN103613220B (en) | A kind of method of extracting several functions component from wheaten starch processing waste water | |
| CN100508781C (en) | Novel method for preparing pectin by soybean seed coat | |
| CN102492054B (en) | Preparation method of soybean episperm pectin gel polysaccharide | |
| CN105394520A (en) | Method for removing cadmium in whole rice | |
| CN105661267B (en) | Heavy metal reduction method for grains | |
| CN1827773A (en) | Process for preparing bacteriostatic peptide by discarded tobacco leaf protein | |
| CN1957736A (en) | Method for producing soyabean protein (peptide) powder with NSI value equal to 100% | |
| CN113621444A (en) | Preparation method and application of rhamnolipid composite surfactant | |
| CN105463040A (en) | Method for raising yield of xylooligosaccharide | |
| CN1277486C (en) | Modification method of soybean protein concentrate | |
| CN1266160C (en) | Process for extracting rubusoside of fruit of Gorsvenor Momordica | |
| CN106008744A (en) | Method for preparing pectin from pomegranate peel residues and pectin prepared with method | |
| CN1837234A (en) | Process for preparing low phytic acid rapeseed protein concentrate by using water and ethanol | |
| CN1410542A (en) | Method of preparing chitin oligosaccharide by coupled enzymolysis and its equipment | |
| CN106636269A (en) | Method for efficient extraction of active protein | |
| CN106478827B (en) | A kind of processing method of the improved Artemisia Glue emulsifier of enzyme process | |
| CN1219068C (en) | Continuous single-tank fermentation process of bacillus in membrane coupled clear liquid for producing levolactic acid | |
| CN214183017U (en) | One set of device of preparation acid type sophorolipid | |
| CN1919062A (en) | Method for extracting series effective ingredient of pyracantha | |
| CN111808904B (en) | Preparation method for extracting hydrolyzed protein from whey waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Novel method for preparing pectin by soybean seed coat Effective date of registration: 20121018 Granted publication date: 20090708 Pledgee: Hengfeng bank, Limited by Share Ltd, Dongying branch Pledgor: Shandong Wonderful Industrial Group Co., Ltd. Registration number: 2012990000611 |
|
| PLDC | Enforcement, change and cancellation of contracts on pledge of patent right or utility model | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20171113 Granted publication date: 20090708 Pledgee: Hengfeng bank, Limited by Share Ltd, Dongying branch Pledgor: Shandong Wonderful Industrial Group Co., Ltd. Registration number: 2012990000611 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right |