CN102492054B - Preparation method of soybean episperm pectin gel polysaccharide - Google Patents
Preparation method of soybean episperm pectin gel polysaccharide Download PDFInfo
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Abstract
The invention relates to a preparation method of soybean episperm pectin gel polysaccharide. The preparation method comprises the following specific steps of: firstly crushing soybean episperm, soaking and persistently stirring the soybean episperm with low concentration ethanol, filtering, recovering ethanol and drying retentate under reduced pressure; and adding ammonium oxalate or a component A to dried soybean episperm powder, carrying out microwave-assisted extraction, carrying out conventional filtering on the material liquid after microwave treatment to obtain filtrate, removing fine impurities by a microfiltration method, carrying out ultrafiltration and concentration on the obtained filtrate, and spray-drying the concentrated material liquid by an atomizer to obtain soybean episperm pectin polysaccharide solid powder, wherein the component A is a mixed solution of ammonium sulfate and a component B, and the component B is oxalic acid or EDTA (ethylene diamine tetraacetic acid) or citric acid. The method is low in production cost and high in extraction rate; and the prepared product solution is low in color value, has unique gel characteristics and can be widely applied to food industry.
Description
Technical field
The invention belongs to the soybean peel deep processing method as food ingredients, additive, particularly a kind of preparation method of soybean peel pectin gellike polysaccharide.
Background technology
Pectin class polysaccharide is the most complicated a kind of of structure in the plant cell wall polysaccharides class family, has multiple physiological functions such as good gelling, emulsifying property, is a kind of important foodstuff additive, also has widely at chemical industry and field of medicaments simultaneously and uses.The raw material of producing pectin at present mainly comprises: the skin slag of citrus, apple, watermelon, pawpaw, pumpkin and orange class, Sunflower Receptacle pallet and stalk, beet pulp etc.In soybean deep processing industry, in order to improve protein and oil quality, manufacturing enterprise generally removes soybean peel earlier, the oil of squeezing system again and preparation soybean protein isolate.Because the nutritive value of soybean peel is lower and contain antinutritional factor, cause utility value not high, so the technological development of high value added utilization soybean peel receives much concern.
As having proposed " novel method for preparing pectin by soybean seed coat " among the document 1:CN200510104457.8, its technical scheme is: soybean peel is through selected, impurity elimination and water washing cleaning, take network and agent once to extract method with extracted twice, utilize two kinds of method decolourings of activated carbon adsorption decolouring and cold alkali aggregate expansion, heavy with acid behind the mineral acid adjust pH, utilize filter press technique deacidification water, adopt pectin to be insoluble to itself and the mixable organic solvent of water, with this class organic solvent its washing of precipitate in the concentrated solution is come out, also available direct spraying drying extracting solution reclaims pectin, adopt suction method and further eluent solvent dehydration impurity elimination, precipitation, crushed after being dried.
As having proposed " the soybean peel coproduction prepares the method for pectin and adsorbent for heavy metal " among the document 2:CN200510104458.2, its pectin technology of preparing scheme is identical with document 1.
And for example proposed among the document 3:CN201010293751.9 " a kind of preparation method of soybean peel water-soluble dietary fibre ", its technical scheme is: earlier soybean hulls is pulverized, the soybean hulls of learning from else's experience and pulverizing, add water, stir, insulation, after being down to room temperature, carry out centrifugation, remove sediment, collect filtrate; Adding hydrogen peroxide in gained filtrate decolours; The solution that will add behind the heat decoloring adds cellulase solution, and centrifugation is carried out in insulation, removes filter residue, collects filtrate; Gained contains soybean hulls water-soluble dietary fibre filtrate, and heating concentrates, and in concentrated solution, adds alcohol, and precipitation is carried out centrifugally, obtains wet soybean hulls water-soluble dietary fibre, and lyophilize is pulverized then, makes water-soluble dietary fibre.
Above-mentioned document 1 and document 2 adopt network and agent once to extract and the extracted twice pectin polysaccharide, and the pectin extraction yield is about 13%, utilize activated carbon adsorption decolouring and cold alkali aggregate expansion, the decoloring method complexity, and activated carbon has residual, and the retention rate of polysaccharide is low; As pectin class polysaccharide typical characteristics-gelling, abide by national standard, galacturonic acid content must surpass 65% in the pectin, and the galacturonic acid content in the current soybean peel polysaccharide does not reach this standard as yet, judges that institute's polysaccharide that extracts is that " pectin " is inappropriate.Document 3 adopts the chemical process decolouring, and residual hydrogen dioxide has toxic action, should not promote.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of soybean peel pectin gellike polysaccharide, this method polysaccharide extract rate height, and the colour of the product solution that makes is low, can be used as food ingredients.
Technical solution of the present invention is:
A kind of preparation method of soybean peel pectin gellike polysaccharide, its concrete steps are as follows:
1.1 pulverize
Milling soya seeds kind skin was collected the pressed powder of 40～60 mesh sieves;
1.2 ethanol decolorization pre-treatment
Take by weighing the soybean peel powder after a certain amount of pulverizing, adding massfraction is 0.5～2% ethanolic soln, and the solid-liquid ratio of soybean peel powder and ethanolic soln is 50～200g/1L, stirring at room is handled 30～100min, filter then, ethanol reclaims, the filter residue drying under reduced pressure;
1.3 microwave auxiliary extraction
With the soybean peel powder after the Ethanol Treatment, add ammonium oxalate solution or component A, the solid-liquid ratio of soybean peel powder after the processing and ammonium oxalate solution or component A is 40～100g/1L, microwave treatment, microwave power is 200～400W, temperature remains on 85～98 ℃, the microwave action time is at 10～100min, the massfraction of described ammonium oxalate solution is 0.2～5%, component A is the mixing solutions of ammonium sulfate and B component, B component is oxalic acid or EDTA or citric acid, and the mass ratio of ammonium sulfate and B component is 1:1;
1.4 membrane sepn
Feed liquid after microwave treatment is filtered to get filtrate, filtrate is used the removal of impurities of millipore filtration micro-filtration, use the polysulphones hyperfiltration membrane ultrafiltration and concentration to 5～20% of original volume then, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 1～10cm/s, working pressure is 0.01～0.1MPa, and temperature is 20～80 ℃;
1.5 spraying drying
Adopt centrifugal spray-dryer or press spray moisture eliminator, to the filtrate spraying drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 160～220 ℃, and air outlet temperature is controlled at 70～90 ℃, namely makes soybean peel pectin gellike polysaccharide.
The preparation method of above-mentioned soybean peel pectin gellike polysaccharide, described soybean peel is the soybean peel through the drying of wet method or dry removal.
The preparation method of above-mentioned soybean peel pectin gellike polysaccharide, the solid-liquid ratio of soybean peel powder and ethanolic soln is 67～100g/1L.
The preparation method of above-mentioned soybean peel pectin gellike polysaccharide, the solid-liquid ratio of the soybean peel powder after the Ethanol Treatment and ammonium oxalate solution or component A is 50～67g/1L.
The preparation method of above-mentioned soybean peel pectin gellike polysaccharide, microwave power is 300～350W, and temperature remains on 95～98 ℃, and the microwave action time is at 60～90min.
The preparation method of above-mentioned soybean peel pectin gellike polysaccharide, cross-flow velocity is 2～6cm/s, and working pressure is 0.08～0.1MPa, and temperature is 60～80 ℃.
The present invention has following beneficial effect:
1, to utilize massfraction be 0.5%～2% ethanolic soln to the pre-treatment of decolouring of soybean peel powder, not only can remove pigment, and good decolorizing effect can be removed part monose, oligose, phenols micromolecular compound and heteroproteins simultaneously;
2, adopt the auxiliary extraction yield that can improve polysaccharide of microwave method, make polysaccharide extract rate reach 15～20%; And micro-wave energy impels the amidate action of ammonium oxalate and pectin molecule, makes polysaccharide have excellent gelling properties;
3, the polysaccharide of Ti Quing all can form gel under divalent cation, monovalent cation or acidic conditions, has unique gel property, and difference is mechanical behavior and the swelling behavior of gel;
4, utilize membrane separating method to prepare the polysaccharide finished product in conjunction with spray drying technology, membrane sepn has molecular level separation, no phase transformation, solvent-free pollution, keeps the activity of biomolecules, excellent characteristics such as operation is simple and reliable easily, save heating and concentrated the energy that needs, reduce consumption of organic solvent, and the drying products good fluidity does not need drying products is pulverized again.
Description of drawings
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the chromatography of ions figure of monose in the soybean peel pectin class polysaccharide that makes of the present invention;
Among the figure: 1-Fucose, 2-rhamnosyl, 3-pectinose, 4-galn, 5-semi-lactosi, 6-glucose, 7-wood sugar, 8-galacturonic acid, 9-glucuronic acid.
Embodiment
Embodiment 1
As shown in Figure 1, it is as follows to prepare the method for soybean peel pectin gellike polysaccharide:
Utilize the Universalpulverizer pulverizing through the soybean peel of the drying of dry removal, collected the pressed powder of 40 mesh sieves; Take by weighing the soybean peel powder 50g after the pulverizing, add massfraction and be 0.5% ethanolic soln 1L, stirring at room is handled 30min, filters then, and ethanol reclaims, the filter residue drying under reduced pressure; Take by weighing soybean peel powder 40g dry after the Ethanol Treatment, add massfraction and be 0.2% ammonium oxalate solution 1L, carry out microwave treatment, microwave power is 200W, and temperature remains on 85 ℃, and microwave treatment time is 10min; Filter to get filtrate, with the removal of impurities of millipore filtration micro-filtration, use polysulfones micropore ultra-filtration membrane ultrafiltration and concentration to 20% of original volume then gained filtrate, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 1cm/s, and working pressure is 0.01MPa, and temperature is 20 ℃; Adopt centrifugal spray-dryer to the liquid spray drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 160 ℃, and air outlet temperature is controlled at 70 ℃, makes pulverous soybean peel pectin gellike polysaccharide, and polysaccharide extract rate is 15.23%.
Utilize Universalpulverizer to pulverize the soybean peel of the drying that removes through wet method, collected the pressed powder of 50 mesh sieves; Take by weighing the soybean peel powder 67g after the pulverizing, add massfraction and be 1% ethanolic soln 1L, stirring at room is handled 50min, filters then, and ethanol reclaims, the filter residue drying under reduced pressure; Take by weighing soybean peel powder 50g dry after the Ethanol Treatment, add massfraction and be 1.6% ammonium oxalate solution 1L, carry out microwave treatment, microwave power is 300W, and temperature remains on 95 ℃, and microwave treatment time is 60min; Filter to get filtrate, with the removal of impurities of millipore filtration micro-filtration, use polysulfones micropore ultra-filtration membrane ultrafiltration and concentration to 10% of original volume then gained filtrate, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 2cm/s, and working pressure is 0.08MPa, and temperature is 60 ℃; Adopt centrifugal spray-dryer to the liquid spray drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 180 ℃, and air outlet temperature is controlled at 80 ℃, makes pulverous soybean peel pectin gellike polysaccharide, and polysaccharide extract rate is 17.85%.
Embodiment 3
Utilize Universalpulverizer milling soya seeds kind skin, collected the pressed powder of 50 mesh sieves; Take by weighing the soybean peel powder 50g after the pulverizing, add massfraction and be 1.5% ethanolic soln 1L, stirring at room is handled 80min, filters then, and ethanol reclaims, the filter residue drying under reduced pressure; Take by weighing soybean peel powder 67g dry after the Ethanol Treatment, add massfraction and be 3% ammonium oxalate solution 1L, carry out microwave treatment, microwave power is 350W, and temperature remains on 98 ℃, and microwave treatment time is 90min; Filter to get filtrate, with the removal of impurities of millipore filtration micro-filtration, use polysulfones micropore ultra-filtration membrane ultrafiltration and concentration to 15% of original volume then gained filtrate, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 6cm/s, and working pressure is 0. 1MPa, and temperature is 80 ℃; Adopt the press spray moisture eliminator to the liquid spray drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 200 ℃, and air outlet temperature is controlled at 80 ℃, makes pulverous soybean peel pectin gellike polysaccharide, and polysaccharide extract rate is 18.12%.
Embodiment 4
Utilize the Universalpulverizer pulverizing through the soybean peel of the drying of dry removal, collected the pressed powder of 60 mesh sieves; Take by weighing the soybean peel powder 200g after the pulverizing, add massfraction and be 2% ethanolic soln 1L, stirring at room is handled 100min, filters then, and ethanol reclaims, the trapped substance drying under reduced pressure; Take by weighing soybean peel powder 100g dry after the Ethanol Treatment, add massfraction and be 5% ammonium oxalate solution 1L, carry out microwave treatment, microwave power is 400W, and temperature remains on 90 ℃, and microwave treatment time is 100min; Filter to get filtrate, with the removal of impurities of millipore filtration micro-filtration, use polysulfones micropore ultra-filtration membrane ultrafiltration and concentration to 5% of original volume then gained filtrate, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 10cm/s, and working pressure is 0.05MPa, and temperature is 40 ℃; Adopt the press spray moisture eliminator to the liquid spray drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 220 ℃, and air outlet temperature is controlled at 90 ℃, makes pulverous soybean peel pectin gellike polysaccharide, and polysaccharide extract rate is 15.16%.
Embodiment 5
Ammonium oxalate solution among above-described embodiment 1～embodiment 4 replaces with the mixing solutions of ammonium sulfate and B component, and B component is oxalic acid (also can be EDTA or citric acid), and the mass ratio of ammonium sulfate and B component is 1:1, and other is with embodiment 1～embodiment 4.
Comparative Examples 1
This Comparative Examples is identical with embodiment 4 processing condition, and just the ethanol decolorization pre-treatment replaces with decolorizing with activated carbon; Decolorizing with activated carbon: interpolation solution quality volume ratio is 1% activated carbon in soybean peel pectin class polysaccharide soln, and bleaching temperature is 50 ℃, and bleaching time is 30 minutes.
Comparative Examples 2
This Comparative Examples is identical with embodiment 4 processing condition, and just the ethanol decolorization pre-treatment replaces with decolorizing with activated carbon; Decolorizing with activated carbon: interpolation solution quality volume ratio is 0.5% activated carbon in soybean peel pectin class polysaccharide soln, and bleaching temperature is 50 ℃, and bleaching time is 30 minutes.
Comparative Examples 3
This Comparative Examples is identical with the above embodiments 4 processing condition, and just microwave auxiliary extraction replaces with high temperature extraction; The ammonium oxalate high temperature extraction: ammonium formiate concentration is 0.6%, and solid-liquid ratio is 1:25, and extracting temperature is 95 ℃, and extraction time is 4 hours.
Comparative Examples 4
This Comparative Examples is identical with embodiment 4 processing condition, and just microwave auxiliary extraction replaces with high temperature extraction; The ammonium oxalate high temperature extraction: ammonium formiate concentration is 0.6%, and solid-liquid ratio is 1:25, and extracting temperature is 90 ℃, and extraction time is 4 hours.
The pectin class polysaccharide that the present invention makes determines that by chromatography of ions figure (as Fig. 2) the monose molar percentage is as shown in table 1:
The soybean peel pectin class polysaccharide monose that table 1 the present invention makes is formed
| The monose title | Molar percentage (%) |
| Fucose | 1.34 |
| Rhamnosyl | 3.02 |
| Pectinose | 3.79 |
| Galn | 0.03 |
| Semi-lactosi | 47.53 |
| Glucose | 3.21 |
| Wood sugar | 25.13 |
| Galacturonic acid | 15.09 |
| Glucuronic acid | 0.86 |
Alcohol pre-treatment is as shown in table 2 to soybean peel pectin class polysaccharide percent of decolourization and protein content influence:
Table 2
| Method | Percent of decolourization | Protein content | The polysaccharide retention rate |
| Without pre-treatment | ----- | 13.26% | 100% |
| Embodiment 1 | 68.37% | 7.52% | 98.8% |
| |
67.53% | 6.32% | 96.2% |
| Embodiment 3 | 69.82% | 7.52% | 97.3% |
| Embodiment 4 | 71.65% | 7.81% | 99.1% |
| Comparative Examples 1 | 75.26% | 12.61% | 51.52% |
| Comparative Examples 2 | 58.68% | 13.14% | 55.36% |
Adopt the short gelling properties contrast of Different Extraction Method gained soybean peel pectin class polysaccharide calcium as shown in table 3:
Table 3
| Method | Gel strength (g/L) | Gel-strength (g power) |
| Acid system extracts | Can not form gel | ------ |
| Alkaline process extracts | Can not form gel | ------ |
| Embodiment 1 | 20 | 140.85 |
| |
20 | 163.28 |
| |
20 | 149.35 |
| Embodiment 4 | 20 | 199.36 |
| Comparative Examples 3 | 50 | 24.33 |
| Comparative Examples 4 | 50 | 35.68 |
Annotate: the calcium chloride volumetric molar concentration is 1mol/L, forms gel spheres and measures with matter structure instrument.
Claims (6)
1. the preparation method of a soybean peel pectin gellike polysaccharide is characterized in that:
1.1 pulverize
Milling soya seeds kind skin was collected the pressed powder of 40～60 mesh sieves;
1.2 ethanol decolorization pre-treatment
Take by weighing the soybean peel powder after a certain amount of pulverizing, adding massfraction is 0.5～2% ethanolic soln, and the solid-liquid ratio of soybean peel powder and ethanolic soln is 50～200g/1L, stirring at room is handled 30～100min, filter then, ethanol reclaims, the filter residue drying under reduced pressure;
1.3 microwave auxiliary extraction
With the soybean peel powder after the Ethanol Treatment, add ammonium oxalate solution or component A, the solid-liquid ratio of soybean peel powder after the processing and ammonium oxalate solution or component A is 40～100g/1L, microwave treatment, microwave power is 200～400W, temperature remains on 85～98 ℃, the microwave action time is at 10～100min, the massfraction of described ammonium oxalate solution is 0.2～5%, component A is the mixing solutions of ammonium sulfate and B component, B component is oxalic acid or EDTA or citric acid, and the mass ratio of ammonium sulfate and B component is 1:1;
1.4 membrane sepn
Feed liquid after microwave treatment is filtered to get filtrate, filtrate is used the removal of impurities of millipore filtration micro-filtration, use the polysulphones hyperfiltration membrane ultrafiltration and concentration to 5～20% of original volume then, the membrane sepn parameter of ultrafiltration and concentration: cross-flow velocity is 1～10cm/s, working pressure is 0.01～0.1MPa, and temperature is 20～80 ℃;
1.5 spraying drying
Adopt centrifugal spray-dryer or press spray moisture eliminator, to the filtrate spraying drying after concentrating through ultra-filtration membrane, inlet temperature is controlled at 160～220 ℃, and air outlet temperature is controlled at 70～90 ℃, namely makes soybean peel pectin gellike polysaccharide.
2. the preparation method of soybean peel pectin gellike polysaccharide according to claim 1, it is characterized in that: soybean peel is the soybean peel through the drying of wet method or dry removal.
3. the preparation method of soybean peel pectin gellike polysaccharide according to claim 1, it is characterized in that: the solid-liquid ratio of soybean peel powder and ethanolic soln is 67～100g/1L.
4. the preparation method of soybean peel pectin gellike polysaccharide according to claim 1, it is characterized in that: the solid-liquid ratio of the soybean peel powder after the Ethanol Treatment and ammonium oxalate solution or component A is 50～67g/1L.
5. the preparation method of soybean peel pectin gellike polysaccharide according to claim 1, it is characterized in that: microwave power is 300～350W, and temperature remains on 95～98 ℃, and the microwave action time is at 60～90min.
6. the preparation method of soybean peel pectin gellike polysaccharide according to claim 1, it is characterized in that: cross-flow velocity is 2～6cm/s, and working pressure is 0.08～0.1MPa, and temperature is 60～80 ℃.
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| CN103224573B (en) * | 2013-04-24 | 2016-01-13 | 上海交通大学 | The method of pectin is extracted in skin of beancurd |
| 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 |
| CN108912242B (en) * | 2018-07-11 | 2021-07-27 | 淮阴工学院 | Method for extracting pectin with high gelatinization degree from pomelo peel in plateau mountain |
| CN110025503A (en) * | 2019-05-15 | 2019-07-19 | 渤海大学 | It is a kind of using soybean polyoses as edibility lipstick of raw material and preparation method thereof |
| CN110101072A (en) * | 2019-06-18 | 2019-08-09 | 渤海大学 | A kind of shellfish conditioning food emulsifying gelling agent and its preparation method and application |
| CN110859301A (en) * | 2019-09-24 | 2020-03-06 | 南昌大学 | Preparation method of mesona chinensis benth polysaccharide-soybean protein isolate composite gel |
| CN111920055A (en) * | 2020-08-06 | 2020-11-13 | 暨南大学 | Application of soybean seed coat extract in preparation of food or health-care product with weight-losing function |
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| CN1861638A (en) * | 2005-10-25 | 2006-11-15 | 山东万得福实业集团有限公司 | Process for preparing pectin and heavy metallic ion adsorber by soybean peel combined production |
| RU2322456C1 (en) * | 2007-02-19 | 2008-04-20 | Государственное образовательное учреждение высшего профессионального образования "Мордовский государственный университет им. Н.П. Огарева" | Method for preparing pectin |
| CN101838343A (en) * | 2010-04-29 | 2010-09-22 | 广西大学 | Method for preparing pectin by using waste sisal dregs |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1861638A (en) * | 2005-10-25 | 2006-11-15 | 山东万得福实业集团有限公司 | Process for preparing pectin and heavy metallic ion adsorber by soybean peel combined production |
| RU2322456C1 (en) * | 2007-02-19 | 2008-04-20 | Государственное образовательное учреждение высшего профессионального образования "Мордовский государственный университет им. Н.П. Огарева" | Method for preparing pectin |
| CN101838343A (en) * | 2010-04-29 | 2010-09-22 | 广西大学 | Method for preparing pectin by using waste sisal dregs |
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