CN111150049A - Preparation method of transparent sanzan glue with high viscosity and high gel strength - Google Patents
Preparation method of transparent sanzan glue with high viscosity and high gel strength Download PDFInfo
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- CN111150049A CN111150049A CN202010017852.7A CN202010017852A CN111150049A CN 111150049 A CN111150049 A CN 111150049A CN 202010017852 A CN202010017852 A CN 202010017852A CN 111150049 A CN111150049 A CN 111150049A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/20—Foods or foodstuffs containing additives; Preparation or treatment thereof containing gelling or thickening agents
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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Abstract
The invention relates to a preparation method of transparent sanzang glue with high viscosity and high gel strength, which comprises the following steps: adding sanzan gum into water, stirring to dissolve completely, heating to 75-95 deg.C, maintaining for 15-45min, cooling, adjusting pH, stirring at constant temperature, and adjusting to neutral; naturally cooling, adding one or more of sodium tripolyphosphate, sodium trimetaphosphate, sodium hexametaphosphate and sodium pyrophosphate, adding one or more of tannic acid, ferulic acid, gallic acid and pyrogallic acid, adding one or more of aluminum sulfate, aluminum chloride, ferric chloride, calcium chloride and magnesium carbonate, and stirring at constant temperature; naturally cooling to room temperature; centrifuging and taking a supernatant; or filtering with plate frame to obtain clear solution; adding inorganic acid into the supernatant or the clear liquid, adjusting the pH value, extracting, neutralizing and drying to obtain the transparent sanzan gum. The method greatly improves the performance of the Sanzan adhesive, and the novel biopolymer has wider application prospect.
Description
Technical Field
The invention belongs to the technical field of microbial glue, and particularly relates to a preparation method of transparent sanzang glue with high viscosity and high gel strength.
Background
Sphingol gums (Sphingans) are a general name for a class of polymers synthesized by certain strains of the genus Sphingomonas (Sphingans), including gellan gum, welan gum, sanzan gum, and the like, and these products are high-molecular polysaccharides composed of glucose, glucuronic acid, rhamnose and/or mannose, and have similar thickening and gelling properties. Because the side chain groups of the gellan gum, the welan gum and the sanzan gum are different in types and positions, the products have unique physical properties and application ranges. The gellan gum has the characteristics of low gelling concentration, high water holding capacity and good stability, is widely used in products such as beverages, bread, dairy products, jelly and the like, and also is used as a carrier material for tissue engineering and drug sustained release. The welan gum has good thickening performance and unique temperature resistance and salt tolerance, and still keeps high viscosity under the conditions of high temperature of 120 ℃ and 10% chloride. Sanzang gum is also called sphingosine gum Ss, is a new variety of sphingosine gum, and is the first kind of sphingosine gum which is completely independently researched and developed at home and realizes industrial production; the sanzang gum is of a proteoglycan structure, is linked with a protein side chain on a polysaccharide component, has the advantages of high fermentation conversion rate and low production cost, has obvious price advantage compared with gellan gum and welan gum, is mainly used as a thickening agent, a stabilizing agent and a coagulating agent, and is used for products such as fruit and vegetable juice (pulp) beverages, vegetable protein beverages, meat sausages and the like. However, as a newly developed product, sanzang glue also has some problems in the application process, such as high turbidity, low viscosity and low gel strength of the aqueous solution of the product.
Currently, patent publications relating to the preparation and properties of sanzan gum products are: "a sphingomonas and adopt the method of this bacterial production microorganism polysaccharide" (CN200610048338.X), detect the viscosity of 1% sanzan glue product water solution reaches 1900cP according to the method of GB13886-92, the shear property value is 7.5; "method for producing microbial polysaccharide-sanzan gum using sphingomonas as strain" (CN201910354160.9), the gel strength of 1% aqueous solution of sanzan gum product is 25-30g/cm2. Compared with the products of sphingosine glue such as gellan gum and welan gum, the viscosity and the gel strength of the current sanzan gum products are lower.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides the preparation method of the transparent sanzan glue with high viscosity and high gel strength, and the method greatly improves the performance of the sanzan glue and enables the novel biopolymer to have wider application prospect.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of transparent sanzang glue with high viscosity and high gel strength comprises the following steps:
adding sanzan glue into water according to the mass volume percentage of 0.1-0.3%, stirring for 12-24h, fully dissolving, heating to 75-95 ℃, maintaining the temperature for 15-45min, cooling to 45-60 ℃, adding alkali liquor to adjust the pH to 10-11, stirring at 45-60 ℃, keeping the temperature for 10-35min, and adjusting the pH of the feed liquid to be neutral by using inorganic acid; naturally cooling to 40-50 deg.C, adding one or more of sodium tripolyphosphate, sodium trimetaphosphate, sodium hexametaphosphate and sodium pyrophosphate until the final concentration is 0-0.1%, adding one or more of tannic acid, ferulic acid, gallic acid and pyrogallic acid until the mass volume percentage is 0-0.03%, adding one or more of aluminum sulfate, aluminum chloride, ferric chloride, calcium chloride and magnesium carbonate until the mass volume percentage is 0.01-0.06%, stirring at 35-45 deg.C, and maintaining the temperature for 10-30 min; naturally cooling to room temperature;
centrifuging for 30min at 4000-; or using 1-3% diatomite as filter aid, 200 mesh filter cloth as filter medium, filtering at 45-80 deg.C under 0.1-0.3MPa to obtain filtrate;
adding inorganic acid into the supernatant or the filtrate, adjusting the pH value to 1-3, extracting to obtain a fibrous sanzan glue product, neutralizing and drying to obtain the transparent sanzan glue.
And the alkali liquor is one or the combination of sodium hydroxide, potassium hydroxide and magnesium hydroxide.
And the inorganic acid is one or the combination of hydrochloric acid, phosphoric acid and acetic acid.
And when in neutralization, one or the combination of sodium carbonate, sodium bicarbonate and calcium carbonate is adopted for neutralization.
And, the drying condition is 60-80 ℃.
The invention has the advantages and positive effects that:
1. the transparent sanzan glue prepared by the method has higher clarity, higher viscosity, gel strength and water retention performance, the viscosity is 4.4-5.6 times of that of the original sanzan glue product, the gel strength is 3.5-3.9 times of that of the original sanzan glue product, the water retention rate is improved by 6.6-8.2%, and the light transmittance is improved by 86.2-88.3%. The method greatly improves the performance of the sanzang gum and ensures that the novel biopolymer has wider application prospect.
2. Sodium trimetaphosphate, sodium tripolyphosphate and the like are used as polysaccharide cross-linking agents, so that the properties of viscosity and the like of the polysaccharide can be improved; polyphenols such as tannic acid and ferulic acid can react with amino acids such as tyrosine and lysine in protein to generate crosslinking effect; the sanzang gum belongs to a proteoglycan structure, a polysaccharide main chain consists of glucose, glucuronic acid, rhamnose and mannose, a side chain has a protein component, and a polysaccharide cross-linking agent and a protein cross-linking agent can generate synergistic interaction under a proper reaction condition, so that the viscosity and the gel strength of the sanzang gum are greatly improved.
Drawings
Fig. 1 is a graph comparing rheological properties of sanzajiao solution in the present invention.
Detailed Description
The following detailed description of the embodiments of the present invention is provided for the purpose of illustration and not limitation, and should not be construed as limiting the scope of the invention.
The raw materials used in the invention are conventional commercial products unless otherwise specified; the methods used in the present invention are conventional in the art unless otherwise specified.
A preparation method of transparent sanzang glue with high viscosity and high gel strength comprises the following steps:
adding sanzan glue into water according to the mass volume percentage of 0.1-0.3%, stirring for 12-24h, fully dissolving, heating to 75-95 ℃, maintaining the temperature for 15-45min, cooling to 45-60 ℃, adding alkali liquor to adjust the pH to 10-11, stirring at 45-60 ℃, keeping the temperature for 10-35min, and adjusting the pH of the feed liquid to be neutral by using inorganic acid; naturally cooling to 40-50 deg.C, adding one or more of sodium tripolyphosphate, sodium trimetaphosphate, sodium hexametaphosphate and sodium pyrophosphate until the final concentration is 0-0.1%, adding one or more of tannic acid, ferulic acid, gallic acid and pyrogallic acid until the mass volume percentage is 0-0.03%, adding one or more of aluminum sulfate, aluminum chloride, ferric chloride, calcium chloride and magnesium carbonate until the mass volume percentage is 0.01-0.06%, stirring at 35-45 deg.C, and maintaining the temperature for 10-30 min; naturally cooling to room temperature;
centrifuging for 30min at 4000-; or using 1-3% diatomite as filter aid, 200 mesh filter cloth as filter medium, filtering at 45-80 deg.C under 0.1-0.3MPa to obtain filtrate;
adding inorganic acid into the supernatant or the filtrate, adjusting the pH value to 1-3, extracting to obtain a fibrous sanzan glue product, neutralizing and drying to obtain the transparent sanzan glue.
Preferably, the alkali liquor is one or a combination of sodium hydroxide, potassium hydroxide and magnesium hydroxide.
Preferably, the inorganic acid is one of hydrochloric acid, phosphoric acid, acetic acid or a combination thereof.
Preferably, one or a combination of sodium carbonate, sodium bicarbonate and calcium carbonate is adopted for neutralization.
Preferably, the drying condition is 60-80 ℃.
Sanzan glue used in the present invention may be provided by hebeixin co-biologicals ltd.
Example 1:
adding sanzan glue into water according to the mass volume percentage of 0.2%, stirring for 12h, heating to 75 ℃ after fully dissolving, maintaining the temperature for 20min, adding 1mol/L sodium hydroxide solution when cooling to 45 ℃, adjusting the pH to about 10.0, stirring at 45 ℃ for 10min at constant temperature, and adjusting the pH of the feed liquid to be neutral by using 1mol/L hydrochloric acid; adding aluminum sulfate to the mass volume percentage of 0.03%, continuing stirring for 10min at 45 ℃, naturally cooling to room temperature, centrifuging for 30min at 7000r/min, taking supernatant, adding 1mol/L hydrochloric acid into the supernatant, adjusting the pH value of the feed liquid to about 3.0, extracting to obtain a fibrous sanzan glue product, neutralizing the product with saturated sodium carbonate solution, and drying at 80 ℃ to obtain a transparent sanzan glue finished product. The indexes of viscosity, shearing property, gel strength, light transmittance, water holding rate and the like of the transparent sanzan glue sample are shown in table 1, the rheological property of 1% colloidal solution is shown in table 1, and the contrast is the original sanzan glue sample.
Example 2:
adding sanzan glue into water according to the mass volume percentage of 0.3%, stirring for 12h, heating to 95 ℃ after fully dissolving, maintaining the temperature for 20min, adding 1mol/L magnesium hydroxide solution when cooling to 45 ℃, adjusting the pH to about 10.0, stirring at 45 ℃ for constant temperature for 30min, and adjusting the pH of the feed liquid to be neutral by using 1mol/L hydrochloric acid; adding calcium chloride to the mass volume percentage of 0.05 percent, continuously stirring for 10min at 45 ℃, using 1 percent of diatomite as a filter aid and 200-mesh filter cloth as a filter medium, carrying out framed filtration under the conditions of 80 ℃ and 0.2MPa of pressure, adding 1mol/L of phosphoric acid into filtrate, adjusting the pH value of the feed liquid to about 2.0, extracting to obtain a fibrous sanzan glue product, neutralizing the product with a saturated sodium bicarbonate solution, and drying at 60 ℃ to obtain a transparent sanzan glue finished product. The indexes of viscosity, shearing property, gel strength, light transmittance, water holding rate and the like of the transparent sanzan glue sample are shown in table 1, the rheological property of 1% colloidal solution is shown in table 1, and the contrast is the original sanzan glue sample.
Example 3:
adding sanzan glue into water according to the mass volume percentage of 0.15%, stirring for 12h, heating to 80 ℃ after fully dissolving, maintaining the temperature for 35min, adding 1mol/L sodium hydroxide solution when cooling to 60 ℃, adjusting the pH to about 11.0, stirring at 60 ℃ for constant temperature for 20min, and adjusting the pH of the feed liquid to be neutral by using 1mol/L hydrochloric acid; naturally cooling to 45 deg.C, adding sodium trimetaphosphate to 0.05%, adding pyrogallic acid to 0.01% by mass volume, adding magnesium carbonate to 0.03% by mass volume, stirring at 45 deg.C and holding the temperature for 30 min; naturally cooling to room temperature, using 1% of diatomite as a filter aid, using 200-mesh filter cloth as a filter medium, performing framed filtration under the conditions of 60 ℃ and 0.25MPa of pressure, adding 1mol/L of hydrochloric acid into filtrate, adjusting the pH value of feed liquid to about 2.0, extracting to obtain a fibrous sanzan gum product, neutralizing the product with a saturated sodium bicarbonate solution, and drying at 60 ℃ to obtain a transparent sanzan gum finished product. The indexes of viscosity, shearing property, gel strength, light transmittance, water holding rate and the like of the transparent sanzan glue sample are shown in table 1, the rheological property of 1% colloidal solution is shown in table 1, and the contrast is the original sanzan glue sample.
Example 4:
adding sanzan glue into water according to the mass volume percentage of 0.1%, stirring for 12h, heating to 80 ℃ after fully dissolving, maintaining the temperature for 35min, adding 1mol/L potassium hydroxide solution when cooling to 60 ℃, adjusting the pH to about 11.0, stirring at 60 ℃ for constant temperature for 20min, and adjusting the pH of the feed liquid to be neutral by using 1mol/L hydrochloric acid; naturally cooling to 40 ℃, adding sodium tripolyphosphate to 0.03%, adding tannic acid to 0.005% by mass volume, adding calcium chloride to 0.03% by mass volume, stirring at 35 ℃ and keeping the temperature for 20 min; 2% of diatomite is used as a filter aid, 200-mesh filter cloth is used as a filter medium, the filter medium is subjected to framed filtration under the conditions that the temperature is 70 ℃ and the pressure is 0.25MPa, 1mol/L of hydrochloric acid is added into filtrate, the pH value of feed liquid is adjusted to be about 3.0, a fibrous sanzan gum product is obtained through extraction, the product is neutralized by saturated sodium carbonate solution and then dried at 80 ℃, and a transparent sanzan gum finished product is obtained. The indexes of viscosity, shearing property, gel strength, light transmittance, water holding rate and the like of the transparent sanzan glue sample are shown in table 1, the rheological property of 1% colloidal solution is shown in table 1, and the contrast is the original sanzan glue sample.
The related detection method of the invention comprises the following steps:
detection of viscosity and shear properties:
preparing 1% colloidal solution, placing 100mL colloidal solution in a high-type beaker, and detecting the viscosity value of η at the rotation speed of 60r/min by using a Brookfield rotary viscometer at the temperature of 25 DEG C1The viscosity value of the product is obtained in cP.
Detecting the viscosity value η of the colloidal solution at the rotating speed of 6r/min under the same condition2Shear performance value N of η2/η1。
Detection of gel strength:
preparing 1% colloidal solution, placing 100mL colloidal solution in a high-type beaker, sealing the beaker mouth with a preservative film, heating in 90 deg.C water bath for 30min, naturally cooling to gel, placing in a 20 deg.C thermostat for 24h, measuring gel strength with TA.XT2i texture analyzer and P/0.5R probe, wherein the unit is g/cm2。
Light transmittance:
preparing 0.1% colloidal solution, placing the colloidal solution in a 10mm glass cuvette, standing at room temperature for 30min, and measuring light transmittance at 497nm with a spectrophotometer with distilled water as control.
Water retention rate:
preparing 1% colloidal solution by mass and volume, placing 100mL of colloidal solution into a high-type beaker, sealing the mouth of the beaker by using a preservative film, placing the beaker in a water bath at 90 ℃ for heating for 30min, placing the beaker at room temperature for 24h, removing the preservative film at the mouth of the beaker, placing the beaker in a ventilation drying oven at constant temperature of 80 ℃, measuring the colloidal mass after 4h, wherein the water holding rate calculation formula is as follows: water retention [% ] (% (mass of colloid after water loss/mass of colloid originally) × 100.
Rheological Properties:
preparing 1% colloid solution, placing 100mL colloid solution in a high-type beaker, measuring the rheological property of the colloid solution under different shear rates by using a Brookfield R/S Plus rheometer at 25 ℃, selecting a cc40 rotor, and adjusting the shear rate within 120S for 1S-1-200s-1-1s-1The rheological behaviour of the colloidal solution was determined in this interval.
TABLE 1 index Table of viscosity, shear property, gel strength, light transmittance and water holding rate of Sanzan glue samples of control and examples 1-4 in the present invention
Examples 1 and 2 show that the cell removal by centrifugation or plate-and-frame filter pressing can obviously improve the transparency of sanzan glue, and the viscosity and the gel strength of the product are improved to a certain extent due to the improvement of purity. In the embodiments 3 and 4, after the composite cross-linking agents such as sodium tripolyphosphate and tannic acid are added, the polysaccharide main chain and the protein side chain of sanzan gum generate a cross-linking effect and aggregate into a network framework through a chain bridge effect, so that the transparency is improved, the viscosity, the gel strength and the water retention performance are also greatly improved, the viscosity is 4.4-5.6 times of that of the original sanzan gum product, the gel strength is 3.5-3.9 times of that of the original sanzan gum product, and the water retention rate is improved by 6.6-8.2%.
Although the embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the embodiments disclosed.
Claims (5)
1. A preparation method of transparent sanzang glue with high viscosity and high gel strength is characterized by comprising the following steps: the method comprises the following steps:
adding sanzan glue into water according to the mass volume percentage of 0.1-0.3%, stirring for 12-24h, fully dissolving, heating to 75-95 ℃, maintaining the temperature for 15-45min, cooling to 45-60 ℃, adding alkali liquor to adjust the pH to 10-11, stirring at 45-60 ℃, keeping the temperature for 10-35min, and adjusting the pH of the feed liquid to be neutral by using inorganic acid; naturally cooling to 40-50 deg.C, adding one or more of sodium tripolyphosphate, sodium trimetaphosphate, sodium hexametaphosphate and sodium pyrophosphate until the final concentration is 0-0.1%, adding one or more of tannic acid, ferulic acid, gallic acid and pyrogallic acid until the mass volume percentage is 0-0.03%, adding one or more of aluminum sulfate, aluminum chloride, ferric chloride, calcium chloride and magnesium carbonate until the mass volume percentage is 0.01-0.06%, stirring at 35-45 deg.C, and maintaining the temperature for 10-30 min; naturally cooling to room temperature;
centrifuging for 30min at 4000-; or using 1-3% diatomite as filter aid, 200 mesh filter cloth as filter medium, filtering at 45-80 deg.C under 0.1-0.3MPa to obtain filtrate;
adding inorganic acid into the supernatant or the filtrate, adjusting the pH value to 1-3, extracting to obtain a fibrous sanzan glue product, neutralizing and drying to obtain the transparent sanzan glue.
2. The method for preparing transparent sanzang glue with high viscosity and high gel strength as claimed in claim 1, wherein the method comprises the following steps: the alkali liquor is one or the combination of sodium hydroxide, potassium hydroxide and magnesium hydroxide.
3. The method for preparing transparent sanzang glue with high viscosity and high gel strength as claimed in claim 1, wherein the method comprises the following steps: the inorganic acid is one or the combination of hydrochloric acid, phosphoric acid and acetic acid.
4. The method for preparing transparent sanzang glue with high viscosity and high gel strength as claimed in claim 1, wherein the method comprises the following steps: and during the neutralization, one or the combination of sodium carbonate, sodium bicarbonate and calcium carbonate is adopted for neutralization.
5. The method for preparing transparent sanzang glue with high viscosity and high gel strength according to any one of claims 1 to 4, wherein the method comprises the following steps: the drying condition is 60-80 ℃.
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| CN113583904A (en) * | 2021-07-24 | 2021-11-02 | 河北沣川生物科技有限公司 | Extracellular polymer sphingomonas and application thereof in preparation of sanzan glue with high gel strength |
| CN113583904B (en) * | 2021-07-24 | 2023-09-12 | 河北沣川生物科技有限公司 | Extracellular multimeric Sphingomonas and application thereof in preparation of high gel strength sanzan gum |
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| CN114014944B (en) * | 2021-11-05 | 2022-08-26 | 南开大学 | Natural synthetic low-acyl sanzan gum and production method and identification method thereof |
| CN116023520A (en) * | 2023-01-17 | 2023-04-28 | 河北沣川生物科技有限公司 | Preparation method of low-acyl sanzan gum |
| CN116023520B (en) * | 2023-01-17 | 2023-08-22 | 河北沣川生物科技有限公司 | Preparation method of low-acyl sanzan gum |
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