CN117362480A - Preparation method of high-quality purified agar - Google Patents

Preparation method of high-quality purified agar Download PDF

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Publication number
CN117362480A
CN117362480A CN202311455303.8A CN202311455303A CN117362480A CN 117362480 A CN117362480 A CN 117362480A CN 202311455303 A CN202311455303 A CN 202311455303A CN 117362480 A CN117362480 A CN 117362480A
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agar
hedge
cleaning
water
preparation
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刘跃彬
赵守辉
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Jiangsu Global Marine Biotechnology Co ltd
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Jiangsu Global Marine Biotechnology Co ltd
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Priority to CN202311455303.8A priority Critical patent/CN117362480A/en
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0003General processes for their isolation or fractionation, e.g. purification or extraction from biomass
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08BPOLYSACCHARIDES; DERIVATIVES THEREOF
    • C08B37/00Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
    • C08B37/0006Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
    • C08B37/0036Galactans; Derivatives thereof
    • C08B37/0039Agar; Agarose, i.e. D-galactose, 3,6-anhydro-D-galactose, methylated, sulfated, e.g. from the red algae Gelidium and Gracilaria; Agaropectin; Derivatives thereof, e.g. Sepharose, i.e. crosslinked agarose

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Molecular Biology (AREA)
  • General Health & Medical Sciences (AREA)
  • Biochemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Sustainable Development (AREA)
  • Edible Seaweed (AREA)

Abstract

The invention discloses a preparation method of high-quality purified agar, which specifically comprises the following steps: s1, preprocessing operation; s2, filtering and purifying operation; s3, preparing agar; s4, preparing a mixed solution; s5, preparing purified agar; the invention relates to the technical field of preparation of purified agar. According to the preparation method of the high-quality purified agar, the enzyme preparation is added to decompose the agar into small molecules, so that the melting point of the agar is reduced, meanwhile, impurities such as fat, protein and fiber can be removed, and other physical conditions are matched, so that the prepared agar can be dissolved at about 65 ℃, has high gel strength and high transmittance, has good water retention, can be applied to the food and pharmaceutical industries, has strong practicability, can reduce the water evaporation of fruits and vegetables by inhibiting the growth of escherichia coli and Alternaria alternata, has good application prospect in the field of fruit and vegetable fresh-keeping, and can realize the automatic production of the agar.

Description

Preparation method of high-quality purified agar
Technical Field
The invention relates to the technical field of preparation of purified agar, in particular to a preparation method of high-quality purified agar.
Background
Agar, also called agar, which is a gelatin product made of algae, such as agar of genus Gelidium and genus Lawsonia , is a curing agent of the most commonly used microorganism culture medium, is also used for meat, fish, poultry cans and cosmetics, medicines and dental care, is a polysaccharide extracted from algae, is one of the most widely used seaweed glues in the world at present, has wide application in many aspects such as food industry, pharmaceutical industry, daily chemical industry, bioengineering, etc., can obviously change the quality of food in food, improves the grade of food, and has high price, and is characterized in that: the agar-agar gel has the physical and chemical properties of coagulability and stability, can form complex with some substances, can be used as a thickening agent, a coagulating agent, a suspending agent, an emulsifying agent, a preservative and a stabilizing agent, and is widely used for preparing granulated orange and various beverages, jelly, ice cream, cakes, soft sweets, cans, meat products, eight-treasure porridge, tremella cubilose, thick soup food, cold dishes and the like, and agar can be used as a culture medium, an ointment base and other purposes in the chemical industry and medical science.
In various equipment devices for extracting agar, the existing equipment structure has the defects of complex structure, high preparation cost, difficult control of technological parameters, low extraction efficiency, difficult guarantee of product quality, unfriendly extraction environment and the like, and impurities in the algae are not removed completely to carry out subsequent work in the processing process of the agar, so that impurities remain in the finished product to influence the final quality of the agar, and the agar cannot inhibit the growth of microorganisms although not utilized by microorganisms, thereby reducing the spoilage of foods caused by bacterial infection.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method of high-quality purified agar, which solves the problems that the extraction efficiency is low, impurities remain in finished products and the final quality of the agar is affected.
In order to achieve the above purpose, the invention is realized by the following technical scheme: the preparation method of the high-quality purified agar specifically comprises the following steps: s1, preprocessing operation: adding sodium hydroxide into a cleaning and soaking device to fully dissolve the selected hedge in water, soaking the hedge in the cleaning and soaking device for 2-4 hours, discharging the water after the soaking is finished, injecting clear water into the cleaning and soaking device, and centrifugally stirring and cleaning the hedge;
s2, filtering and purifying operation: taking out the cleaned hedge from the cleaning and soaking device, putting the hedge into a glue boiling device, adding water into the glue boiling device, heating and boiling the hedge to form colloid, controlling the temperature to be 90-100 ℃, pouring the colloid-formed hedge into a stirring pot, adding perlite filtering agent, stirring uniformly, removing impurities which are not removed in the colloid-formed hedge again, putting the colloid-formed hedge into a dryer for drying, controlling the drying time to be 1-2 hours, controlling the drying temperature to be 60-80 ℃, and grinding the hedge into powder after drying;
s3, preparation of agar: dispersing agar powder in deionized water to obtain agar suspension, adding benzoic anhydride under stirring, adjusting pH to 6-9 for reaction, centrifuging to remove supernatant, washing with deionized water, adding deionized water to form agar suspension, adding agar flocculant, and flocculating to obtain agar;
s4, preparing a mixed solution: adding water into agar, heating to dissolve the agar completely, obtaining an agar solution at 80-90 ℃, adding organic acid into the agar solution, adjusting the pH to 6.0-6.5, obtaining an acid solution, adding an enzyme preparation into the acid solution, and decomposing the agar in the acid solution to obtain a mixed solution;
s5, preparing purified agar: and (3) centrifugally separating the slurry obtained in the step (S4) to obtain a dehydrated material, carrying out microwave drying and sterilization on the dehydrated material to obtain a dried product, crushing the dried product, removing iron, sieving and screening to obtain agar.
Preferably, in the step S1, after the first soaking is finished, the soaked water is discharged from the cleaning and soaking device, recovered and stored until the water is used next time, and after stirring and cleaning, the water is discharged from the cleaning and soaking device, and stirring and cleaning are repeated for five times until the hedge is beige.
Preferably, in the step S1, the gracilaria is centrifuged, so that impurities in the gracilaria can be thrown out, and the purity of the gracilaria is improved.
Preferably, in the step S2, the evenly stirred colloidal hedge is conveyed into a filter for the first time filtration, the effluent colloid enters another filter for the second time filtration, and the colloidal hedge is filtered and purified.
Preferably, in the step S3, the sulfuric acid group content of the agar powder is 0.30.9w/v%, and the gel strength is 300-500g/cm < 2 >; the mass ratio of the agar to the benzoic anhydride in the heterogeneous aqueous solution is 3:1 to 6:1, the pH of the reaction is 6-9, the temperature is 30-50 ℃ and the time is 1-3 h, and in S3, the agar flocculant is one or a mixture of more of ethanol, propanol, butanol, glycol, propylene glycol and glycerol.
Preferably, in the step S4, the heating time is 25-35min, the organic acid comprises at least one of citric acid, acetic acid, sorbic acid and malic acid, the adding amount of the organic acid is 0.1% -2.5% of the mass of the agar solution, the enzyme preparation comprises xylanase, lipase and amylase, and the adding amount of the enzyme preparation is 0.02% -0.03% of the mass of the agar.
Preferably, in the step S5, the temperature of microwave drying and sterilization is 90-100 ℃, and the sieving is a 60-100 mesh sieve.
Advantageous effects
The invention provides a preparation method of high-quality purified agar. Compared with the prior art, the method has the following beneficial effects: the preparation method of the high-quality purified agar specifically comprises the following steps: s1, preprocessing operation; s2, filtering and purifying operation; s3, preparing agar; s4, preparing a mixed solution; s5, preparing purified agar; the preparation method has the advantages that the melting point of the agar is reduced by adding the enzyme preparation, meanwhile, impurities such as fat, protein and fiber can be removed, and meanwhile, other physical conditions are matched, so that the prepared agar can be dissolved at about 65 ℃, has high gel strength, high transmittance and good water holding capacity, can be applied to the food and pharmaceutical industries, has strong practicability, can reduce the water evaporation of fruits and vegetables by inhibiting the growth of escherichia coli and alternaria alternata, and has good application prospect in the field of fruit and vegetable fresh-keeping.
Drawings
FIG. 1 is a flow chart of the steps of the present invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Referring to fig. 1, the present invention provides three technical solutions: the preparation method of the high-quality purified agar specifically comprises the following examples:
example 1
S1, preprocessing operation: adding sodium hydroxide into a cleaning and soaking device to fully dissolve the sodium hydroxide in water, putting selected hedge vegetables into the cleaning and soaking device, soaking for 3 hours, discharging the water after the soaking is finished, injecting clear water into the cleaning and soaking device, and centrifugally stirring and cleaning the hedge vegetables;
s2, filtering and purifying operation: taking out the cleaned hedge from the cleaning and soaking device, putting the hedge into a glue boiling device, adding water into the glue boiling device, heating and boiling the hedge to form colloid, controlling the temperature to be 95 ℃, pouring the colloid-formed hedge into a stirring pot, adding perlite filtering agent, stirring uniformly, removing impurities which are not removed in the colloid-shaped hedge again, putting the colloid-shaped hedge into a dryer for drying, controlling the drying time to be 1.5 hours, controlling the drying temperature to be 70 ℃, and grinding the hedge into powder after drying;
s3, preparation of agar: dispersing agar powder in deionized water to obtain agar suspension, adding benzoic anhydride under stirring, adjusting pH to 7.5 for reaction, centrifuging to remove supernatant, washing with deionized water, adding deionized water to form agar suspension, adding agar flocculant, and flocculating to obtain agar;
s4, preparing a mixed solution: adding water into agar, heating to dissolve the agar completely, obtaining an agar solution at a temperature of 85 ℃, adding organic acid into the agar solution, adjusting the pH to 6.25 to obtain an acidic solution, and adding an enzyme preparation into the acidic solution to decompose the agar in the acidic solution to obtain a mixed solution;
s5, preparing purified agar: and (3) centrifugally separating the slurry obtained in the step (S4) to obtain a dehydrated material, carrying out microwave drying and sterilization on the dehydrated material to obtain a dried product, crushing the dried product, removing iron, sieving and screening to obtain agar.
Example two
S1, preprocessing operation: adding sodium hydroxide into a cleaning and soaking device to fully dissolve the sodium hydroxide in water, putting selected hedge vegetables into the cleaning and soaking device to soak for 2 hours, discharging the water after the soaking is finished, injecting clear water into the cleaning and soaking device, and centrifugally stirring and cleaning the hedge vegetables;
s2, filtering and purifying operation: taking out the cleaned hedge from the cleaning and soaking device, putting the hedge into a glue boiling device, adding water into the glue boiling device, heating and boiling the hedge to form colloid, controlling the temperature to be 90 ℃, pouring the colloid-formed hedge into a stirring pot, adding perlite filtering agent, stirring uniformly, removing impurities which are not removed in the colloid-shaped hedge again, putting the colloid-shaped hedge into a dryer for drying, controlling the drying time to be 1 hour, controlling the drying temperature to be 60 ℃, and grinding the hedge into powder after drying;
s3, preparation of agar: dispersing agar powder in deionized water to obtain agar suspension, adding benzoic anhydride under stirring, adjusting pH to 6, centrifuging to remove supernatant, washing with deionized water, adding deionized water to form agar suspension, adding agar flocculant, and flocculating to obtain agar;
s4, preparing a mixed solution: adding water into agar, heating to dissolve the agar completely, obtaining an agar solution at 80 ℃, adding organic acid into the agar solution, adjusting the pH to 6.0 to obtain an acidic solution, and adding an enzyme preparation into the acidic solution to decompose the agar in the acidic solution to obtain a mixed solution;
s5, preparing purified agar: and (3) centrifugally separating the slurry obtained in the step (S4) to obtain a dehydrated material, carrying out microwave drying and sterilization on the dehydrated material to obtain a dried product, crushing the dried product, removing iron, sieving and screening to obtain agar.
Example III
S1, preprocessing operation: adding sodium hydroxide into a cleaning and soaking device to fully dissolve the sodium hydroxide in water, putting selected hedge vegetables into the cleaning and soaking device to soak for 4 hours, discharging the water after the soaking is finished, injecting clear water into the cleaning and soaking device, and centrifugally stirring and cleaning the hedge vegetables;
s2, filtering and purifying operation: taking out the cleaned hedge from the cleaning and soaking device, putting the hedge into a glue boiling device, adding water into the glue boiling device, heating and boiling the hedge to form colloid, controlling the temperature to be 100 ℃, pouring the colloid-formed hedge into a stirring pot, adding perlite filtering agent, stirring uniformly, removing impurities which are not removed in the colloid-shaped hedge again, putting the colloid-shaped hedge into a dryer for drying, controlling the drying time to be 2 hours, controlling the drying temperature to be 80 ℃, and grinding the hedge into powder after drying;
s3, preparation of agar: dispersing agar powder in deionized water to obtain agar suspension, adding benzoic anhydride under stirring, adjusting pH to 9, centrifuging to remove supernatant, washing with deionized water, adding deionized water to form agar suspension, adding agar flocculant, and flocculating to obtain agar;
s4, preparing a mixed solution: adding water into agar, heating to dissolve the agar completely, obtaining an agar solution at 90 ℃, adding organic acid into the agar solution, adjusting the pH to 6.5 to obtain an acidic solution, and adding an enzyme preparation into the acidic solution to decompose the agar in the acidic solution to obtain a mixed solution;
s5, preparing purified agar: and (3) centrifugally separating the slurry obtained in the step (S4) to obtain a dehydrated material, carrying out microwave drying and sterilization on the dehydrated material to obtain a dried product, crushing the dried product, removing iron, sieving and screening to obtain agar.
Test method and conclusion
Agar sensory evaluation, sensory criteria, obtained in each of the above examples: according to the requirements of GB1975-2010, in an environment with sufficient light and no peculiar smell, spreading agar fine powder in Bai Cipan, observing the shape and color of agar, and smelling the smell to obtain the following data:
solid appearance Liquid appearance Smell of
Example 1 Off-white Transparent and transparent Without any means for
Example two Off-white Transparent and transparent Without any means for
Example III Off-white Transparent and transparent Without any means for
Comparative example Pale yellow Semitransparent light Has a slight sour taste
According to the table, the agar is decomposed into small molecules by adding the enzyme preparation, so that the melting point of the agar is reduced, meanwhile, impurities such as fat, protein and fiber can be removed, and meanwhile, the prepared agar can be dissolved at about 65 ℃ by matching with other physical conditions, has high gel strength and high transmittance, has good water retention, can be applied to the food and pharmaceutical industries, has strong practicability, can reduce the water evaporation of fruits and vegetables by inhibiting the growth of escherichia coli and alternaria, and has good application prospect in the fruit and vegetable fresh-keeping field.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (7)

1. A preparation method of high-quality purified agar is characterized by comprising the following steps: the method specifically comprises the following steps:
s1, preprocessing operation: adding sodium hydroxide into a cleaning and soaking device to fully dissolve the selected hedge in water, soaking the hedge in the cleaning and soaking device for 2-4 hours, discharging the water after the soaking is finished, injecting clear water into the cleaning and soaking device, and centrifugally stirring and cleaning the hedge;
s2, filtering and purifying operation: taking out the cleaned hedge from the cleaning and soaking device, putting the hedge into a glue boiling device, adding water into the glue boiling device, heating and boiling the hedge to form colloid, controlling the temperature to be 90-100 ℃, pouring the colloid-formed hedge into a stirring pot, adding perlite filtering agent, stirring uniformly, removing impurities which are not removed in the colloid-formed hedge again, putting the colloid-formed hedge into a dryer for drying, controlling the drying time to be 1-2 hours, controlling the drying temperature to be 60-80 ℃, and grinding the hedge into powder after drying;
s3, preparation of agar: dispersing agar powder in deionized water to obtain agar suspension, adding benzoic anhydride under stirring, adjusting pH to 6-9 for reaction, centrifuging to remove supernatant, washing with deionized water, adding deionized water to form agar suspension, adding agar flocculant, and flocculating to obtain agar;
s4, preparing a mixed solution: adding water into agar, heating to dissolve the agar completely, obtaining an agar solution at 80-90 ℃, adding organic acid into the agar solution, adjusting the pH to 6.0-6.5, obtaining an acid solution, adding an enzyme preparation into the acid solution, and decomposing the agar in the acid solution to obtain a mixed solution;
s5, preparing purified agar: and (3) centrifugally separating the slurry obtained in the step (S4) to obtain a dehydrated material, carrying out microwave drying and sterilization on the dehydrated material to obtain a dried product, crushing the dried product, removing iron, sieving and screening to obtain agar.
2. The method for preparing high-quality purified agar according to claim 1, wherein: in the step S1, after the first soaking is finished, the soaked water is discharged from the cleaning soaking device, recovered and stored until the next use, the water is discharged from the cleaning soaking device after stirring and cleaning, and stirring and cleaning are repeated for five times until the hedge is in a beige color.
3. The method for preparing high-quality purified agar according to claim 1, wherein: in the S1, the gracilaria is centrifugally operated, so that impurities in the gracilaria can be thrown out, and the purity of the gracilaria is improved.
4. The method for preparing high-quality purified agar according to claim 1, wherein: in the step S2, the evenly stirred colloidal hedge is conveyed into a filter for the first time filtration, the effluent colloid enters another filter for the second time filtration, and the colloidal hedge is filtered and purified.
5. The method for preparing high-quality purified agar according to claim 1, wherein: in the step S3, the sulfuric acid group content of the agar powder is 0.30.9w/v%, and the gel strength is 300-500g/cm < 2 >; the mass ratio of the agar to the benzoic anhydride in the heterogeneous aqueous solution is 3:1 to 6:1, the pH of the reaction is 6-9, the temperature is 30-50 ℃ and the time is 1-3 h, and in S3, the agar flocculant is one or a mixture of more of ethanol, propanol, butanol, glycol, propylene glycol and glycerol.
6. The method for preparing high-quality purified agar according to claim 1, wherein: in the step S4, the heating time is 25-35min, the organic acid comprises at least one of citric acid, acetic acid, sorbic acid and malic acid, the adding amount of the organic acid is 0.1-2.5% of the mass of the agar solution, the enzyme preparation comprises xylanase, lipase and amylase, and the adding amount of the enzyme preparation is 0.02-0.03% of the mass of the agar.
7. The method for preparing high-quality purified agar according to claim 1, wherein: in the step S5, the temperature of microwave drying and sterilization is 90-100 ℃, and the sieving is that a 60-100 mesh sieve is adopted.
CN202311455303.8A 2023-11-03 2023-11-03 Preparation method of high-quality purified agar Pending CN117362480A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117343215A (en) * 2023-12-06 2024-01-05 中国海洋大学 Method for extracting agar from agar

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117343215A (en) * 2023-12-06 2024-01-05 中国海洋大学 Method for extracting agar from agar
CN117343215B (en) * 2023-12-06 2024-02-09 中国海洋大学 Method for extracting agar from agar

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