CN114634655A - Pectin production process for coating probiotics - Google Patents

Pectin production process for coating probiotics Download PDF

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Publication number
CN114634655A
CN114634655A CN202210302928.XA CN202210302928A CN114634655A CN 114634655 A CN114634655 A CN 114634655A CN 202210302928 A CN202210302928 A CN 202210302928A CN 114634655 A CN114634655 A CN 114634655A
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pectin
water
temperature
clear water
mixing
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Inventor
叶祖光
邢子刚
孙仕桥
魏于千
王代军
潘玉林
崔秋檀
刘建龙
陈学哲
司书锋
张华磊
刘雁成
梅彬彬
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Chongqing Meng Tai Bio Tech Ltd
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Chongqing Meng Tai Bio Tech Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L5/00Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
    • C08L5/06Pectin; Derivatives thereof
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/04Polysaccharides, i.e. compounds containing more than five saccharide radicals attached to each other by glycosidic bonds
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12QMEASURING OR TESTING PROCESSES INVOLVING ENZYMES, NUCLEIC ACIDS OR MICROORGANISMS; COMPOSITIONS OR TEST PAPERS THEREFOR; PROCESSES OF PREPARING SUCH COMPOSITIONS; CONDITION-RESPONSIVE CONTROL IN MICROBIOLOGICAL OR ENZYMOLOGICAL PROCESSES
    • C12Q1/00Measuring or testing processes involving enzymes, nucleic acids or microorganisms; Compositions therefor; Processes of preparing such compositions
    • C12Q1/02Measuring or testing processes involving enzymes, nucleic acids or microorganisms; Compositions therefor; Processes of preparing such compositions involving viable microorganisms
    • C12Q1/025Measuring or testing processes involving enzymes, nucleic acids or microorganisms; Compositions therefor; Processes of preparing such compositions involving viable microorganisms for testing or evaluating the effect of chemical or biological compounds, e.g. drugs, cosmetics
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate

Abstract

The invention discloses a pectin production process for coating probiotics, and relates to the technical field of pectin production. The invention comprises the following steps: the first step is as follows: mixing fresh lemon peel with clear water according to the proportion of 1: 5, mixing in a container, cleaning the fresh lemon peels for 30min, and repeating for 3 times; the second step is that: mixing the washed lemon peel with clear water according to the proportion of 1: 6 is put into a stirring tank to be stirred, the temperature is controlled to be 75-84 ℃, and 65 percent of concentrated nitric acid is added according to 2 per mill of the addition of clear water; the third step: keeping the temperature at 80 ℃, stirring for 2h, and then adding ammonia water with the concentration of 23 percent to adjust the pH value to 3; the fourth step: separating the extractive solution with plate-and-frame filter press, removing residual insoluble particles from the separated extractive solution with diatomite, and vacuum concentrating with experimental MVR evaporator until pectin content is greater than 2.8%. By adopting the enzymatic viscosity reduction and compound granulation modes, the pectin produced by the process has the characteristics of low viscosity, good solubility and good probiotic coating performance.

Description

Pectin production process for coating probiotics
Technical Field
The invention belongs to the technical field of pectin production, and particularly relates to a production process of pectin for coating probiotics.
Background
Pectin is a high-molecular high-viscosity substance, is difficult to dissolve in water and is often difficult to realize the function development, so various pectin production processes appear in the market; however, pectin produced by the pectin production process in the prior art has high viscosity and poor solubility, and the coating performance of probiotics is generally not ideal.
Disclosure of Invention
The invention aims to provide a pectin production process for coating probiotics, which aims to solve the existing problems that: pectin produced by the pectin production process in the prior art is high in viscosity and poor in solubility, and the coating performance of probiotics is generally not ideal.
In order to solve the technical problems, the invention is realized by the following technical scheme:
the invention relates to a pectin production process for coating probiotics, which comprises the following steps:
the first step is as follows: mixing fresh lemon peel with clear water according to the proportion of 1: 5 in a container, cleaning the fresh lemon peel for 30min, and repeating for 3 times;
the second step is that: mixing the washed lemon peel with clear water according to the proportion of 1: 6 is put into a stirring tank to be stirred, the temperature is controlled to be 75-84 ℃, and 65 percent of concentrated nitric acid is added according to 2 per mill of the addition of clear water;
the third step: keeping the temperature at 80 ℃, stirring for 2h, and then adding ammonia water with the concentration of 23 percent to adjust the pH value to 3;
the fourth step: separating the extractive solution with plate-and-frame filter press, removing residual insoluble particles from the separated extractive solution with diatomite, vacuum concentrating with experimental MVR evaporator until pectin content is more than 2.8%, and maintaining the temperature of the concentrated solution at 40 deg.C;
the fifth step: adjusting pH of the concentrated solution to 3.6 with 23% concentrated ammonia water, adding 500U/mg pectinase (one thirty ten-thousandth of the total amount of the solution), performing enzymolysis for 25min, and adjusting pH to 2 with 65% concentrated nitric acid to stop enzymolysis;
and a sixth step: according to the volume ratio of the enzymolysis liquid to 78% alcohol of 1: 2.2, performing mixed precipitation, separating, and then performing water precipitation for 15min by using 85% alcohol with the same volume, wherein the separated solid is wet pectin, and the solid content is controlled at 78%;
the seventh step: weighing sodium alginate and sodium carbonate, and dissolving in water;
eighth step: spraying the dissolved sodium alginate and sodium carbonate on the surface of the wet pectin, uniformly stirring, drying at 90 ℃ by using a boiling dryer, and crushing after drying until the water content is less than 6%;
the ninth step: and (4) sieving the mixture by a 60-mesh sieve to obtain finished pectin, and using the sieved pectin in a probiotic coating performance test.
Further, the temperature in the second step is controlled at 80 ℃.
Further, the weighed amount of sodium alginate in the seventh step is 0.44% of the weight of the wet pectin, the weighed amount of sodium carbonate is 0.22% of the weight of the wet pectin, and the weighed amount of water is 5% of the weight of the wet pectin.
The invention has the following beneficial effects:
the pectin production process adopts an enzymatic viscosity reduction and compound granulation mode, so that the pectin produced by the process has the characteristics of low viscosity, good solubility and good probiotic coating performance.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a pectin production process for coating probiotics, which comprises the following steps:
the first step is as follows: mixing fresh lemon peel with clear water according to the proportion of 1: 5 in a container, cleaning the fresh lemon peel for 30min, and repeating for 3 times;
the second step is that: mixing the washed lemon peel with clear water according to the proportion of 1: 6 is put into a stirring tank to be stirred, the temperature is controlled to be 75-84 ℃, in the embodiment, the temperature can be controlled to be 80 ℃, and then 65 percent of concentrated nitric acid is added according to 2 per mill of the addition of clear water;
the third step: keeping the temperature at 80 ℃, stirring for 2h, and then adding ammonia water with the concentration of 23 percent to adjust the pH value to 3;
the fourth step: separating the extractive solution with filter pressing equipment, removing residual insoluble particles from the separated extractive solution with diatomite, vacuum concentrating with experimental MVR evaporator until pectin content is more than 2.8%, and maintaining the temperature of the concentrated solution at 40 deg.C; in the embodiment, in order to effectively separate the extracting solution, the filter pressing equipment adopts a plate-and-frame filter press;
the fifth step: adjusting pH of the concentrated solution to 3.6 with 23% concentrated ammonia water, adding 500U/mg pectinase one-thirty-ten-thousandth of the total amount of the solution, performing enzymolysis for 25min, and adjusting pH to 2 with 65% concentrated nitric acid to stop enzymolysis;
and a sixth step: according to the volume ratio of the enzymolysis liquid to 78% alcohol of 1: 2.2, performing mixed precipitation, separating, and then performing water precipitation for 15min by using 85% alcohol with the same volume, wherein the separated solid is wet pectin, and the solid content is controlled at 78%;
the seventh step: weighing sodium alginate and sodium carbonate, dissolving the sodium alginate and the sodium carbonate in water, wherein the weighing amount of the sodium alginate is 0.44% of the weight of the wet pectin, the weighing amount of the sodium carbonate is 0.22% of the weight of the wet pectin, and the weighing amount of the water is 5% of the weight of the wet pectin;
eighth step: spraying the dissolved sodium alginate and sodium carbonate on the surface of the wet pectin, uniformly stirring, drying at 90 ℃ by using a boiling dryer, and crushing after drying until the water content is less than 6%;
the ninth step: then sieving the pectin with a 60-mesh sieve to obtain the finished pectin.
Finally, the finished pectin after being screened by the 60-mesh sieve is used for testing the probiotic coating performance experiment, and the method comprises the following specific steps:
(1) adding the finished pectin produced by the process into a coating agent to prepare a probiotic suspension;
(2) spraying the probiotic suspension in a high-pressure jet device to form atomized uniform coated liquid drops, and blowing the atomized liquid drops by using frozen airflow to quickly solidify the formed uniformly coated probiotic atomized liquid drops; in the embodiment, the high-pressure air can be one of nitrogen, argon or carbon dioxide, the injection pressure of the high-pressure air is 10-15MPa, and the purging pressure is 1-10 MPa; the purging pressure of the freezing airflow is 1-10MPa, the freezing airflow is specifically freezing carbon dioxide, and the temperature of the adopted carbon dioxide is-40 ℃ to-60 ℃;
(3) and collecting the solidified powder product, and decompressing and heating to normal temperature to obtain the uniformly coated probiotic product.
In the step (1), the concentration of the probiotic suspension is 2-5% (w/w), and the concentration of the coating agent is 30-50% (w/w);
specifically, the coating agent can be one or more of fucoidin, skimmed milk powder, sodium alginate, dextran, inulin, sorbitol, sodium acetate, malto-oligosaccharide, alanine, sodium glutamate, lactitol, vitamin C, calcium chloride, and fructo-oligosaccharide;
in detail, the flow rate of the probiotic suspension liquid is 5-10cm 3/s;
in this embodiment, there are 2 probiotic turbid liquid inlet pipes, and the symmetric distribution.
The probiotic bacteria after coating have gastric acid and bile resistance experiment:
1. gastric juice preparation and manipulation
Weighing a plurality of products with 150 hundred million/g of viable bacteria of the coated lactobacillus plantarum prepared by the process as samples, wherein the weight of each sample is 1g, transferring the samples into a preheated test tube filled with 9mL of simulated gastric juice, and treating the samples for 1h, 2h, 3h and 4h at 37 ℃ and 80r/min respectively, wherein each treatment is repeated for 3 times.
The simulated gastric juice is prepared according to the following method: diluting with 9.5% hydrochloric acid and distilled water to pH 1.5; adding 1.0g of pepsin into each 100mL of the mixture, uniformly mixing the mixture, and filtering the mixture by using a sterile filter membrane of 0.22 mu m, wherein the mixture is used as the preparation;
performing gradient dilution on the treated sample solution and the control strain solution, counting viable bacteria by using a pouring method, and calculating the survival rate, wherein the survival rate is (the number of treated bacteria/the number of original bacteria) multiplied by 100%;
2. preparation and operation of intestinal juice
Weighing a plurality of products with 100 hundred million/g of viable bacteria of the coated lactobacillus plantarum prepared by the process as samples, wherein the weight of each sample is 1g, transferring the samples into a test tube filled with 9mL of simulated intestinal juice, and treating the samples for 1h, 2h, 3h and 4h at 37 ℃ and 80r/min respectively, wherein each treatment is repeated for 3 times;
the simulated intestinal juice is prepared according to the following method: dissolving 6.8g of KH2PO4 in 500mL of distilled water, adding 3g of cholate and 10g of trypsin, adjusting the pH value of the solution to 6.8 by using a NaOH solution with the concentration of 4g/L, fixing the volume to 1L by using the distilled water, mixing uniformly, and filtering by using a sterile filter membrane with the diameter of 0.22 mu m, wherein the preparation is ready for use;
performing gradient dilution on the treated sample solution and the control strain solution, counting viable bacteria by using a pouring method, and calculating the survival rate, wherein the survival rate is (the number of treated bacteria/the number of original bacteria) multiplied by 100%;
TABLE 1 JYBB-163 survival rate data sheet under in vitro simulated gastrointestinal environment
Figure BDA0003563532040000051
The survival rate data of coated lactobacillus plantarum in an in vitro simulated gastrointestinal environment is shown in table 1, and the survival rate of coated probiotics in an in vitro simulated gastrointestinal environment is very high, 4 hours in gastric juice, the survival rate is still more than 80%, 4 hours in intestinal juice, the survival rate reaches more than 90%, and the functional action is performed to fill up the foundation for the fixed planting of subsequent strains on intestinal tracts.
In conclusion, the pectin production process adopts an enzymatic viscosity reduction and compound granulation mode, so that the obtained pectin has the characteristics of low viscosity, good solubility and good probiotic coating performance.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.

Claims (3)

1. A production process of pectin for coating probiotics is characterized by comprising the following steps: the method comprises the following steps:
the first step is as follows: mixing fresh lemon peel with clear water according to the proportion of 1: 5 in a container, cleaning the fresh lemon peel for 30min, and repeating for 3 times;
the second step is that: mixing the washed lemon peel with clear water according to the proportion of 1: 6 is put into a stirring tank to be stirred, the temperature is controlled to be 75-84 ℃, and 65 percent of concentrated nitric acid is added according to 2 per mill of the addition of clear water;
the third step: keeping the temperature at 80 ℃, stirring for 2h, and then adding ammonia water with the concentration of 23 percent to adjust the pH value to 3;
the fourth step: separating the extractive solution with plate-and-frame filter press, removing residual insoluble particles from the separated extractive solution with diatomite, vacuum concentrating with experimental MVR evaporator until pectin content is more than 2.8%, and maintaining the temperature of the concentrated solution at 40 deg.C;
the fifth step: adjusting pH of the concentrated solution to 3.6 with 23% concentrated ammonia water, adding 500U/mg pectinase one-thirty-ten-thousandth of the total amount of the solution, performing enzymolysis for 25min, and adjusting pH to 2 with 65% concentrated nitric acid to stop enzymolysis;
and a sixth step: according to the volume ratio of the enzymolysis liquid to 78% alcohol of 1: 2.2, performing mixed precipitation, separating, and then performing water precipitation for 15min by using 85% alcohol with the same volume, wherein the separated solid is wet pectin, and the solid content is controlled at 78%;
the seventh step: weighing sodium alginate and sodium carbonate, and dissolving in water;
eighth step: spraying the dissolved sodium alginate and sodium carbonate on the surface of the wet pectin, uniformly stirring, drying at 90 ℃ by using a boiling dryer, and crushing after drying until the water content is less than 6%;
the ninth step: sieving with 60 mesh sieve to obtain pectin product.
2. The process for the production of pectin for probiotic coating according to claim 1, characterized in that said temperature in said second step is controlled at 80 ℃.
3. The process for producing pectin for probiotic coating according to claim 1, characterized in that said sodium alginate in said seventh step is weighed as 0.44%, said sodium carbonate is weighed as 0.22% and said water is weighed as 5% of the weight of the wet pectin.
CN202210302928.XA 2022-03-24 2022-03-24 Pectin production process for coating probiotics Pending CN114634655A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116103207A (en) * 2023-03-17 2023-05-12 山东中科嘉亿生物工程有限公司 Bifidobacterium bifidum JYBB-163 for improving semen quality and fertility of male, and microbial inoculum, preparation method and application thereof

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