CN111374295A - Preparation method and application of high-quality food-grade plant-derived compound amino acid - Google Patents
Preparation method and application of high-quality food-grade plant-derived compound amino acid Download PDFInfo
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- CN111374295A CN111374295A CN202010301864.2A CN202010301864A CN111374295A CN 111374295 A CN111374295 A CN 111374295A CN 202010301864 A CN202010301864 A CN 202010301864A CN 111374295 A CN111374295 A CN 111374295A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 30
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- 238000001694 spray drying Methods 0.000 claims abstract description 28
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- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 abstract description 9
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- 239000004278 EU approved seasoning Substances 0.000 description 3
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Images
Classifications
-
- 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
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/20—Synthetic spices, flavouring agents or condiments
- A23L27/21—Synthetic spices, flavouring agents or condiments containing amino acids
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/17—Amino acids, peptides or proteins
- A23L33/175—Amino acids
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention discloses a preparation method and application of high-quality food-grade plant source compound amino acid, which comprises the steps of pretreating vegetable protein, removing impurities and purifying the protein; mixing the pretreated vegetable protein with hydrochloric acid, and performing acid hydrolysis; removing more than 80% of hydrochloric acid from the hydrolysate by a hydrogen chloride recovery device, and realizing the cyclic utilization of the hydrochloric acid; decolorizing the deacidification solution, and removing anions and cations by using anion exchange resin and cation exchange resin; concentrating and spray-drying the effluent to obtain the high-quality food-grade plant source compound amino acid. The invention has the advantages of simple preparation process, low energy consumption, low salt content in the product, short production period and high product quality. Compared with the traditional acid hydrolysis plant protein product, the salt content and the chloropropanol content are greatly reduced, and the development trend of low-salt health food is met.
Description
Technical Field
The invention belongs to the technical field of plant protein, and particularly relates to a preparation method and application of high-quality food-grade plant source compound amino acid.
Background
The plant source compound amino acid is a liquid delicate flavor seasoning prepared by using defatted soybean meal, peanut meal, wheat protein meal (gluten) or corn protein meal and rice protein meal containing edible plant protein as raw materials and performing hydrochloric acid hydrolysis and alkali neutralization, and is widely applied to seasonings and leisure foods.
At present, the process for industrially preparing the plant-derived compound amino acid product generally comprises the steps of hydrolyzing plant-derived protein meal by concentrated hydrochloric acid, adding alkali for neutralization, and preparing the product with neutral or weak acid pH, wherein the method has the advantages of thorough hydrolysis, economy and high efficiency, and has the defect that the method cannot be avoided, such as: the product has more impurities, and the carbohydrate generates bitter taste after high-temperature hydrolysis, so that the taste is influenced; fat generates a large amount of 3-chloropropanol after high-temperature reaction, and the high-dose 3-chloropropanol has physiological toxicity and can cause tumor and damage to kidney and reproductive system; the product has more impurities, low amino acid content and no prominent delicate flavor; the product has high salt content, is not in accordance with the concept of healthy life, and limits the use amount, thereby influencing the addition effect and the like.
Therefore, there is a need in the art for a method for preparing a plant-derived compound amino acid product with high purity, low salt content, fresh flavor and good taste, so as to solve the problems of high salt content, many impurities and low safety of the plant-derived compound amino acid product.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The present invention has been made keeping in mind the above and/or other problems occurring in the prior art.
Therefore, the invention aims to overcome the defects in the prior art and provide a preparation method of high-quality food-grade plant source compound amino acid.
In order to solve the technical problems, the invention provides the following technical scheme: a preparation method of high-quality food-grade plant-derived compound amino acid comprises the steps of crushing a plant protein raw material, sieving the crushed plant protein raw material by 120-140 meshes, and mixing the crushed raw material with water to obtain 10-20% of mixed material liquid; adjusting the pH of the slurry-mixed feed liquid to 9-10 by using sodium hydroxide, stirring for 20-30 minutes, performing centrifugal separation to obtain a filtrate, adding hydrochloric acid into the filtrate, adjusting the pH to 4-5, stirring for 20-30 minutes, and performing centrifugal separation to obtain filter residues; adding water into the obtained filter residue, mixing the obtained filter residue with the water to 10-20%, stirring, and performing centrifugal separation to obtain filter residue separated after mixing, wherein the filter residue is prepared from the following plant protein raw materials: mixing filter residues separated after size mixing with hydrochloric acid according to the mass ratio of 1: 4-6, hydrolyzing at 105-110 ℃ for 6-24 hours under normal pressure to obtain a feed liquid, performing suction filtration to remove insoluble impurities, adjusting the obtained filtrate to the solid content of 10-20%, adding 4-6% of activated carbon, stirring for 15-30 minutes, performing suction filtration to obtain a filtrate, and repeating the steps for 2 times to obtain a decolorized solution; sequentially passing the decolorized solution through pretreated anion exchange resin and cation exchange resin to remove salt; and concentrating the obtained desalted filtrate, and performing spray drying to obtain a powdery product, namely the high-quality food-grade plant source compound amino acid.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: and after stirring for 20-30 minutes, performing centrifugal separation to obtain a filtrate, wherein the stirring temperature is 45-55 ℃, the stirring rotating speed is 150rpm/min, the centrifugal separation rotating speed is 4000rpm/min, and the time is 10 min.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: and adjusting the pH value to 4-5, stirring for 20-30 minutes, and performing centrifugal separation to obtain filter residues, wherein the stirring temperature is 40-50 ℃, the stirring speed is 150rpm/min, the centrifugal separation speed is 4000rpm/min, and the time is 10 min.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: adding water into the obtained filter residue, mixing the filter residue to 10-20%, stirring, and performing centrifugal separation, wherein the stirring temperature is room temperature, the stirring time is 10-20 minutes, the stirring speed is 150rpm/min, the centrifugal separation speed is 4000rpm/min, and the time is 10 minutes.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: the vegetable protein raw material is one or a composition of any more of soybean meal, peanut meal, corn meal and wheat meal.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: the decolorizing solution sequentially passes through pretreated anion exchange resin and cation exchange resin, wherein the anion exchange resin is D201 resin, and the cation exchange resin is 001x4 resin.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: the flow rate of the decolored solution passing through the anion exchange resin and the cation exchange resin is 100-200 mL/min.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: and concentrating the obtained filtrate with the salinity removed, and performing spray drying, wherein the concentration is performed until the solid content of the filtrate is 30%, the air inlet temperature of the spray drying is 170-190 ℃, and the air outlet temperature of the spray drying is 80-95 ℃.
As a preferred scheme of the preparation method of the high-quality food-grade plant source compound amino acid, the preparation method comprises the following steps: the high-quality food-grade plant source compound amino acid has the total nitrogen content of more than or equal to 13 percent, the amino acid nitrogen content of more than or equal to 9 percent, the chloride content of less than or equal to 1 percent, the ash content of less than or equal to 4 percent and the 3-chloropropanol content of less than or equal to 0.3 mg/kg.
The invention further aims to overcome the defects in the prior art and provide application of the high-quality food-grade plant source compound amino acid in food seasonings.
The invention has the beneficial effects that:
(1) the invention provides a preparation method of high-quality food-grade plant source compound amino acid, which comprises the steps of pretreating vegetable protein, removing impurities and purifying the protein; mixing the pretreated vegetable protein with hydrochloric acid, and performing acid hydrolysis; removing more than 80% of hydrochloric acid from the hydrolysate by a hydrogen chloride recovery device, and realizing the cyclic utilization of the hydrochloric acid; decolorizing the deacidification solution, and removing anions and cations by using anion exchange resin and cation exchange resin; concentrating and spray-drying the effluent to obtain the high-quality food-grade plant source compound amino acid. The invention has the advantages of simple preparation process, low energy consumption, low salt content in the product, short production period and high product quality. Compared with the traditional acid hydrolysis plant protein product, the salt content and the chloropropanol content are greatly reduced, and the development trend of low-salt health food is met. In the obtained high-quality food-grade plant source compound amino acid, the total nitrogen is more than or equal to 13 percent, the amino acid nitrogen is more than or equal to 9 percent, the chloride content is less than or equal to 1 percent, the ash content is less than or equal to 4 percent, and the 3-chloropropanol content is less than or equal to 0.3mg/kg, which is far higher than the industrial standard and the current commercial product.
(2) The high-quality food-grade plant-derived compound amino acid prepared by the invention has the advantages of outstanding delicate flavor, low salt content and extremely low salty taste, and can be widely applied to the field of low-salt foods; the high-quality food-grade plant source compound amino acid prepared by the invention has various amino acids and rich nutrition, and can be widely used in the fields of medicines, health products and agriculture; the preparation process is simple and feasible, and is suitable for industrial application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is a flow chart of a preparation process of high-quality food-grade plant-derived compound amino acid in the practice of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention more comprehensible, specific embodiments thereof are described in detail below with reference to examples of the specification.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Weighing 1kg of soybean meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 4kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, rotating speed to 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 2
Weighing 1kg of corn meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 4kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, rotating speed to 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid; (ii) a
After the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 3
Weighing 1kg of peanut meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 4kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, rotating speed to 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 4
Weighing 1kg of soybean meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 6kg of hydrochloric acid, mixing the filter residue with slurry, putting the mixture into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to be 108 ℃, the rotating speed to be 150rpm/min, reacting for 6 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 5
Weighing 1kg of soybean meal, and crushing to 60 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 4kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, rotating speed to 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 6
Weighing 1kg of soybean meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
adding 2kg of hydrochloric acid into the part of filter residue, mixing the filter residue with the slurry, putting the mixture into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to be 108 ℃, the rotating speed to be 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 7
Weighing 1kg of soybean meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 4kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, rotating speed to 150rpm/min, reacting for 20 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrogen chloride recovery device to obtain more than 80 percent hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 10g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, flowing a decolorizing solution through the D201 and 001x4 resin at a flow rate of 100mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 8
Weighing 1kg of soybean meal, and crushing to 120 meshes;
mixing with water to 10L;
adjusting pH to 9 with sodium hydroxide, stirring at 50 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filtrate;
adjusting pH of the filtrate to 4.5 with hydrochloric acid, stirring at 45 deg.C and 150rpm/min for 20 min, centrifuging at 4000rpm/min for 10min, and separating to obtain filter residue;
mixing the filter residue to 20%, stirring at normal temperature at 150rpm/min for 10 minutes, centrifuging at 4000rpm/min for 10 minutes, and separating to obtain filter residue;
taking the part of filter residue, adding 6kg of hydrochloric acid, mixing the filter residue with slurry, putting the mixture into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to be 108 ℃, the rotating speed to be 150rpm/min, reacting for 6 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, the hydrolysate is recycled by a hydrochloric acid recycling device to obtain more than 80% hydrochloric acid;
after the reaction liquid is cooled, discharging the feed liquid, and filtering the feed liquid to remove insoluble impurities;
adjusting the solid content of the filtrate to 10%, adding 20g of active carbon, stirring at 80 ℃ for 15 minutes, carrying out suction filtration to obtain filtrate, and repeating for 2 times to obtain a decolorized solution;
weighing 5kg of D201 and 001x4 resin respectively, pretreating, loading into a column, linking with a peristaltic pump, allowing a decolorized solution to flow through the D201 and 001x4 resin at a flow rate of 300mL/min in sequence, and removing salt;
receiving 001x4 resin effluent, and performing rotary concentration until the solid content is 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is the high-quality food-grade plant source composite amino acid. The technical indexes are shown in Table 1 after being measured by the national standard method.
Example 9
Weighing 1kg of soybean meal, and crushing to 120 meshes;
adding 6kg of hydrochloric acid, mixing, placing into a normal pressure reaction kettle, adjusting the temperature of the reaction kettle to 108 ℃, the rotating speed to 150rpm/min, reacting for 6 hours, and condensing and refluxing in the hydrolysis process;
after the reaction is finished, adding sodium hydroxide, and adjusting the pH value of the product to be between 5 and 6;
rotary concentrating to solid content of 30%;
spray drying the concentrated solution, wherein the specific conditions of the spray drying are as follows: the air inlet temperature is 170 ℃ and 190 ℃, the air outlet temperature is 80-95 ℃, and the obtained powdery product is a commercially available compound amino acid product. The technical indexes are shown in Table 1 after being measured by the national standard method.
TABLE 1 technical indexes of high-quality food-grade plant-derived compound amino acid products in examples 1 to 9
From examples 1-3, the invention is not limited by the type of protein raw materials, and high-quality food-grade plant source compound amino acid can be prepared from raw materials such as bean pulp, peanut pulp, corn pulp and the like by the technical scheme; comparing example 1 and example 5, it is known that incomplete pulverization can lead to incomplete dissolution of impurities or salts in the product, thereby affecting the ash content in the product; comparative examples 1 and 6 show that insufficient hydrochloric acid ratio during acid hydrolysis results in incomplete hydrolysis, low hydrolysis degree, and reduced amino acid content in the product; from example 8, it is known that too high a flow rate of the ion exchange resin affects the ion exchange effect, resulting in incomplete removal of impurities (significantly reduced total nitrogen and amino acid nitrogen contents, high chloride and ash contents) in the product.
From example 9 (a method for producing a plant-derived compound amino acid which is commercially available at present), it is understood that the plant-derived compound amino acid product produced by the ordinary acid hydrolysis method has a small amino acid content of 30% or less of that of the present invention, contains a large amount of chloride and ash, and has a serious excess (1mg/kg) in the content of 3-chloropropanol.
The sensory index evaluation criteria of the invention are shown in Table 2.
TABLE 2 sensory index evaluation criteria
Examples 1-9 sensory evaluation of high quality food grade plant-derived complex amino acids are shown in table 3.
Table 3 sensory evaluation of high quality food grade plant-derived complex amino acids in examples 1 to 9
As can be seen from tables 2 and 3, the invention can improve the color, taste and mouthfeel of the plant source compound amino acid, and the high-quality plant source compound amino acid product prepared by the invention has light color, prominent delicate flavor, little peculiar smell and low salty taste. The products prepared in examples 1 to 4 all have good sensory feel, and example 5 is slightly salty due to incomplete crushing and high salt content, so that the mouthfeel is affected; example 6 the addition ratio of hydrochloric acid is low, hydrolysis is incomplete, and the amino acid content is low, so that the delicate flavor is slightly low, and the taste is influenced; example 7 because the addition ratio of the activated carbon is small, the color of the product is slightly yellow due to incomplete decolorization, and the color of the product is influenced; in example 8, the removal of impurities is incomplete due to the over-high flow rate of the ion exchange resin, which affects the overall appearance; example 9 as a preparation process of a commercially available compound amino acid, the product process is simple and coarse, high in salt content, many in impurities, and poor in overall appearance. Therefore, the high-quality plant source compound amino acid product prepared by the invention has light color, prominent delicate fragrance, less peculiar smell and low salty taste through the synergistic effect of the processes. The high-quality food-grade plant source compound amino acid product prepared by the invention can be used as a freshener of low-salt food and can also be used as a nutritional supplement of health-care food.
Example 10
The application of the high-quality food-grade plant source compound amino acid in the cold dish seasoning is as follows: the components are compounded according to the weight ratio as follows: 10 parts of high-quality food-grade compound amino acid, 5 parts of yeast extract, 2 parts of nucleotide disodium, 20 parts of maltodextrin, 10 parts of cane sugar, 5 parts of salt and 100 parts of water. And (3) taking 5g to 500g of cucumber shreds from the blended sauce, uniformly stirring, and tasting the taste.
Example 11
The application of the common plant source compound amino acid in the cold vegetable sauce comprises the following steps: the components are compounded according to the weight ratio as follows: 10 parts of common plant source compound amino acid, 5 parts of yeast extract, 2 parts of nucleotide disodium, 20 parts of maltodextrin, 10 parts of cane sugar and 100 parts of water. And (3) taking 5g to 500g of cucumber shreds from the blended sauce, uniformly stirring, and tasting the taste.
TABLE 4 application of plant-derived compound amino acids in cold dish sauce
From examples 10 and 11, it is known that the taste of the common plant-derived compound amino acid product is affected due to the presence of a large amount of salt and impurities, other seasonings can be excessively salty even if the compound amino acid product is compounded without adding salt, and the burnt taste in the product affects the overall sense.
Example 12
The application of the high-quality food-grade plant source compound amino acid in the low-salt puffed food seasoning is as follows: 10 parts of high-quality food-grade plant source compound amino acid, 2 parts of yeast extract, 1 part of nucleotide disodium, 1 part of salt, 2 parts of sugar, 2 parts of chicken essence, 10 parts of starch and 1 part of anticaking agent.
The salt content of the common plant source compound amino acid product is more than 40%, the adding amount of the common plant source compound amino acid product is limited by salt in the subsequent use, 10 parts of compound amino acid is added, at least 4 parts of salt is added, the use is inconvenient, the high-quality food-grade plant source compound amino acid product not only solves the problem of salt limitation of the product, but also removes 3-chloropropanol and impurities, improves the safety and improves the taste.
The prepared plant source compound amino acid product with high purity, low salt content, fresh fragrance and good taste can not only solve the problems of high salt content, more impurities and low safety of the plant source compound amino acid product produced by the prior acid hydrolysis process, but also can reduce the dosage of the plant source compound amino acid under the condition of freshness, reduce the salt content and expand the application field of the product. Under the condition of equal freshness, the same delicate flavor effect is achieved, and the addition amount of the product is less; the product can also be used as a freshness-enhancing component of low-salt food. Therefore, the preparation of the high-quality plant source compound amino acid product has great significance.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A preparation method of high-quality food-grade plant source compound amino acid is characterized by comprising the following steps: comprises the steps of (a) preparing a mixture of a plurality of raw materials,
crushing a vegetable protein raw material, sieving the crushed vegetable protein raw material by 120-140 meshes, and mixing the crushed raw material with water to obtain a mixed material liquid, wherein the mixed material liquid is 10-20%;
adjusting the pH of the slurry-mixed feed liquid to 9-10 by using sodium hydroxide, stirring for 20-30 minutes, performing centrifugal separation to obtain a filtrate, adding hydrochloric acid into the filtrate, adjusting the pH to 4-5, stirring for 20-30 minutes, and performing centrifugal separation to obtain filter residues;
adding water into the obtained filter residue, mixing the obtained filter residue with the water to 10-20%, stirring, and performing centrifugal separation to obtain filter residue separated after mixing, wherein the filter residue is prepared from the following plant protein raw materials: mixing filter residues separated after size mixing with hydrochloric acid according to the mass ratio of 1: 4-6, hydrolyzing at 105-110 ℃ for 6-24 hours under normal pressure to obtain a feed liquid, performing suction filtration to remove insoluble impurities, adjusting the obtained filtrate to the solid content of 10-20%, adding 4-6% of activated carbon, stirring for 15-30 minutes, performing suction filtration to obtain a filtrate, and repeating the steps for 2 times to obtain a decolorized solution;
sequentially passing the decolorized solution through pretreated anion exchange resin and cation exchange resin to remove salt;
and concentrating the obtained desalted filtrate, and performing spray drying to obtain a powdery product, namely the high-quality food-grade plant source compound amino acid.
2. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: and after stirring for 20-30 minutes, performing centrifugal separation to obtain a filtrate, wherein the stirring temperature is 45-55 ℃, the stirring rotating speed is 150rpm/min, the centrifugal separation rotating speed is 4000rpm/min, and the time is 10 min.
3. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: and adjusting the pH value to 4-5, stirring for 20-30 minutes, and performing centrifugal separation to obtain filter residues, wherein the stirring temperature is 40-50 ℃, the stirring speed is 150rpm/min, the centrifugal separation speed is 4000rpm/min, and the time is 10 min.
4. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: adding water into the obtained filter residue, mixing the filter residue to 10-20%, stirring, and performing centrifugal separation, wherein the stirring temperature is room temperature, the stirring time is 10-20 minutes, the stirring speed is 150rpm/min, the centrifugal separation speed is 4000rpm/min, and the time is 10 minutes.
5. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: the vegetable protein raw material is one or a composition of any more of soybean meal, peanut meal, corn meal and wheat meal.
6. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: the decolorizing solution sequentially passes through pretreated anion exchange resin and cation exchange resin, wherein the anion exchange resin is D201 resin, and the cation exchange resin is 001x4 resin.
7. The method for preparing high-quality food-grade plant-derived compound amino acids according to claim 6, wherein the method comprises the following steps: the flow rate of the decolored solution passing through the anion exchange resin and the cation exchange resin is 100-200 mL/min.
8. The method for preparing high-quality food-grade plant-derived compound amino acid according to claim 1, wherein the method comprises the following steps: and concentrating the obtained filtrate with the salinity removed, and performing spray drying, wherein the concentration is performed until the solid content of the filtrate is 30%, the air inlet temperature of the spray drying is 170-190 ℃, and the air outlet temperature of the spray drying is 80-95 ℃.
9. The method for preparing high-quality food-grade plant-derived compound amino acid according to any one of claims 1 to 8, wherein the method comprises the following steps: the high-quality food-grade plant source compound amino acid has the total nitrogen content of more than or equal to 13 percent, the amino acid nitrogen content of more than or equal to 9 percent, the chloride content of less than or equal to 1 percent, the ash content of less than or equal to 4 percent and the 3-chloropropanol content of less than or equal to 0.3 mg/kg.
10. Use of the high quality food grade plant-derived complex amino acid of claim 9 in food flavoring.
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