CN117223862A

CN117223862A - High-expansion-ratio algae dietary fiber slow-release capsule and preparation method and application thereof

Info

Publication number: CN117223862A
Application number: CN202311247342.9A
Authority: CN
Inventors: 赵孟冬; 赵楠
Original assignee: Tangshan Caofeidian Hengrui Marine Biotechnology Industry Co ltd
Current assignee: Tangshan Caofeidian Hengrui Marine Biotechnology Industry Co ltd
Priority date: 2023-09-26
Filing date: 2023-09-26
Publication date: 2023-12-15

Abstract

The invention relates to a high-expansion-rate algae dietary fiber slow-release capsule and a preparation method and application thereof, wherein the slow-release capsule comprises a core material and a wall material, and the mass ratio of the core material to the wall material is 1: (1-3); the core material comprises 15-25 parts of probiotics, 5-15 parts of carboxymethyl cellulose and 5-10 parts of chitosan by mass; the wall material comprises 20-30 parts of algae dietary fiber and 10-20 parts of resistant dextrin, wherein the core material forms a self-assembled coating layer on the surface of the probiotics through electrostatic adsorption of carboxymethyl cellulose and chitosan; the expansion force of the alga dietary fiber is more than 100mL/g, and the water holding capacity is more than 10000%; the core material and the wall material are prepared into the sustained-release capsule by negative pressure low-temperature spray drying. The wall material algae dietary fiber and the resistant dextrin of the slow-release capsule have good taste, increase satiety, and are beneficial to intestinal peristalsis and promote intestinal health by combining core probiotics released by intestinal positioning.

Description

High-expansion-ratio algae dietary fiber slow-release capsule and preparation method and application thereof

Technical Field

The invention belongs to the technical field of extraction and application of alga dietary fibers, and particularly relates to a high-expansion-rate alga dietary fiber slow-release capsule, and a preparation method and application thereof.

Background

The dietary fiber is called as 'scavenger of human body', can promote discharge of cholic acid and neutral steroid, reduce cholesterol, relieve constipation, increase satiety, facilitate toxin expelling and skin caring of human body, prevent constipation, delay carbohydrate absorption, and control blood sugar. Seaweed type foods have extremely high dietary fiber content and minerals such as calcium, iron, sodium, magnesium, phosphorus, iodine and the like, and widely comprise: hair weeds, laver, kelp, sea lettuce, undaria pinnatifida and the like. The seaweed dietary fiber has excellent water holding capacity, expansibility and adsorption capacity to saturated and unsaturated fat, is rich in algin, cellulose, hemicellulose, vitamins, minerals and the like, has quite high content of soluble polysaccharide, and is a high-quality raw material for extracting high-activity dietary fiber. The seaweed dietary fiber has the functions of relaxing bowels, resisting and preventing cancer, preventing cardiovascular and cerebrovascular diseases, reducing weight, reducing blood sugar and the like. The seaweed dietary fiber contains a large amount of calcium, so that the calcium demand of a human body can be supplemented, and side chain groups such as hydroxyl groups or carboxyl groups in the dietary fiber can be embedded, and the groups are prevented from affecting the metabolism balance of minerals in the intestinal tract of the human body.

The yield and scale of kelp planting in China are the first world, and the yield of kelp dried products in 2009 reaches 6.0X10 ⁵ t, which accounts for more than 50% of the total world yield. In addition to being used for direct eating, kelp is one of the main raw materials of brown algae industry. In China, kelp processing currently forms an industrial system which takes algin, mannitol and iodine as main products. But the product has high production cost and increasingly severe environmental protection pressure due to low added value, large water consumption, large energy consumption, serious pollution and large proportion of waste in the production process. On the other hand, with the increasing living standard of people, fine foods are gradually increased, meat and vegetable foods are gradually unbalanced, the intake of dietary fiber is gradually reduced, and civilization diseases caused by unbalanced diet, such as obesity, hypertension and sugarUropathy and the like are common, and the situation is particularly serious in coastal cities with developed economy. Therefore, how to obtain the alga dietary fiber with high quality, high efficiency and low pollution, maintain the bioactivity of the alga dietary fiber, play a role in metabolism and health care, and become one of the research hot spots of dietary fiber functional foods and medicines.

Patent CN110074418B discloses a method for extracting seaweed dietary fiber, which comprises the steps of firstly carrying out steam explosion wall pretreatment on seaweed, and then sequentially carrying out enzymolysis, acid-base treatment and deodorization, activation and extraction for three times to obtain the seaweed dietary fiber. The seaweed dietary fiber is extracted by a method of combining a chemical reagent and an enzyme reagent, the dietary fiber extraction rate is high (up to 41.77%), the expansion force (up to 278.90 mL/g) and the water holding capacity (up to 11892.69%) are high, and no fishy smell exists. The dietary fiber has good physiological functions, and is helpful for intestinal peristalsis, carbohydrate and lipid metabolism, etc. The invention focuses on the extraction method of the seaweed dietary fiber, does not relate to the protection, synergistic effect and the like of the dietary fiber in the application process, has relatively single material, and is difficult to meet the actual use requirement.

Patent CN114931562a discloses a microcapsule delivery system based on insoluble dietary fiber, wherein the microcapsule is prepared by a microfluidic technology, and comprises a microcapsule wall material and a microcapsule core material, wherein the wall material consists of sodium alginate and insoluble dietary fiber, the core material consists of core components, and the core components are probiotics, functional components of health products, medicines, functional factors of foods and other substances suitable for embedding. The kelp nanocellulose-based microcapsule keeps good sphericity in the stomach, obviously improves the protection of core components, can quickly release the core components in the intestinal tract, and plays a good gastrointestinal slow-release function. The microcapsule prepared by the invention has the particle size below 500 mu m, good monodispersity, simple and convenient preparation method operation and low cost. The microcapsule structure is introduced in the patent, and the sodium alginate and the insoluble dietary fiber wall material are utilized to play a good gastrointestinal slow-release function on the inner probiotics, however, the product is difficult to provide satiety in the stomach due to the limitation of the insoluble dietary fiber, and the wall material still can be disintegrated to a certain extent under the action of gastric acid dissolution and swelling due to the relatively simple coating components and structure, so that the inactivation risk of the inner probiotics exists.

Therefore, the composition and the structure are provided to reasonably utilize the algae dietary fiber and other active substances, thereby achieving the effects of providing satiety in the stomach, promoting intestinal health and the like.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a high-expansion-rate alga dietary fiber slow-release capsule, and a preparation method and application thereof. The carboxymethyl cellulose-chitosan self-assembled coating layer is formed on the surface of the probiotics by utilizing the electrostatic adsorption effect, so that a core material which can be used for realizing gastrointestinal slow release and intestinal positioning release is provided, and then the wall material containing the algae dietary fiber, the resistant dextrin and the carboxymethyl cellulose is stably coated outside the core material, so that long-term and obvious satiety is provided.

In a first aspect, the invention provides a high-expansion-rate algae dietary fiber slow-release capsule, which comprises a core material and a wall material, wherein the mass ratio of the core material to the wall material is 1: (1-3);

the core material comprises the following components in parts by mass:

15-25 parts of probiotics

5-15 parts of carboxymethyl cellulose

5-10 parts of chitosan;

the wall material comprises the following components:

20-30 parts of algae dietary fiber

10-20 parts of resistant dextrin;

the core material forms a self-assembled coating layer on the surface of the probiotics through electrostatic adsorption of carboxymethyl cellulose and chitosan;

the expansion force of the alga dietary fiber is more than 100mL/g, and the water holding capacity is more than 10000%;

the core material and the wall material are prepared into the sustained-release capsule by negative pressure low-temperature spray drying.

The chitosan serving as a carrier can stabilize the core material component, promote the absorption of the core material, delay or control the dissolution rate, help the core material to reach target organs and prevent the irritation to the stomach. The chitosan microsphere surface is rich in polysaccharide chains, can be identified by specific cells or tissues, and can be stored and released from targeted delivery core materials to target positions; the drug release of the chitosan drug-loaded microsphere is related to the molecular weight of chitosan, the release rate of the core material generally decreases along with the increase of the molecular weight of chitosan, and the higher the concentration of chitosan is, the lower the diffusion rate of the core material from the chitosan into the biological medium is.

Carboxymethyl cellulose is a low cost and readily available anionic cellulose derivative commonly used in food processing, COO ^- NH with chitosan ³⁺ The high-strength electrostatic coating structure has a strong electrostatic effect, can be self-assembled into a stable layered coating structure, has good barrier property to oil and water, and has a lasting protective effect to an internal core material. In practical application, when the product is matched with water, beverage and other carriers or is matched with other substances, the core material protected by the self-assembled coating layer has better stability, and the core material is not deactivated and invalid due to rapid disintegration of the structure, so that the self-assembled coating layer has better application value.

Specifically preferred, chitosan has a viscosity average molecular weight of 500-1000KD and a deacetylation degree of 70-95%; the viscosity average molecular weight of the carboxymethyl cellulose is 15000-25000KD, and the substitution degree is higher than 55%.

According to the invention, the algae dietary fiber is used in the wall material, and through reasonable treatment, the dietary fiber with the swelling power of more than 100mL/g, preferably more than 120mL/g, more preferably more than 150mL/g, the water holding capacity of more than 10000%, preferably more than 11000%, more preferably more than 12000% can be obtained, so that the algae dietary fiber has a good swelling effect, can provide remarkable satiety, and retains the nutrition components and activity of the algae dietary fiber.

In the invention, besides the algae dietary fiber, another dietary fiber and resistant dextrin are added into the wall material. The resistant dextrin is low-calorie glucan, can be fermented into short-chain fatty acids by human digestive tract microorganisms, and the short-chain fatty acids can increase satiety, reduce food intake of people and are beneficial to achieving the effect of controlling weight. Resistant dextrins become dextrins after entering the human digestive system, which have slower digestion rates and can delay digestion and absorption of carbohydrates, thereby reducing the glycemic response. Then fermented by intestinal microorganisms to produce short chain fatty acid to promote intestinal health.

Preferably, the probiotics are at least one selected from streptococcus thermophilus, lactobacillus bulgaricus, lactobacillus acidophilus, lactobacillus casei, bifidobacterium, lactobacillus brevis and lactobacillus plantarum. Preferably, the viable count of the probiotics is more than or equal to 5 multiplied by 10 ⁹ CFU/ml, more preferably the probiotic is formulated, for example streptococcus thermophilus is formulated with lactobacillus bulgaricus.

Preferably, the algal dietary fiber is prepared by the steps of:

(1) Pretreatment: soaking algae raw materials in water, cleaning, crushing, and mixing with water to obtain algae jam;

(2) Enzymolysis: adding complex enzyme into the algae jam, and cooling after enzymolysis to obtain an enzymolysis material;

(3) Acid-base treatment: adding hydrochloric acid into the enzymolysis material to adjust the pH to 2-4, and filtering to collect filter residues; washing the residue to remove Cl ^- Draining, adding into sodium carbonate aqueous solution for reaction, cooling, and adding hydrochloric acid for neutralization until the pH value is 6-7;

(4) And (3) gelation treatment: adding a calcium chloride solution, performing gel, filtering, collecting filter residues, and washing to obtain a crude product containing water;

(5) Removing fishy smell: adding the water-containing crude product into 1-6w/v% yeast water solution, preferably 4-6w/v%, stirring at 20-30deg.C for 20-60min, centrifuging, washing, filtering, and collecting fishy smell removing residue;

(6) Activating the fishy smell removed filter residues by using a sodium chloride solution to obtain an activated crude product;

(7) Freeze-drying the activated crude product, and crushing to obtain the alga dietary fiber.

The invention adopts multistage enzymolysis to gently remove impurities such as protein, starch, fat and the like. The deodorization and deodorization treatment of the seaweed dietary fiber has great influence on the use experience of users, the invention adopts a yeast deodorization mode, ensures that the seaweed nutrient components are not damaged, and the yeast can be reused after being separated. The acid-base treatment process can fully remove impurities such as protein, fat and the like, and the dietary fiber is extracted to the maximum extent. The calcium chloride is added in the early extraction process, so that the loss of dietary fiber and the operation convenience are reduced, but the activity of the dietary fiber is easily reduced, and therefore, the sodium chloride is used for performing functional activation treatment in the subsequent process, so that the extraction rate and the activity of the seaweed dietary fiber are both considered.

Preferably, in the step (2), the enzymolysis process of the complex enzyme includes:

(2.1) adding yeast aqueous solution into the algae paste, and keeping the temperature at 25-35 ℃ for 2-5h;

(2.2) adding aqueous solution of cellulase, heating at a speed of 1-3 ℃/min, and keeping the temperature at 50+/-2 ℃ under stirring for enzymolysis for 1-2h;

(2.3) adding aqueous protease solution, heating to 55+ -1deg.C at a speed of 0.5-1deg.C/min, then maintaining the temperature at 50+ -2deg.C under stirring for enzymolysis for 1-2h, and cooling to 35+ -2deg.C.

The enzymolysis process adopts a graded enzymolysis and gradual heating mode, so that the enzymolysis can be performed more gently and controllably.

Preferably, the freeze-drying is carried out at a freezing temperature of-60 ℃ to-40 ℃ and a vacuum degree of 10 to 50Pa, and the algae dietary fiber is crushed to 2-30 mu m; in the particle size distribution obtained by the laser diffraction scattering method, the average particle diameter D50 is preferably 5 to 20 μm, the particle diameter D10 having a cumulative frequency of 10% from the small particle diameter side is preferably 2 to 8 μm, and Dx represented by dx= (D50-D10)/D50 is preferably in the range of 0.4 to 0.8 inclusive, thereby achieving a combination of low loss rate, high expansion force, high water holding capacity, and the like of the fiber.

The freeze drying is combined with low-temperature crushing, liquid nitrogen is used as a cold source, the material to be crushed is frozen and embrittled at low temperature, meanwhile, water is sublimated and discharged by vacuumizing, the material with loose and fragile structure directly enters a crushing cavity of the low-temperature crusher and rotates at high speed through an impeller, and the material and the blade, the fluted disc and the material repeatedly impact, collide, shear, rub and other comprehensive effects are achieved, so that the crushing effect is achieved. The particle size distribution range of the crushed powder is narrower, the specific surface area of the powder is large, the water holding capacity and the expansion capacity of the dietary fiber are improved, the uniformity of the dietary fiber is better, and meanwhile, the structure of the dietary fiber is more loose.

Preferably, the core material is prepared by the steps of:

step one: spraying carboxymethyl cellulose water solution onto probiotics, and drying with hot air to obtain a coating coated with carboxymethyl cellulose; in order to completely coat the probiotics with carboxymethyl cellulose, spraying is preferably carried out for 2-5 times, and the probiotics are stirred after each spraying;

step two: adding the coating into chitosan solution, oscillating for reaction, forming a chitosan self-assembly layer on the surface of the coating through electrostatic adsorption of carboxymethyl cellulose and chitosan, filtering and drying to obtain the core material.

Preferably, the steps one to two can be repeatedly carried out for 1 to 3 times to obtain 2 to 4 groups of self-assembled composite layers, and when the coating is added into the chitosan solution for the last time, along with the oscillating reaction, sodium tripolyphosphate solution is slowly added to crosslink the outermost chitosan, and the mass ratio of the sodium tripolyphosphate to the outermost chitosan is 1: (40-60).

The sodium tripolyphosphate molecule contains a plurality of negative-charge phosphate ions, the chitosan molecule contains a plurality of amino cations, hydroxyl and other functional groups, the phosphate ions and the amino cations perform electrostatic interaction to generate a structure of crosslinking of one phosphate ion and two or three amino cations, and a crosslinked network structure formed by a plurality of sodium tripolyphosphates and chitosan is formed. The crosslinked product of chitosan and sodium tripolyphosphate has good biocompatibility and biodegradability.

The invention provides a preparation method of a high-expansion-rate algae dietary fiber slow-release capsule, which is characterized by comprising the following steps of:

s1, preparing a core material:

s1.1, preparing a carboxymethyl cellulose water solution with the concentration of 1-10w/v%, and preheating probiotics in a coating pot; spraying the carboxymethyl cellulose aqueous solution onto probiotics, and carrying out hot air drying, wherein spraying and hot air drying are alternately carried out to obtain a coating coated with carboxymethyl cellulose;

s1.2, dissolving chitosan in acetic acid aqueous solution with the concentration of 1-2wt% to obtain chitosan solution with the concentration of 1-3w/v%, adding a coating into the chitosan solution, carrying out oscillation reaction, filtering and drying to obtain a core material;

s2, preparing a slow-release capsule by a negative pressure low-temperature spray drying method:

s2.1, adding the wall material raw material into deionized water at 60-80 ℃, stirring to obtain a wall material solution, and cooling to room temperature;

s2.2, adding the core material into the wall material solution, and homogenizing at high speed and/or pressurizing and homogenizing;

s2.3, atomizing the material homogenized in the step S2.2 in a negative pressure drying cavity, simultaneously introducing drying gas, wherein the vacuum degree in the drying cavity is-0.1 to-0.01 Mpa, the air inlet temperature of the drying cavity is 30-45 ℃, and the air outlet temperature is 20-35 ℃.

Preferably, the wall material also comprises carboxymethyl cellulose, and the dosage of the carboxymethyl cellulose is 20-30% of the total mass of the algae dietary fiber and the resistant dextrin.

The third aspect of the invention provides application of the high-expansion-rate alga dietary fiber slow-release capsule in foods and medicines.

The invention has the advantages that:

(1) The high-nutrition high-activity algae dietary fiber with the grain diameter of 2-30 mu m, preferably the average grain diameter D50 of 5-20 mu m, the average grain diameter D10 of 2-8 mu m, the Dx expressed by Dx= (D50-D10)/D50 of more than 0.4 and less than 0.8 is prepared by adopting the process links of pretreatment, enzymolysis, acid-base treatment, activation treatment, freeze drying, low-temperature crushing and the like, the distribution range is narrow, the specific surface area of powder is large, the expansion force is more than 100mL/g, preferably more than 120mL/g, more preferably more than 150mL/g, the water holding capacity is more than 10000%, preferably more than 11000%, more preferably more than 12000%. In addition, the wall material is also matched with resistant dextrin, the resistant dextrin cannot be digested and absorbed in the digestive tract, so that the feeling of satiety is further enhanced, the resistant dextrin enters the intestinal tract, and the resistant dextrin also plays a role in the intestinal tract as dietary fiber.

(2) By utilizing the self-assembly characteristic of chitosan and carboxymethyl cellulose, a carboxymethyl cellulose coating layer is formed outside the probiotics, chitosan is further coated outside the carboxymethyl cellulose, and alternating layers of the chitosan and the carboxymethyl cellulose can be formed according to the requirement, so that stable and durable protection is formed for the probiotics. In addition, after the carboxymethyl cellulose component is added into the wall material, the dietary fiber is more beneficial to being driven to wrap around the core material due to the electrostatic effect of the carboxymethyl cellulose and the chitosan in the process of coating the core material by the wall material. The slow-release capsule disclosed by the invention has various beneficial components, including composite dietary fibers, so as to be a material combination of probiotics and the like beneficial to intestinal health.

Drawings

FIG. 1 is a schematic diagram of the structure of a high expansion rate algae dietary fiber slow release capsule of the present invention;

figure 2 is a satiety profile for samples of the examples and comparative examples.

Reference numerals illustrate: 1. core material, 2. Carboxymethyl cellulose layer, 3. Chitosan layer, 4. Wall material.

Detailed Description

The present invention will be described in further detail below in order to make the objects, technical solutions and advantages of the present invention more apparent. Unless otherwise indicated, all reagents used in the detailed description and examples were commercially available.

The high-expansion-ratio algae dietary fiber slow-release capsule can be used in various fields of foods, medicines and the like, and comprises a core material 1 and a wall material 4, wherein the mass ratio of the core material 1 to the wall material 4 is 1: (1-3);

(1) The core material 1 comprises the following components in parts by mass:

15-25 parts of probiotics

5-15 parts of carboxymethyl cellulose

5-10 parts of chitosan;

the probiotics are at least one selected from Streptococcus thermophilus, lactobacillus bulgaricus, lactobacillus acidophilus, lactobacillus casei, bacillus bifidus, lactobacillus brevis and Lactobacillus plantarum, and the viable count of the probiotics is not less than 5×10 ⁹ CFU/ml。

The core material 1 forms self-assembled coating layers (2, 3) on the surface of the probiotics through electrostatic adsorption of carboxymethyl cellulose and chitosan, and referring to fig. 1, the self-assembled coating layers comprise carboxymethyl cellulose layers 2 and chitosan layers 3, and the two layers can continue to be thickened alternately, for example, self-assembled composite layers of 2-4 groups or more are formed, but the outermost layer is preferably the chitosan layer 3, so that the later intestinal targeting positioning effect is facilitated, and the bonding effect with wall materials is improved;

(2) The wall material 4 comprises the following components in parts by mass:

20-30 parts of algae dietary fiber

10-20 parts of resistant dextrin

The optional carboxymethyl cellulose is used in an amount of 20-30% of the total mass of the algae dietary fiber and the resistant dextrin, and the carboxymethyl cellulose is used in the wall material, so that the wall material 4 and the outermost chitosan layer 3 of the core material 1 are better in electrostatic combination.

The expansion force of the alga dietary fiber is more than 100mL/g, preferably more than 120mL/g, more preferably more than 150mL/g; the water holding capacity is greater than 10000%, preferably greater than 11000%.

The preparation method of the high-expansion-rate algae dietary fiber slow-release capsule comprises the following steps:

s1, preparing a core material 1:

s1.1, preparing a carboxymethyl cellulose aqueous solution with the concentration of 1-10w/v%, preheating probiotics in a coating pot at the preheating temperature of 30-40 ℃ and the rotating speed of the coating pot of 10-40r/min; spraying carboxymethyl cellulose water solution onto probiotics at the spraying pressure of 1-5kg/cm ² Hot air drying at 35-50deg.C, spraying and hot air drying alternately to obtain coated product coated with carboxymethyl cellulose layer 2;

s1.2, dissolving chitosan in acetic acid aqueous solution with the concentration of 1-2wt% to obtain chitosan solution with the concentration of 1-3w/v%, adding a coating into the chitosan solution, carrying out oscillation reaction, filtering and drying to obtain a core material coated with a chitosan layer 3;

wherein, the steps S1.1 to S1.2 can be repeatedly carried out for 1 to 3 times, and when the coating is added into the chitosan solution for the last time, along with the oscillating reaction, sodium tripolyphosphate solution is slowly added to carry out light crosslinking on the outermost chitosan layer, and the mass ratio of the sodium tripolyphosphate to the outermost chitosan is 1: (40-60).

S2, preparing a slow-release capsule by using the core material 1 and the wall material 4 through a negative pressure low temperature spray drying method:

s2.1, adding the wall material raw material into deionized water at 60-80 ℃, stirring to obtain a wall material solution, and cooling to room temperature; the wall material comprises algae dietary fiber and resistant dextrin, and optionally carboxymethyl cellulose, wherein the dosage of the carboxymethyl cellulose is 20-30% of the total mass of the algae dietary fiber and the resistant dextrin; the adding sequence is preferably to add carboxymethyl cellulose firstly for dissolution, then add algae dietary fiber and resistant dextrin, and stir and mix.

Wherein the algae dietary fiber is prepared by the following steps:

(2) Enzymolysis: adding complex enzyme into the algae jam, and cooling after enzymolysis to obtain an enzymolysis material; has the following steps:

(2.1) adding 1-5w/v% yeast aqueous solution into the algae jam, and maintaining the temperature at 25-35 ℃ for 2-5h;

(2.2) adding aqueous solution of cellulase, heating at a speed of 1-3 ℃/min, and keeping the temperature at 50+/-2 ℃ under stirring for enzymolysis for 1-2h; the dosage of the cellulase is 0.01-0.03% of the mass of the algae jam, and the activity of the cellulase is 80-120U/g;

(2.3) adding protease aqueous solution, heating to 55+/-1 ℃ at the speed of 0.5-1 ℃/min, then keeping the temperature at 50+/-2 ℃ for enzymolysis for 1-2h under stirring, and cooling to 35+/-2 ℃; the amount of protease is 0.1-0.3% of the mass of the algae jam, and the protease activity is 1800-2200U/g.

(5) Removing fishy smell: adding 1-6w/v% yeast water solution into the water-containing crude product, stirring at 20-30deg.C for 20-60min, centrifuging, washing, filtering, and collecting fishy smell removed filter residue;

(7) The activated crude product is freeze-dried at a freeze temperature of-60 ℃ to-40 ℃ and a vacuum degree of 10 to 50Pa, and the algal dietary fiber is crushed to 2 to 30 μm, preferably, in a particle size distribution obtained by a laser diffraction scattering method, an average particle diameter D50 is 5 to 20 μm, a particle diameter D10 having a cumulative frequency of 10% from the small particle diameter side is 2 to 8 μm, and Dx expressed by Dx= (D50-D10)/D50 is in a range of 0.4 or more and 0.8 or less.

S2.2, adding the core material 1 into the wall material solution, and homogenizing at a high speed and/or homogenizing under pressure; wherein the rotation speed of the high-speed homogenization is 10000-20000rpm, and the time of the high-speed homogenization is 1-3 minutes; the rotation speed of the pressurizing homogenization is 8000-15000r/min, and the homogenization is carried out for 1-3 times under 40-50 MPa;

s2.3 atomizing the homogenized material in the step S2.2 in a negative pressure drying cavity, and simultaneously introducing drying gas, wherein the vacuum degree in the drying cavity is-0.1 to-0.01 Mpa, the air inlet temperature of the drying cavity is 30-45 ℃, and the air outlet temperature is 20-35 ℃, so as to prepare the high-expansion-rate alga dietary fiber slow-release capsule with the particle size of 50-500 mu m, preferably 100-300 mu m.

Aiming at the preparation and performance test of algae dietary fibers, the invention provides preparation examples 1-3 and comparative examples 1-3; and the high expansion rate alga dietary fiber is selected to prepare the sustained-release capsules, so that examples 1-3 and comparative examples 1-2 are obtained to compare the relevant performances of the sustained-release capsules.

Preparation example 1

The preparation example relates to a preparation method of seaweed dietary fiber, which comprises the following steps:

(2) Enzymolysis: adding complex enzyme into the algae jam, and cooling after enzymolysis to obtain an enzymolysis material; the method specifically comprises the following steps:

(2.1) adding 3w/v% yeast aqueous solution into the algae jam, and maintaining the temperature at 25 ℃ for 3 hours;

(2.2) adding aqueous solution of cellulase, heating at a speed of 3 ℃/min, maintaining the temperature at 50 ℃ under stirring, and carrying out enzymolysis for 1h; the consumption of the cellulase is 0.017% of the mass of the algae jam, and the activity of the cellulase is 100U/g;

(2.3) adding protease aqueous solution, heating to 55 ℃ at a speed of 1 ℃/min, then keeping the temperature at 50 ℃ for enzymolysis for 1h under stirring, and cooling to 35 ℃; the amount of protease is 0.15% of the mass of the algae jam, and the protease activity is 2000U/g.

(3) Acid-base treatment: adding hydrochloric acid into the enzymolysis material to adjust the pH value to 3, and filtering and collecting filter residues; washing the residue to remove Cl ^- Draining, adding into sodium carbonate aqueous solution for reaction, cooling, and adding hydrochloric acid for neutralization until the pH value is 7;

(5) Removing fishy smell: adding the water-containing crude product into 4w/v% yeast water solution, stirring at 25deg.C for 30min, centrifuging, washing, filtering, and collecting the fishy smell removed filter residue;

(7) Freeze drying the activated crude product at-45deg.C under vacuum degree of 40Pa, and directly crushing at low temperature to obtain particle diameter D ₅₀ Algae dietary fiber at 18.6 μm and D10 at 5.8 μm with Dx of about 0.69.

Preparation example 2

(2.1) adding 3w/v% yeast aqueous solution into the algae jam, and keeping the temperature at 35 ℃ for 2 hours;

(2.2) adding aqueous solution of cellulase, heating at a speed of 2 ℃/min, maintaining the temperature at 50 ℃ under stirring, and carrying out enzymolysis for 2h; the consumption of the cellulase is 0.017% of the mass of the algae jam, and the activity of the cellulase is 100U/g;

(2.3) adding protease aqueous solution, heating to 55 ℃ at a speed of 1 ℃/min, then keeping the temperature at 50 ℃ for enzymolysis for 2 hours under stirring, and cooling to 35 ℃; the amount of protease is 0.15% of the mass of the algae jam, and the protease activity is 2000U/g.

(5) Removing fishy smell: adding the water-containing crude product into 5w/v% yeast water solution, stirring at 25deg.C for 40min, centrifuging, washing, filtering, and collecting the fishy smell removed filter residue;

(7) Freeze drying the activated crude product at-50deg.C under vacuum degree of 30Pa, and directly crushing at low temperature to obtain particle diameter D ₅₀ Algae dietary fiber at 8.6 μm and D10 at 4.7 μm with Dx of about 0.45.

Preparation example 3

(2.1) adding 5w/v% yeast aqueous solution into the algae jam, and keeping the temperature at 30 ℃ for 4 hours;

(2.2) adding aqueous solution of cellulase, heating at a speed of 1.5 ℃/min, and keeping the temperature at 50 ℃ under stirring for enzymolysis for 1.5h; the consumption of the cellulase is 0.017% of the mass of the algae jam, and the activity of the cellulase is 100U/g;

(2.3) adding aqueous protease solution, heating to 55 ℃ at the speed of 0.5 ℃/min, then keeping the temperature at 50 ℃ for enzymolysis for 1.5h under stirring, and cooling to 35 ℃; the amount of protease is 0.15% of the mass of the algae jam, and the protease activity is 2000U/g.

(3) Acid-base treatment: adding hydrochloric acid into the enzymolysis material to adjust the pH value to 3, and filtering and collecting filter residues; washing filter residues to remove Cl-, draining, adding the filter residues into a sodium carbonate aqueous solution for reaction, cooling, and adding hydrochloric acid for neutralization until the pH value is 7;

(5) Removing fishy smell: adding the water-containing crude product into 6w/v% yeast water solution, stirring at 25deg.C for 50min, centrifuging, washing, and filtering to collect fishy smell-removed residues;

(7) Freeze drying the activated crude product at-55deg.C under vacuum degree of 20Pa, and directly crushing at low temperature to obtain particle diameter D ₅₀ Algae dietary fiber at 12.2 μm and D10 at 5.1 μm with Dx of about 0.58.

Comparative example 1

The comparative example differs from preparation example 3 in that the deodorization of step (5) was omitted and the aqueous crude product obtained by gelation treatment of step (4) was directly subjected to sodium chloride activation treatment, freeze-drying and low-temperature crushing.

Comparative example 2

The difference between the comparative example and the preparation example 3 is that the enzymolysis process in the step (2) is different, and specifically includes: adding aqueous solution of cellulase and aqueous solution of protease, heating at a speed of 3 ℃/min, maintaining the temperature at 50 ℃ under stirring, performing enzymolysis for 2h, and cooling to 35 ℃; the dosage of the cellulase is 0.017% of the mass of the algae paste, the activity of the cellulase is 100U/g, the dosage of the protease is 0.15% of the mass of the algae paste, and the activity of the protease is 2000U/g.

Comparative example 3

The comparative example differs from preparation example 3 in that the conventional dry crushing method is used instead of step (7) to obtain the particle size D ₅₀ Algae dietary fiber at 33.6 μm and D10 at 3.5 μm with Dx of about 0.90.

The algal dietary fiber samples obtained in preparation examples 1 to 3 and comparative examples 1 to 3 were subjected to measurement of yield, water holding capacity, swelling power and odor, and the results are shown in Table 1.

Yield (%) = total dietary fiber content in sample/dry weight of seaweed x 100%

Water holding capacity (%) = (wet weight of sample-dry weight of sample)/dry weight of sample x 100%

Swelling force (mL/g) = (dietary fiber volume after swelling with water-dry powder sample volume)/dry sample weight x 100%.

TABLE 1 results of measurement of the yields, water holding power, swelling power and odor of the samples

	Yield/%	Water holding capacity/%	Expansion force/mL/g	Smell scoring
					Preparation example 1	47.98	11795	169	2
Preparation example 2	48.46	11828	173	1
					Preparation example 3	49.38	12028	186	0
Comparative example 1	47.94	9882	151	8
					Comparative example 2	45.46	6062	78	6
Comparative example 3	42.75	5896	66	3

Compared with the prior art, the samples of the preparation examples 1-3 obtained by the complete preparation method have better performances in terms of yield, water holding capacity, expansion force, smell and the like, particularly the sample of the preparation example 3 is basically and completely deodorized, the water holding capacity is more than 12000%, the expansion force is more than 180mL/g, the comprehensive performance is excellent, and the preparation method has wide market value and better user satisfaction. The high expansion rate alga dietary fiber slow release capsule of the present invention was further prepared using the alga dietary fiber sample of preparation example 3.

Example 1

The high-expansion-ratio algae dietary fiber slow-release capsule comprises a core material and a wall material, wherein the mass ratio of the core material to the wall material is 1:2;

(1) The core material comprises the following components in parts by mass:

20 parts of probiotics

10 parts of carboxymethyl cellulose

8 parts of chitosan;

the probiotics are mixed by streptococcus thermophilus and lactobacillus bulgaricus according to a mass ratio of 1:1;

the core material forms a self-assembled coating layer on the surface of the probiotics through electrostatic adsorption of carboxymethyl cellulose and chitosan, and the self-assembled coating layer comprises 1 inner carboxymethyl cellulose layer and 1 outer chitosan layer.

(2) The wall material comprises the following components in parts by mass:

PREPARATION EXAMPLE 3 alga dietary fiber 25 parts

15 parts of resistant dextrin.

s1, preparing a core material:

s1.1, preparing a carboxymethyl cellulose water solution with the concentration of 5w/v%, and mixing and preheating probiotics in a coating pot; spraying the carboxymethyl cellulose water solution onto probiotics, and carrying out hot air drying at 35 ℃ alternately to obtain a coating coated with a carboxymethyl cellulose layer;

s1.2, dissolving chitosan in acetic acid aqueous solution with the concentration of 1wt% to obtain chitosan solution with the concentration of 2w/v%, adding a coating into the chitosan solution, carrying out oscillating reaction, slowly adding sodium tripolyphosphate solution to carry out light crosslinking on the outermost chitosan layer, wherein the mass ratio of the sodium tripolyphosphate to the outermost chitosan is 1:50, filtering and drying to obtain a core material coated with the chitosan layer;

s2, preparing the slow-release capsules from the core material and the wall material by a negative pressure low-temperature spray drying method:

s2.1, adding the wall material raw material into deionized water at 70 ℃, stirring to obtain a wall material solution, and cooling to room temperature;

s2.2, adding the core material into the wall material solution, homogenizing at a high speed of 15000rpm for 1 minute, and pressurizing and homogenizing at 10000r/min for 2 times under 45 MPa;

s2.3, atomizing the material homogenized in the step S2.2 in a negative pressure drying cavity, simultaneously introducing drying gas, wherein the vacuum degree in the drying cavity is-0.05 Mpa, the air inlet temperature of the drying cavity is 40 ℃, and the air outlet temperature is 30 ℃.

Example 2

The difference between this example and example 1 is that the wall material comprises carboxymethyl cellulose, and all the wall material materials are mixed with deionized water when preparing the wall material solution. The wall material comprises the following components in parts by mass:

PREPARATION EXAMPLE 3 alga dietary fiber 25 parts

Resistant dextrin 15 parts

10 parts of carboxymethyl cellulose.

Example 3

The difference between this embodiment and embodiment 2 is that the mass ratio of the core material to the wall is 1:2.5, the self-assembled coating layer of the core material comprises 2 carboxymethyl cellulose layers and 2 chitosan layers alternately formed, and the outermost layer is a chitosan layer. And the preparation of the core material comprises the following steps:

(1) Preparing a carboxymethyl cellulose water solution with the concentration of 5w/v%, and mixing and preheating probiotics in a coating pot; spraying the carboxymethyl cellulose water solution onto probiotics, and carrying out hot air drying at 35 ℃ alternately to obtain a coating coated with a carboxymethyl cellulose layer;

(2) Dissolving chitosan in acetic acid aqueous solution with the concentration of 1wt% to obtain chitosan solution with the concentration of 2w/v%, adding a coating into the chitosan solution, carrying out oscillation reaction, filtering and drying to obtain a coating coated with a chitosan layer;

(3) Preheating the coating obtained in the step (2) in a coating pot again; spraying by using carboxymethyl cellulose water solution, and carrying out hot air drying at 35 ℃ alternately to obtain a coating with two carboxymethyl cellulose layers;

(4) Adding the coating obtained in the step (3) into chitosan solution, carrying out oscillation reaction, slowly adding sodium tripolyphosphate solution to carry out light crosslinking on the outermost chitosan layer, wherein the mass ratio of the sodium tripolyphosphate to the outermost chitosan is 1:50, filtering and drying to obtain a core material alternately coated with 2 carboxymethyl cellulose layers and 2 chitosan layers, see figure 1.

Comparative example 1

The comparative example differs from example 3 in that the probiotics were directly used as the core material, and no self-assembled coating layer was formed. The mass ratio of the core material to the wall material is 1:2.5;

(1) The core material comprises probiotics, and is prepared by mixing streptococcus thermophilus and lactobacillus bulgaricus in a mass ratio of 1:1;

(2) The wall material comprises the following components in parts by mass:

PREPARATION EXAMPLE 3 alga dietary fiber 25 parts

Resistant dextrin 15 parts

10 parts of carboxymethyl cellulose.

The preparation method of the comparative sample comprises the following steps:

(1) Adding the wall material raw material into 70 ℃ deionized water, stirring to obtain a wall material solution, and cooling to room temperature;

(2) Adding the probiotic core material into the wall material solution, homogenizing at a high speed of 10000rpm for 1 minute, and homogenizing at a pressure of 10000r/min and 45MPa for 2 times;

(3) Atomizing the homogenized material in a negative pressure drying cavity, and simultaneously introducing drying gas, wherein the vacuum degree in the drying cavity is-0.05 Mpa, the air inlet temperature in the drying cavity is 40 ℃, and the air outlet temperature is 30 ℃.

Comparative example 2

The present comparative example differs from example 3 in that the algal dietary fiber of preparation example 3 was not used, and the wall material only includes, in parts by mass: 15 parts of resistant dextrin and 3.5 parts of carboxymethyl cellulose.

The following tests were performed on examples 1-3 and comparative examples 1-2:

1. satiety test

10 subjects were selected to test the above samples and glucose samples with comparable calories, respectively, for 3 hours, every 15 minutes during hour 1, every 30 minutes during hour 2 and 3, and the satiety of the subjects was recorded every 30 minutes, and the satiety curve was plotted after averaging, as shown in fig. 2. Based on fasted or fasting state, wherein:

"-1": extremely starved;

"0": hunger;

"1": moderate starvation;

"2": no sense;

"3": a moderate feeling of satiety;

"4": saturation;

"5": extremely full.

Overall, each sample provided a more pronounced change in satiety before 15 minutes, reaching higher values in about 30 minutes, followed by a gradual decay. In comparison, examples 1-3 and comparative example 1 contained algae dietary fiber, and overall satiety was better than comparative example 2 and the glucose group data, and comparative example 2 contained resistant dextrin was better than the glucose group data. The samples of examples 1-3 decayed relatively slowly and were able to provide a longer feeling of satiety.

2. Long term stability test

3g of each sample and untreated probiotic control example are weighed, sealed by a gland, packaged in an aluminum bag and stored in a constant temperature experimental box at 4 ℃, the viable count is measured on a 90-day sample to obtain the bacterial survival rate, the long-term stability is examined, and the result is shown in Table 2.

Table 2 results of long term stability layer test for each sample

	Example 1	Example 2	Example 3	Comparative example 1	Comparative example 2	Comparative example
							Survival/%	93.9	94.2	95.2	72.5	86.4	0.5

3. Artificial gastric juice stability test

Preparing artificial gastric juice: 16.4ml of diluted hydrochloric acid with the concentration of about 10 percent is taken, about 800ml of water and 10g of pepsin are added, and the mixture is uniformly shaken and then diluted into 1000ml of water to obtain the finished product.

1g of each sample is respectively placed in artificial gastric juice, cultured at 37 ℃ and 180rpm in a shaking table, and is sampled and neutralized to be neutral when treated for 0.5h, 1h, 1.5h, 2h, 2.5h and 3h, the number of viable bacteria is measured, the survival rate is calculated, and the stability condition of each sample under the condition of the artificial gastric juice is analyzed according to the survival rate, and the result is shown in Table 3.

TABLE 3 results of stability test of samples in artificial gastric juice

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Examples 1-3 and comparative example 2 have a coating of chitosan which is less likely to be destroyed by gastric acid, and thus they have a limited amount of release in the stomach, and the above-mentioned samples have a good probiotic protecting function in the stomach, depending on food and the like, for about 3 hours in the stomach. The probiotic core material of comparative example 1 is not protected by a self-assembled coating layer, is released faster under the action of gastric acid with low pH value, and the survival rate of the probiotics is obviously reduced.

4. Intestinal fluid release, colon simulated release test and embedding rate calculation for examples 1-3

Preparing artificial simulated intestinal juice: taking 6.8g of monopotassium phosphate, adding 500ml of water for dissolution, and adjusting the pH value to 6.8 by using 0.1mol/L sodium hydroxide solution; another 10g of pancreatin is taken, dissolved in a proper amount of water, and the two solutions are mixed and diluted to 1000ml by adding water.

Preparing colon simulating liquid: 0.0123g of chitosan enzyme is dissolved in 1L of water, and the pH value is adjusted to 7.2.

2.5g of the samples of examples 1-3 were placed in 30mL of artificial simulated intestinal fluid and colon-simulating fluid, respectively, and incubated at 37℃and 180rpm in a shaker, and the samples were taken out for 1h, 2h, 3h and 6h, respectively, to determine the viable count in the artificial intestinal fluid and the colon-simulating fluid.

After each sample was thoroughly disintegrated in the colon-simulating liquid, the number of viable bacteria in the liquid was measured, and the embedding rate was calculated according to the following formula. The results are shown in Table 4.

TABLE 4 results of intestinal fluid release, colon simulated release test and entrapment rate for examples 1-3

The probiotics protected by the self-assembled coating layer are released slowly in the intestinal juice, but can be rapidly subjected to enzymolysis under the action of chitosanase, and the release rate of the probiotics is far higher than that of similar samples in the intestinal juice.

According to the related tests of satiety, stomach, intestinal canal and the like, the invention adopts the wall material component compounded by the alga dietary fiber and the resistant dextrin, can form better and durable satiety in the stomach, and the release rate of the probiotic component in the stomach and the small intestine is lower through the protection of the self-assembled coating layer, and the probiotic component stably enters the colon to exert the efficacy, so that meal replacement products can be provided for users with the requirements of losing weight and reducing fat and the like, the intestinal health of the users can be protected, and more scientific, safe and durable health care effects can be provided.

The foregoing description of the preferred embodiments of the present invention has been presented for purposes of clarity and understanding, and is not intended to limit the invention to the particular embodiments disclosed, but is intended to cover all modifications, alternatives, and improvements within the spirit and scope of the invention as outlined by the appended claims.

Claims

1. The high-expansion-rate algae dietary fiber slow-release capsule is characterized by comprising a core material and a wall material, wherein the mass ratio of the core material to the wall material is 1: (1-3);

the core material comprises the following components in parts by mass:

15-25 parts of probiotics

5-15 parts of carboxymethyl cellulose

5-10 parts of chitosan;

the wall material comprises the following components:

20-30 parts of algae dietary fiber

10-20 parts of resistant dextrin;

2. The sustained-release capsule according to claim 1, wherein the probiotics are at least one selected from streptococcus thermophilus, lactobacillus bulgaricus, lactobacillus acidophilus, lactobacillus casei, bifidobacterium, lactobacillus brevis and lactobacillus plantarum.

3. The sustained release capsule according to claim 1 or 2, wherein the algal dietary fiber is prepared by:

4. A sustained release capsule according to claim 3, wherein in step (2), the enzymolysis process of the complex enzyme comprises:

5. A slow release capsule according to claim 3, wherein the freeze-dried algae dietary fiber is crushed to 2-30 μm at a freeze temperature of-60 ℃ to-40 ℃ and a vacuum of 10 to 50 Pa.

6. The sustained release capsule according to claim 4 or 5, wherein the core material is prepared by:

step one: spraying carboxymethyl cellulose water solution onto probiotics, and drying with hot air to obtain a coating coated with carboxymethyl cellulose;

step two: adding the coating into chitosan solution, oscillating for reaction, forming a self-assembled chitosan layer on the surface of the coating through electrostatic adsorption of carboxymethyl cellulose and chitosan, filtering and drying to obtain the core material.

7. The sustained-release capsule according to claim 6, wherein steps one to two are repeated 1 to 3 times, and when the coating is added to the chitosan solution for the last time, slowly adding sodium tripolyphosphate solution to crosslink the outermost chitosan with shaking, wherein the mass ratio of sodium tripolyphosphate to the outermost chitosan is 1: (40-60).

8. A method for preparing the high expansion rate algae dietary fiber slow release capsule according to any one of claims 1-7, comprising the steps of:

s1, preparing a core material:

9. The method of claim 8, wherein the wall material further comprises carboxymethyl cellulose in an amount of 20-30% of the total mass of the algae dietary fiber and the resistant dextrin.

10. Use of the high expansion rate algae dietary fiber slow release capsule of any one of claims 1-7 in food and medicine.