WO2019184307A1 - Feed additive for preventing intestinal infection, preparation method therefor and use thereof - Google Patents

Abstract

A feed additive for preventing intestinal infection, a preparation method therefor and the use thereof. The feed additive is prepared from the following raw materials in parts by weight: 15 to 40 parts of Sapindus mukorossi peel, 10 to 30 parts of walnut peel, 10 to 30 parts of Camellia oleifera peel, 5 to 20 parts of Castanopsis sclerophylla shell, 5 to 20 parts of chestnut shell, 5 to 20 parts of peanut shell, and 5 to 20 parts of acorn shell. Said method comprises (1) performing subcritical water extraction of the raw materials to obtain an extracted liquid and a residue; (2) treating the residue to obtain water-insoluble fibers; and (3) mixing the water-insoluble fibers with the extracted liquid, adsorbing and then drying the resultant to obtain a feed additive. The addition of the feed additive to feeds can prevent intestinal infection of livestock and improve disease resistance of livestock, and the addition can also improve the stability in the gastrointestinal tract and dispensability in feeds. The extraction rate of active ingredients in said method is high.

Description

Feed additive for preventing intestinal infection and preparation method and application thereof Technical field

The invention belongs to the technical field of feed additives, and particularly relates to a feed additive for preventing intestinal infection and a preparation method and application thereof.

Background technique

As the scale of animal husbandry production in China continues to expand and the degree of intensification continues to increase, various intestinal diseases have a tendency to appear frequently. The direct economic losses caused by intestinal diseases are as high as tens of billions of yuan each year. Common intestinal diseases of livestock and poultry are mainly intestinal infections caused by bacteria, viruses and parasites. At present, the main prevention and treatment measures are the use of antibiotics. However, the use of a large number of antibiotics causes the resistance of pathogenic microorganisms and the large amount of antibiotic residues in animal products, which is a serious threat to human health. Therefore, it is an urgent need to find a natural product that can prevent intestinal infections instead of antibiotics.

The rough processing of agricultural products produces more waste, which contains a variety of active ingredients. If these wastes are properly screened and extracted, it is expected to form a preparation or feed additive that can effectively and effectively prevent intestinal infection of livestock and poultry.

Summary of the invention

In order to overcome the shortcomings and deficiencies of the prior art, it is a primary object of the present invention to provide a feed additive for preventing intestinal infections.

Another object of the present invention is to provide a method for preparing the above-described feed additive for preventing intestinal infection.

Still another object of the present invention is to provide an application of the above feed additive for preventing intestinal infection preparations in livestock and poultry.

The object of the invention is achieved by the following technical solution:

A feed additive for preventing intestinal infection is prepared from the following raw materials in parts by weight: 15 to 40 parts of the fruitless skin, 10 to 30 parts of the walnut peel, 10 to 30 parts of the oil tea peel, and bitter buckwheat 5-20 parts of shell, 5-20 parts of chestnut shell, 5-20 parts of peanut shell, and 5-20 parts of acorn shell.

The preparation method of the above feed additive for preventing intestinal infection includes the following steps:

(1) extracting the seedless skin, the walnut peel, the camellia peel, the bitter buckwheat shell, the chestnut shell, the peanut shell and the acorn shell by subcritical water to obtain an extract and a residue;

(2) treating the residue to obtain water-insoluble fibers;

(3) The water-insoluble fiber is mixed with the extract, adsorbed, and dried to obtain a feed additive for preventing intestinal infection.

The subcritical water extraction condition in the step (1) is a pressure of 5 to 20 MPa, a temperature of 150 to 300 ° C; and the extraction time is 0.5 to 3 hours. The volume-to-mass ratio of the subcritical water to the total amount of the raw materials is (8 to 50) mL: 1 g.

The treatment in the step (2) refers to acid hydrolysis using an acid and alkali hydrolysis using an alkali, which may be acidolysis or alkali hydrolysis or first alkaline hydrolysis and acidolysis.

The acidified acid is hydrochloric acid, sulfuric acid or nitric acid; the alkalized base is sodium hydroxide solution or potassium hydroxide solution;

The acid hydrolysis condition is an acid concentration of 0.5 to 2.5 mol/L, an acid hydrolysis time of 1 to 5 hours, an acid hydrolysis temperature of 50 to 100 ° C, and an acid to mass ratio of the residue to the acid of 1 g: (3) ～20)mL;

The alkali hydrolysis condition is that the concentration of the alkali is 2 wt% to 5 wt%, the alkali hydrolysis time is 1 to 5 h, and the alkali hydrolysis temperature is 50 to 100 ° C; when the alkali solution, the mass to volume ratio of the residue to the alkali is 1 g: (3~) 20) mL.

The adsorption in the step (3) is oscillating adsorption, and the adsorption conditions are: adsorption temperature is 20 to 45 ° C, oscillation frequency is 50 to 300 times / min, and shaking adsorption time is 0.5 to 2 h.

The drying in the step (3) is vacuum drying, and the conditions of vacuum drying are: a temperature of 50 to 80 ° C, a pressure of 0.01 to 0.1 MPa, and a drying time of 2 to 8 hours. In the step (3), filtration can be carried out after adsorption.

The raw materials are mixed, pulverized and sieved before the extraction in the step (1). The sieving means a sieve of 40 to 120 mesh.

The above feed additive is used for preventing intestinal infection preparation of livestock and poultry; and for preparing livestock and poultry feed for preventing intestinal infection of livestock and poultry and/or improving disease resistance of livestock and poultry.

The feed additive is added in a mass fraction of 0.05 to 1% (meaning that the additive is 0.05 to 1% of the feed quality) to livestock and poultry feed, and can be used for preventing intestinal infection of livestock and poultry and improving disease resistance of livestock and poultry.

The principle of the invention: utilizing the insecticidal, anti-inflammatory, antibacterial and anti-viral effects of Camellia oleracea, sapindus peel, walnut peel and bitter buckwheat, combined with the gastrointestinal regulation function of peanut shell and chestnut shell, and acorn shell The immune enhancement function, reasonable composition, can effectively prevent intestinal infection of livestock and poultry and improve the disease resistance of livestock and poultry. The invention adopts subcritical water extraction, and utilizes the polarity change of the subcritical water to sufficiently extract active components of different polarities in the peel or the husk. After the active substance in the peel or the husk is extracted, the degradable component of the husk is removed by acid hydrolysis and alkaline hydrolysis, leaving water-insoluble cellulose. The cellulose has a large porosity and a specific surface area, and contains a large amount of hydroxyl groups, and is easy to form a hydrogen bond with an active ingredient such as polyphenol, has a strong adsorption property, and supports the extracted active ingredient in the shell fiber. Improve the stability of the active ingredient in the intestinal tract of the animal and the dispersibility in the feed. The following are the sources and efficacy of the ingredients:

Camellia peel: the fruit shell of the Camellia shrub or the middle tree (the part other than the seed in the fruit), which has the functions of detoxification, insecticidal and antibacterial, but has not been exploited;

Sapindus rind: The sap of the saplings of the Sapindus genus, the fruit rind (the part other than the nucleus (seed) in the fruit) is rich in saponins, which has heat, phlegm, elimination, and insecticidal efficacy;

Walnut peel: the peel of the arbor fruit of the genus Juglans, which has the functions of insecticidal, anti-inflammatory and antibacterial; the use of the walnut peel of the present invention is the exocarp and mesocarp of the fruit;

Bitter shell: the shell of the genus of the genus Fagaceae, the bitter buckwheat has the functions of clearing away heat and detoxifying, decomposing silt, stopping diarrhea, etc., but its shell is not used; the bitter buckwheat is the outer skin of the fruit (ie the shell , the part that wraps the seeds);

Peanut shell: The shell of the annual herbaceous seed of the genus Arachis, containing resveratrol, monounsaturated fatty acid and β-sitosterol, has the effect of strengthening the spleen and appetizing, relieving blood and relieving blood;

Chestnut shell: Cassia chestnut tree, chestnut shell has the effect of reducing stagnation, clearing heat, stopping bleeding, preventing nausea, but has not been exploited; chestnut shell is chestnut shell (ie chestnut outer peel);

Acorn shell: The shell of the fruit of the genus Araceae, the plant has strong adaptability, and its seeds can cure diarrhea and enhance immune function. The shell contains flavonoids but is not utilized. The acorn shell is the outer skin of the shell, the acorn.

The present invention has the following advantages and effects over the prior art:

(1) The invention adopts subcritical water extraction to extract the active compound in the peel and the shell, has high extraction rate, good activity, no organic solvent and is environmentally friendly.

(2) The present invention employs a nut-loaded polyphenol structural compound to improve its stability in the gastrointestinal tract and dispersibility in feed.

(3) The preparation process of the invention is simple and convenient for industrial production.

detailed description

The present invention will be further described in detail below with reference to the embodiments, but the embodiments of the present invention are not limited thereto.

Example 1

(1) Mixing 40g of podless fruit, 20g of walnut peel, 20g of camellia peel, 5g of tartary buckwheat, 5g of chestnut shell, 5g of peanut shell and 5g of acorn shell, crushed, sieved through 40 mesh, added with 1L water, extracted The pressure is 15 MPa, the extraction temperature is 200 ° C, and the extraction time is 1 h, and 820 g of the extract and 230 g of the residue are obtained;

(2) The residue of step (1) is added to 1150 mL of a 1.5 mol/L hydrochloric acid solution for acid hydrolysis, the acid hydrolysis temperature is 70 ° C, acid hydrolysis for 2 h, and filtration; the filter residue is added with 1150 mL of 2% sodium hydroxide aqueous solution. After alkaline hydrolysis, after 2h alkaline hydrolysis, filtration, the filter residue washed to neutral, to obtain 56g of product;

(3) The product obtained in the step (2) is added to the extract of the step (1), oscillated at a frequency of 300 times/min at 20 ° C for 2 hours, and then at a temperature of 50 ° C, a pressure of 0.01 MPa, and dried for 2 hours to prevent intestinal 62g of feed additive for infection.

Example 2

(1) Mix 20g of sapindus peel, 30g of walnut peel, 15g of camellia peel, 10g of tartary buckwheat shell, 10g of chestnut shell, 10g of peanut shell and 5g of acorn shell, crush, pass through 120 mesh sieve, add 2L water to extract, extract The pressure is 20 MPa, the extraction temperature is 300 ° C, and the extraction time is 0.5 h, and 1850 g of the extract and 210 g of the residue are obtained;

(2) The residue of step (1) was added to 4.2 L of a 0.5 mol/L hydrochloric acid aqueous solution for acid hydrolysis, the acid hydrolysis temperature was 100 ° C, and after acid hydrolysis for 3 h, it was filtered; 2.1 L of a hydroxide having a mass fraction of 2% was added to the filter residue. The sodium aqueous solution is subjected to alkaline hydrolysis, and after alkali hydrolysis for 3 hours, it is filtered, and the residue is washed with water until neutral, to obtain 47 g of a product;

(3) The product obtained in the step (2) is added to the extract of the step (1), oscillated at a frequency of 50 times/min at 45 ° C for 0.5 h; then at a temperature of 80 ° C, a pressure of 0.05 MPa, and dried for 4 hours to prevent 53 g of feed additive for intestinal infection.

Example 3

(1) 30 g of sapindus peel, 15 g of walnut peel, 15 g of camellia peel, 5 g of tartary buckwheat, 5 g of chestnut shell, 20 g of peanut shell and 10 g of acorn shell, crushed, sieved through 60 mesh, and added with 0.8 L of water for extraction. The extraction pressure is 5 MPa, the extraction temperature is 150 ° C, and the extraction time is 3 h, and 590 g of the extract and 270 g of the residue are obtained;

(2) Adding the residue of step (1) to 810 mL of a 2.5 mol/L hydrochloric acid aqueous solution for acid hydrolysis, the acid hydrolysis temperature is 50 ° C, acid hydrolysis for 1.5 h, and filtering; the filter residue is added with 1080 mL of 2.5% sodium hydroxide. The aqueous solution is subjected to alkaline hydrolysis, and after alkali hydrolysis for 1.5 hours, it is filtered, and the residue is washed with water until neutral, to obtain 63 g of a product;

(3) The product obtained in the step (2) is added to the extract of the step (1), oscillated at a frequency of 100 times/min for 1 hour at 35 ° C; filtered, and then dried at a temperature of 80 ° C, a pressure of 0.1 MPa, and dried for 3 hours. 68g of feed additive for preventing intestinal infection.

Example 4

(1) 15 g of sapindus peel, 15 g of walnut peel, 30 g of camellia peel, 15 g of tartary buckwheat, 5 g of chestnut shell, 5 g of peanut shell and 15 g of acorn shell, crushed, passed through a mesh of 80 mesh, and extracted with 5 L of water, extracted The pressure is 10 MPa, the extraction temperature is 250 ° C, and the extraction time is 1.5 h, and 4,450 g of an extract and 240 g of a residue are obtained;

(2) The residue of step (1) was added to 2.4 L of a 2 mol/L hydrochloric acid aqueous solution for acid hydrolysis, the acid hydrolysis temperature was 80 ° C, and after acid hydrolysis for 1 h, it was filtered; 1.2 L of sodium hydroxide having a mass fraction of 5% was added to the filter residue. The aqueous solution is subjected to alkaline hydrolysis, and after alkali hydrolysis for 1 hour, it is filtered, and the residue is washed with water until neutral, to obtain a product of 44 g;

(3) The product obtained in the step (2) is added to the extract of the step (1), and shaken at a frequency of 200 times/min at 25 ° C for 1.5 hours; then at a temperature of 70 ° C, a pressure of 0.03 MPa, and dried for 8 hours to prevent 50 g of feed additive for intestinal infection.

Example 5

(1) Mix 20g of sapindus peel, 15g of walnut peel, 15g of camellia peel, 20g of tartary buckwheat shell, 20g of chestnut shell, 5g of peanut shell and 5g of acorn shell, crush, pass 60 mesh sieve, add 3L water extract, extract The pressure is 8 MPa, the extraction temperature is 180 ° C, and the extraction time is 1.5 h, and 2750 g of the extract and 280 g of the residue are obtained;

(2) The residue of step (1) was added to 1.4 L of a 1.5 mol/L hydrochloric acid aqueous solution for acid hydrolysis, the acid hydrolysis temperature was 60 ° C, and after acid hydrolysis for 4 h, it was filtered; the filter residue was added with 1.4 L of 3% by weight of hydroxide. The sodium aqueous solution is subjected to alkali hydrolysis, and after alkali hydrolysis for 4 hours, it is filtered, and the residue is washed with water until neutral, to obtain 62 g of a product;

(3) The product obtained in the step (2) is added to the extract of the step (1), and shaken at a frequency of 250 times/min at 35 ° C for 1 hour; then at a temperature of 60 ° C, a pressure of 0.01 MPa, and dried for 5 hours to prevent intestinal 70g of feed additive for infection.

Example 6

(1) 25 g of sapindus peel, 10 g of walnut peel, 10 g of camellia peel, 10 g of tartary buckwheat shell, 10 g of chestnut shell (exocarp of chestnut), 15 g of peanut shell and 20 g of acorn shell, and pulverized, and passed through a 100 mesh sieve. 4L water extraction, extraction pressure 12MPa, extraction temperature 250 ° C, extraction time 2.5h, to obtain extract 3700g and residue 310g;

(2) The residue of step (1) is added to 3.1 L of a 2.5 mol/L hydrochloric acid aqueous solution for acid hydrolysis, the acid hydrolysis temperature is 70 ° C, acid hydrolysis is 3.5 h, and then filtered; 5 L of 5% hydroxide is added to the residue. The sodium aqueous solution was subjected to alkali hydrolysis, and after alkali hydrolysis for 3.5 hours, it was filtered, and the residue was washed with water to neutralness to obtain 65 g of product.

(3) The product obtained in the step (2) is added to the extract of the step (1), and shaken at a frequency of 150 times/min at 40 ° C for 1.5 hours; then at a temperature of 70 ° C, a pressure of 0.05 MPa, and dried for 6 hours to prevent 73 g of feed additive for intestinal infection.

Example 7

Therapeutic effect of feed additives for preventing intestinal infection on chickens infected with Salmonella

METHODS: A total of 300 Qingyuan Ma chickens of 1 day old were randomly divided into 10 groups, 30 in each group. Divided into control group, antibiotic group, Example 1 additive high, medium and low dose group, and Examples 2-6 additive medium dose group. Infected with Salmonella typhimurium C79-1 once (feeding 0.1 mL, about 10 ⁸ live bacteria), the additive was added in the feed at 1% (high dose), 0.5% (medium dose) and 0.1% (low dose) The antibiotic is amikacin sulfate, and the amount added in the feed is 30 mg/kg. Feed for 30 days in a row. The number of chicken deaths was counted, and the spleen and thymus were taken out after the death of the undead chicken, and the spleen index and thymus index were calculated.

Results: The additive of the invention has a good control effect on chicken infection caused by Salmonella, no death occurs, and the spleen and thymus index are significantly improved compared with the control. Explain that they have the therapeutic effect of antibiotics and the effect of improving chicken immunity. The results are shown in Table 1.

Table 1 Therapeutic effect of additives on Salmonella infected chickens

Extract	Add amount	mortality rate/%	Spleen index /%	Thymus index /%
Control group	/	40	0.097±0.023	0.408±0.064
Example 1 low dose	0.1%	0	0.108±0.027	0.419±0.054
The dose in Example 1	0.5%	0	0.116±0.028	0.427±0.067
Example 1 high dose	1%	0	0.125±0.032	0.438±0.062
Example 2 dose	0.5%	0	0.112±0.024	0.421±0.056
The dose in Example 3	0.5%	0	0.118±0.033	0.429±0.064
Example 4 dose	0.5%	0	0.120±0.031	0.431±0.072
The dose in Example 5	0.5%	0	0.114±0.027	0.422±0.054

Example 6 dose	0.5%	0	0.117±0.029	0.424±0.058
Amikacin	30mg/kg	0	0.102±0.025	0.413±0.055

Example 8

Therapeutic effect of feed additives for preventing intestinal infection on pigs infected with Escherichia coli

Methods: 200 ternary pigs were taken from 10 to 20 days and randomly divided into 10 groups, 20 in each group. The groups were divided into the control group, the high-, medium-, and low-dose groups of the additive of Example 1, the middle-dose group of the additives of Examples 2 to 6, and the antibiotic group. Infected with E. coli O ₃₀₁ (fed 5 mL/day, about 10 ⁹ live bacteria) for 5 days, the additive was added in the feed at 0.2% (high dose), 0.1% (medium dose) and 0.05% (low dose). The antibiotic is gentamicin sulfate, and the amount added in the feed is 10 mg/kg. Continuous medication for 3 days. Observing the condition of the pig: the symptoms disappeared, the diet and mental condition were good for cure; the diarrhea condition was reduced, the appetite improved to be markedly effective; the diarrhea condition was not alleviated or aggravated, and the appetite did not improve.

Results: The additive of the invention has a good control effect on pig infection caused by Escherichia coli, the effective rate is 80-100%, and the cure rate is 50-90%. Explain that they have an alternative effect on antibiotics in pigs infected with E. coli. The results are shown in Table 2.

Table 2 Therapeutic effect of additives on E. coli infected pigs

Extract	Number of animals / only	Effective number / only	Cure number / only	Invalid number / only	Explicit efficiency /%	Cure rate /%
Control group	20	0	0	20	0	0
Example 1 low dose	20	16	10	4	80	50
The dose in Example 1	20	19	16	1	95	80
Example 1 high dose	20	20	18	0	100	90
Example 2 dose	20	18	14	2	90	70
The dose in Example 3	20	19	16	1	95	80
Example 4 dose	20	20	17	0	100	85
The dose in Example 5	20	18	15	2	90	75
Example 6 dose	20	19	17	1	95	85
Gentamicin	20	20	17	0	100	85

Example 9

The feed additives for preventing intestinal infections prepared in Examples 1 to 6 were separately added to chicken feed, and the amount of addition was 5%. After 14 days of use, the chickens grew well, and no chicken intestinal infection occurred within two months.

Example 10

The feed additives for preventing intestinal infection prepared in Examples 1 to 6 were respectively added to the cattle feed, and the added amount was 0.1%. After 7 days of use, the growth and milk production of the cattle were good, and no intestinal infection occurred within two months. .

The above-described embodiments are preferred embodiments of the present invention, and are not to be construed as being limited to the details of the invention. The invention may be modified, modified, and substituted without departing from the spirit and scope of the invention. Combinations and simplifications should all be equivalent replacements and are included in the scope of the present invention.

Claims (10)

1. The invention relates to a feed additive for preventing intestinal infection, which is prepared by the following raw materials in parts by weight: 15 to 40 parts of the fruitless skin, 10 to 30 parts of the walnut peel, and 10 to 30 pieces of the oil tea peel. 5 parts, 20 to 20 parts of tartary buckwheat, 5 to 20 parts of chestnut shell, 5 to 20 parts of peanut shell, and 5 to 20 parts of acorn shell.
2. The method for preparing a feed additive for preventing intestinal infection according to claim 1, comprising the steps of:

   (1) extracting the seedless skin, the walnut peel, the camellia peel, the bitter buckwheat shell, the chestnut shell, the peanut shell and the acorn shell by subcritical water to obtain an extract and a residue;

   (2) treating the residue to obtain water-insoluble fibers;

   (3) The water-insoluble fiber is mixed with the extract, adsorbed, and dried to obtain a feed additive for preventing intestinal infection.
3. The method for preparing a feed additive for preventing intestinal infection according to claim 2, wherein the subcritical water extraction condition in the step (1) is a pressure of 5 to 20 MPa and a temperature of 150 to 300 ° C; The extraction time is 0.5 to 3 hours.
4. The method for preparing a feed additive for preventing intestinal infection according to claim 2, wherein the volume-to-mass ratio of the subcritical water to the total amount of the raw materials is (8 to 50) mL: 1 g.
5. The method for preparing a feed additive for preventing intestinal infection according to claim 2, wherein the treatment in the step (2) refers to acid hydrolysis using an acid and alkali hydrolysis using an alkali, which is an acid hydrolysis first. Alkaline or first alkaline hydrolysis and acidolysis.
6. The method for preparing a feed additive for preventing intestinal infection according to claim 5, wherein the acidified acid is hydrochloric acid, sulfuric acid or nitric acid;

   The alkalized base is a sodium hydroxide solution or a potassium hydroxide solution;

   The acid hydrolysis condition is an acid concentration of 0.5 to 2.5 mol / L, an acid hydrolysis time of 1 to 5 h, and an acid hydrolysis temperature of 50 to 100 ° C;

   The alkaline hydrolysis conditions are a concentration of the base of 2 wt% to 5 wt%, an alkali hydrolysis time of 1 to 5 h, and an alkali hydrolysis temperature of 50 to 100 °C.
7. The method for preparing a feed additive for preventing intestinal infection according to claim 5, characterized in that: in the acid hydrolysis, the mass to volume ratio of the residue to the acid is 1 g: (3 to 20) mL; when alkaline hydrolysis, the residue and The mass to volume ratio of the base is 1 g: (3 to 20) mL.
8. The method for preparing a feed additive for preventing intestinal infection according to claim 2, wherein the adsorption in the step (3) is oscillating adsorption, and the adsorption condition is: the adsorption temperature is 20 to 45 ° C, and the oscillation frequency is 50 to 300 times / min, the shock adsorption time is 0.5 ~ 2h;

   The drying described in the step (3) is vacuum drying.
9. Use of the feed additive according to claim 1 for the prevention of intestinal infection preparations in livestock and poultry.
10. The use of a feed additive for preventing intestinal infection according to claim 1, characterized in that the feed additive is used for preparing livestock feed for preventing intestinal infection of livestock and/or improving disease resistance of livestock and poultry .