Preparation method and application of long-acting antibacterial fiber functional feed

Abstract

The invention discloses a preparation method of a long-acting antibacterial fiber functional feed, and belongs to the technical field of biomass resource development and utilization. The preparation method comprises the following steps: firstly, mixing and stirring crushed and screened agriculture and forestry wood fibers and an ammoniating agent solution to obtain ammoniated wood fiber pulp, and drying to obtain ammoniated wood fiber powder; and mixing and stirring the ammoniated wood fiber powder and a citral solution to obtain citral composite fiber pulp, recovering the solvent, and drying to obtain the fiber functional feed. By controlling the ammoniation degree of the agriculture and forestry fibers and controlling the addition amount and moisture of citral, the prepared fiber functional feed has good stability, long-acting antibacterial property and slow release property, and the long-acting quality guarantee performance of the fibers can be effectively achieved; meanwhile, the fiber is good in dispersity, good in normal-temperature storage stability, capable of being added into fluid, semi-fluid and solid, wide in application range and good in application prospect in the fields of agriculture and forestry biomass resource development and utilization, feed processing industry and the like.

Description

Technical Field

[0001] The invention belongs to the technical field of biomass resource development and utilization, and specifically relates to a preparation method and application of a long-acting antibacterial fiber functional feed. Background Art

[0002] Using agricultural and forestry fibers as raw materials and vigorously developing agricultural and forestry food and feed utilization is of great strategic significance for further improving the high-value utilization of agricultural and forestry biomass and partially replacing grain and feed. Agricultural and forestry wood fibers are mainly composed of cellulose, hemicellulose and lignin, of which cellulose and hemicellulose can be widely used by microorganisms. Therefore, fiber feeds are extremely susceptible to environmental microorganisms during storage and transportation, and are prone to mold and deterioration, which seriously affects the subsequent processing and utilization of food and feed. Therefore, the development of efficient agricultural and forestry fiber preservation technology is of great significance to the promotion of agricultural and forestry fiber food and feed utilization.

[0003] At present, the preservation and fresh-keeping technologies of feed mainly include: adding chemical preservatives, vacuum packaging, adding natural antibacterial agents, etc. As the harmfulness of chemical preservatives is constantly being explored, the types and dosages used have become increasingly strictly controlled in recent years. Once the vacuum packaging is unsealed, there is still a risk of deterioration during a long feeding cycle, and it cannot actually play a long-term preservation role. As natural antibacterial preservatives, natural plants and their extracts have the advantages of rich resources, comprehensive functions, high safety, small side effects, and not easy to develop drug resistance. Compared with chemical preservatives, the antibacterial mechanism of natural plants is more inclined to the "holistic concept" of multi-target / multi-component, so it is safer and more effective in treating complex diseases or body disorders. Therefore, it has obvious advantages in comprehensively improving the health status of animals, preventing animal diseases, improving production performance and improving product quality. Natural plant extracts can be roughly divided into polyphenols, polysaccharides, terpenes, alkaloids, etc. according to their chemical structure, and they have both commonalities and characteristics in the field of breeding. Among them, plant polyphenols and essential oils have broad-spectrum bactericidal properties and are most widely used in feed preservation. Currently, the most commonly used ones are oregano oil, carvacrol, thymol, cinnamaldehyde, lemon oil, chili oil, etc. These ingredients have the functions of regulating enzyme activity, protecting intestinal villi, improving feed conversion efficiency, inhibiting the growth of harmful microorganisms, stimulating the reproduction of beneficial microorganisms, and improving the antioxidant capacity and storage time of meat.

[0004] Natural citral mainly includes two configurations: α-citral (nerol) and β-citral (geranial), which are mainly derived from Cymbopogon winterianus oil and Litsea cubeba oil. Litsea cubeba is one of the unique forest-source spice resources in China, and its natural resources are very rich. The relative content of natural citral in Litsea cubeba oil can reach more than 70%. Citral has a wide range of applications in food additives, plant growth hormones, daily chemical products, and pharmaceutical intermediates, and has functions such as flavor enhancement, food attraction, antibacterial and pheromone. Therefore, the introduction of citral as a fiber feed preservative has certain advantages in terms of safety and multiple functions. However, citral is easy to volatilize and has a relatively active chemical property, and it is easy to undergo redox reactions to generate geranic acid or geraniol / nerol. Therefore, the stability of citral restricts its wide application.

[0005] Using ammonia and its derivatives to pretreat wood fiber can effectively destroy the structure of wood fiber, and form aminated lignin that can be adsorbed in wood fiber to form an aminated wood fiber mixture (hereinafter referred to as aminated wood fiber). Aminated lignin has amino and amide structures, and can form a Schiff base complex with better stability with aldehyde groups. The present invention uses agricultural and forestry wood fiber as raw material, citral as the main antibacterial activator, and uses ammoniation to treat wood fiber and aldehyde-amino Schiff base reaction to obtain an aminated wood fiber citral Schiff base complex with better stability. This complex can be decomposed into fiber and citral in an acidic environment, and has a slow-release citral performance. The present invention develops a method for preparing a long-acting antibacterial citral fiber functional feed, which is conducive to improving the effective utilization of agricultural and forestry wood fiber and citral. The prepared fiber feed has good stability, long-acting antibacterial and slow-release properties, and can effectively improve the shelf life of agricultural and forestry fibers, and has potential appetizing properties for animals. Summary of the invention

[0006] The technical problem to be solved by the present invention is to provide a method for preparing a long-acting antibacterial fiber functional feed. The method is simple, environmentally friendly, has good process stability, can be added to fluids, semi-fluids and solids, has a wide range of applications, and has good application prospects in the fields of agricultural and forestry biomass resource development and utilization, feed processing industry, etc. Another technical problem to be solved by the present invention is to provide an application of a fiber functional feed, which can be used for addition to various formula feeds or as a single feed.

[0007] In order to solve the above technical problems, the technical solution adopted by the present invention is as follows:

[0008] A method for preparing a long-acting antibacterial fiber functional feed comprises the following steps: mixing and stirring crushed and screened agricultural and forestry wood fibers with an aminating agent solution to obtain ammoniated wood fiber pulp, which is dried to obtain ammoniated wood fiber powder; then mixing and stirring the ammoniated wood fiber powder with a citral solution to obtain a citral composite fiber pulp, and recovering the solvent and drying to obtain the fiber functional feed.

[0009] Furthermore, the agricultural and forestry wood fibers include bamboo shoot shells, corn stalks, caragana, and poplar; and the particle size after crushing and screening is 0.02-2 mm.

[0010] Furthermore, the type of the aminating agent is selected from one or more of urea, ammonium carbonate, ammonium bicarbonate, and ammonia water.

[0011] Furthermore, the mass ratio of the agricultural and forestry wood cellulose to the ammoniating agent solution is 1:0.05~0.2; the reaction temperature of the agricultural and forestry wood fiber and the ammoniating agent solution is 100~140°C, and the closed fumigation reaction time is 0.5~4 h; the drying temperature of the ammoniated wood fiber pulp is 50~90°C.

[0012] Furthermore, the solid content of the ammoniated wood fiber pulp accounts for 18% to 27% of the total content; the pH of the ammoniated wood fiber pulp is 8 to 11; and the water content of the ammoniated wood fiber powder accounts for 1% to 10% of the total content.

[0013] Furthermore, the mass ratio of the ammoniated wood fiber powder to the citral solution is 1:0.005-0.05; the reaction temperature of the ammoniated wood fiber powder and the citral solution is 80-120°C, and the closed fumigation reaction time is 0.5-6 h.

[0014] Furthermore, the solvent of the citral solution is selected from one or more of ethanol and ethyl acetate; the mass fraction of the citral solution is 10% to 50%.

[0015] Furthermore, the drying temperature of the citral composite fiber pulp is 50-80° C.; the moisture content of the fiber functional feed accounts for 1%-10% of the total content.

[0016] Furthermore, any of the above-mentioned methods for preparing long-acting antibacterial fiber functional feed can produce fiber functional feed.

[0017] Furthermore, the fiber functional feed is used in addition to various formula feeds or as a single feed.

[0018] Compared with the prior art, the present invention has the following advantages:

[0019] (1) The present invention uses abundant and low-cost agricultural and forestry fibers as raw materials, and the production process is simple and easy, which is conducive to the high-value utilization of agricultural and forestry biomass resources.

[0020] (2) The preparation method of the present invention is simple, environmentally friendly and has good process stability. By controlling the degree of ammoniaization of agricultural and forestry fibers and the amount of citral added and the moisture content, the prepared fiber functional feed has good stability, long-term antibacterial properties and sustained release properties, and can effectively achieve the long-term shelf life of the fiber.

[0021] (3) The fiber of the present invention has good dispersibility and good storage stability at room temperature. It can be added to fluids, semi-fluids and solids and has a wide range of applications.

[0022] (4) The main raw materials used in the present invention meet the requirements of feed raw materials and additives. The prepared fiber functional feed has a rich ammonia nitrogen content and can be mainly used in the field of ruminant feed such as cattle and sheep. The present invention has good application prospects in the fields of agricultural and forestry biomass resource development and utilization, feed processing industry, etc. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 This is an infrared comparison diagram of the long-acting antibacterial fiber functional feed and its intermediate products and raw materials prepared in Example 1 of the present invention;

[0024] Figure 2 This is an infrared comparison diagram of the long-acting antibacterial fiber functional feed and its intermediate products and raw materials prepared in Example 2 of the present invention;

[0025] Figure 3 This is an infrared comparison diagram of the long-acting antibacterial fiber functional feed and its intermediate products and raw materials prepared in Example 3 of the present invention;

[0026] Figure 4 This is an infrared comparison diagram of the long-acting antibacterial fiber functional feed and its intermediate products and raw materials prepared in Example 4 of the present invention;

[0027] Figure 5 This is a diagram showing the release of citral in the long-acting antibacterial fiber functional feed prepared in Examples 1-4 of the present invention in artificial simulated rumen fluid;

[0028] Figure 6 This is a graph showing the change in the total number of molds in the long-acting antibacterial fiber functional feed prepared in Examples 1-4 of the present invention and its raw materials during open storage. DETAILED DESCRIPTION

[0029] The present invention is further illustrated below in conjunction with specific examples. The examples are implemented based on the technical solutions of the present invention. It should be understood that these examples are only used to illustrate the present invention and are not used to limit the scope of the present invention.

[0030] Example 1

[0031] 50 g (calculated on a dry basis) of crushed and sieved corn straw powder with a particle size of 0.05-1 mm was slowly added to 300 mL of 2% ammonia solution, and the mixture was sealed and fumigated at 120 °C for 1 h to obtain an ammoniated wood fiber pulp with a solid content of 18% and a pH value of about 11. It was further hot-air dried at 70 °C to obtain about 59 g of ammoniated wood fiber powder with a moisture content of 5%. Subsequently, 12.5 mL of 20% citral ethanol solution was added and the mixture was sealed and fumigated at 100 °C for 2 h. It was dried at 60 °C to a moisture content of 5%, thus obtaining about 60 g of fiber functional feed (derived from corn straw) with long-term shelf life.

[0032] Example 2

[0033] 100 g (calculated on a dry basis) of crushed and sieved bamboo shoot shell powder with a particle size of 0.02-0.5 mm was slowly added to 500 mL of 4% urea and 1% ammonia solution, and the mixture was fumigated at 140 °C for 0.5 h to obtain an ammoniated wood fiber pulp with a solid content of 25% and a pH value of about 9. It was further hot-air dried at 50 °C to obtain about 136 g of ammoniated wood fiber powder with a moisture content of 10%. Subsequently, 4 mL of 50% citral ethyl acetate solution was added and the mixture was fumigated at 80 °C for 6 h. The mixture was dried at 80 °C to a moisture content of 10%, to obtain about 137 g of fiber functional feed (derived from bamboo shoot shells) with long-term shelf life.

[0034] Example 3

[0035] 20 g (calculated on a dry basis) of crushed and sieved Caragana korshinskii powder with a particle size of 0.1-2 mm was slowly added to 100 mL of an aqueous solution containing 1% ammonium carbonate and 1% urea, and the mixture was fumigated at 100 °C for 4 h to obtain an ammoniated wood fiber pulp with a solid content of 22% and a pH value of about 8. The mixture was further hot-air dried at 90 °C to obtain about 22 g of ammoniated wood fiber powder with a moisture content of 1%. Subsequently, 1 mL of a 10% citral ethanol solution was added and the mixture was fumigated at 120 °C for 0.5 h. The mixture was dried at 90 °C to a moisture content of 1%, to obtain about 22 g of a fiber functional feed (derived from Caragana korshinskii) with long-term shelf life.

[0036] Example 4

[0037] 1 kg (calculated on a dry basis) of poplar wood powder with a particle size of 0.05-2 mm after crushing and screening was slowly added into 4 L of 1% ammonium bicarbonate and 1% ammonia solution, and fumigated at 130 °C for 2 h to obtain an ammoniated wood fiber pulp with a solid content of 27% and a pH value of about 10. It was further hot-air dried at 80 °C to obtain about 1.1 kg of ammoniated wood fiber powder with a moisture content of 4%. Subsequently, 100 mL of 25% citral ethanol solution was added and fumigated at 100 °C for 3 h. It was dried at 80 °C to a moisture content of 4%, to obtain about 1.12 kg of (poplar wood source) fiber functional feed with long-term shelf life.

[0038] Example 5

[0039] The infrared spectra of the fiber functional feed with long-term shelf life obtained in Examples 1-4 and its corresponding raw materials and intermediate products are as follows: Figure 1-4 As shown, the following characterization analyses were performed respectively:

[0040] By the attached Figure 1-4 It can be seen that the infrared absorption peaks of wood fiber before and after ammoniation are similar, but the absorption intensities are different. The fiber functional feed with long-term shelf life prepared after citral treatment has great differences. Specifically, after ammoniation of wood fiber, the infrared absorption peaks at 1720 cm -1 The carbonyl absorption peaks in the surrounding areas are all weakened, indicating that the carbonyl groups in the wood fiber are reduced after amination. -1 The band at 1630-1680 cm -1 The region is a typical Schiff base bond (C=N) absorption peak. Figure 1-4 In this region, the absorption peaks are obviously enhanced, which proves the formation of citral wood fiber Schiff base structure; at 1420 cm -1 Carbon-nitrogen bond (CN) stretching vibration absorption bands appeared in nearby areas, suggesting that by-products such as amide structures may have been formed at the same time.

[0041] Example 6

[0042] The fiber functional feed with long-term shelf life obtained in Examples 1-4 was subjected to an in vitro simulated release test. Figure 5 As shown, the analysis is as follows:

[0043] Feed generally stays in the rumen of cattle for no more than 24 hours. The artificial rumen fluid system was used as a simulation of the initial digestive environment of ruminants to study the release of citral in fiber functional feeds with long-term shelf life within 24 hours. The artificial rumen fluid system is based on ELITE-MEDIA clarified bovine rumen fluid, and complex enzymes (including cellulase, xytase, pectinase, amylase and protease, etc.) are appropriately added to simulate the digestive fluid in the initial digestive environment of cattle. The specific conditions are: pH value modulation 6.0-6.5, constant temperature control 39 ℃, uninterrupted 1-3 times / minute oscillation to simulate bovine rumen peristalsis. The results showed that citral in the four fiber functional feeds with long-term shelf life was mainly released at a uniform rate within 24 hours, and there was no "sudden release" phenomenon. Among them, the cumulative release rate of citral in the fiber functional feed derived from corn straw was the highest, reaching 80.5%, followed by the fiber functional feed derived from poplar wood and the fiber functional feed derived from bamboo shoot shell, and the cumulative release rate of citral in the fiber functional feed derived from caragana was the lowest, at 61.2%.

[0044] Example 7

[0045] The antibacterial effect of the fiber functional feed with long-term shelf life obtained in Examples 1-4 above was studied in open storage. Figure 6 As shown, the analysis is as follows:

[0046] According to the provisions of GB13078-2017 National Feed Hygiene Standard for Microbial Contaminants in Cereals and Other Processed Products in GBT / 13092: Total mold count < 4×10 4 CFU / g. The total number of molds is the most important microbial indicator affecting the quality of fiber feed. The fiber functional feeds with long-term shelf life obtained from four wood fiber sources in Examples 1-4 of the present invention were compared for microbial contaminants in an open storage environment (normal temperature and humidity range: temperature 10-30 °C, humidity: 40%-60%) for 90 days. The results showed that the total number of molds in the four fiber functional feeds prepared by the present invention within 90 days was far lower than the national standard of 4×10 4 The total number of molds in the four wood fiber raw materials exceeded the limit after 30 days of open storage.

[0047] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing a long-acting antibacterial fiber functional feed, characterized in that: The crushed and screened agricultural and forestry wood fibers are mixed and stirred with an aminating agent solution to obtain an ammoniated wood fiber pulp, which is dried to obtain an ammoniated wood fiber powder; the ammoniated wood fiber powder is then mixed and stirred with a citral solution to obtain a citral composite fiber pulp, and the solvent is recovered and dried to obtain a fiber functional feed.

2. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The agricultural and forestry wood fibers include bamboo shoot shells, corn stalks, caragana, and poplar wood; the particle size after crushing and screening is 0.02-2 mm.

3. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The type of the aminating agent is selected from one or more of urea, ammonium carbonate, ammonium bicarbonate and ammonia water.

4. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The mass ratio of the agricultural and forestry wood cellulose to the ammoniating agent solution is 1:0.05-0.2; the reaction temperature of the agricultural and forestry wood fiber and the ammoniating agent solution is 100-140°C, and the closed fumigation reaction time is 0.5-4 h; the drying temperature of the ammoniated wood fiber pulp is 50-90°C.

5. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The solid content of the ammoniated wood fiber pulp accounts for 18% to 27% of the total content; the pH of the ammoniated wood fiber pulp is 8 to 11; and the water content of the ammoniated wood fiber powder accounts for 1% to 10% of the total content.

6. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The mass ratio of the ammoniated wood fiber powder to the citral solution is 1:0.005-0.05; the reaction temperature of the ammoniated wood fiber powder and the citral solution is 80-120°C, and the closed fumigation reaction time is 0.5-6 h.

7. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The solvent of the citral solution is selected from one or more of ethanol and ethyl acetate; the mass fraction of the citral solution is 10% to 50%.

8. The method for preparing a long-acting antibacterial fiber functional feed according to claim 1, characterized in that: The drying temperature of the citral composite fiber pulp is 50-80°C; the moisture content of the fiber functional feed accounts for 1%-10% of the total content.

9. The method for preparing a long-acting antibacterial fiber functional feed according to any one of claims 1 to 8, to obtain a fiber functional feed.

10. Use of the fiber functional feed according to claim 9 in addition to various formula feeds or as a single feed.

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