Tributyrin solid preparation, preparation method thereof and feed additive

Abstract

The invention relates to the technical field of tributyrin, and particularly discloses a tributyrin solid preparation which comprises the following raw materials in parts by mass: 30-60 parts of tributyrin, 5-10 parts of nano cellulose, 1-2 parts of chitosan, 1-2 parts of vinyltriethoxysilane, 100-200 parts of fatty acid, 1-2 parts of sodium alginate, 1-2 parts of hyperbranched polylysine and 1-2 parts of an emulsifier. 0.01-0.1 part of sodium tripolyphosphate, 1-2 parts of sodium carboxymethyl cellulose, 1-2 parts of calcium chloride and 6-12 parts of an anionic surfactant. The invention also discloses a preparation method of the tributyrin solid preparation. The invention also discloses a feed additive which comprises the tributyrin solid preparation.

Description

Technical Field

[0001] The present invention relates to the technical field of tributyrin, and in particular to a solid preparation of tributyrin and a preparation method thereof, and a feed additive. Background Art

[0002] Tributyrin is a short-chain fatty acid ester formed by the esterification of one glycerol molecule and three butyric molecules. It is a good donor of butyric acid and can release butyric acid in the intestine as an important energy source for the colon. It has the functions of repairing intestinal villi, inhibiting harmful intestinal bacteria, and promoting the absorption and utilization of nutrients. In addition, butyric acid plays an important role in regulating growth performance, gastrointestinal function, immunity, gastrointestinal microecological balance and intestinal pH, and has bactericidal and antibacterial functions.

[0003] As a feed additive, tributyrin has many benefits for the body's functions, such as regulating the structure of intestinal flora, promoting animal growth and development, stimulating intestinal epithelial cell proliferation, increasing the height of small intestinal villi, promoting nutrient absorption, and enhancing the body's immunity. However, tributyrin is an oily liquid with strong irritation, poor fluidity, easy oxidation and deterioration, and has a fat smell that affects the animal's appetite. It is not conducive to direct feeding and is difficult to store, transport and use.

[0004] In order to solve this problem, adsorbent materials are often used to prepare solid tributyrin. CN104106734A discloses a solid granular preparation of tributyrin, a preparation method and application thereof, wherein the traditional liquid tributyrin is solidified into granules, and the liquid tributyrin is adsorbed or bonded on the surface or in the pores of the granular white carbon black silica gel. However, when a large amount of tributyrin is adsorbed, agglomeration is very likely to occur, which affects the product form.

[0005] At present, how to prepare a solid preparation of tributyrin, solve its easy agglomeration problem, and enhance the stability of the product has become a problem that needs to be solved urgently. Summary of the invention

[0006] The purpose of the present invention is to solve the shortcomings of the prior art and to propose a solid preparation of tributyrin and a preparation method thereof and a feed additive.

[0007] A tributyrin solid preparation, the raw materials of which include, by mass, 50-80 parts of tributyrin, 2.5-4.5 parts of nanocellulose, 1-1.7 parts of chitosan, 1-1.8 parts of vinyl triethoxysilane, 10-20 parts of fatty acids, 1-1.8 parts of sodium alginate, 1-2 parts of hyperbranched polylysine, 1-1.8 parts of emulsifier, 0.01-0.1 parts of sodium tripolyphosphate, 1-2 parts of sodium carboxymethyl cellulose, 1-1.8 parts of calcium chloride and 3-6 parts of anionic surfactant.

[0008] Preferably, the number of generations of the hyperbranched polylysine is 1.0-3.0.

[0009] Preferably, the emulsifier is at least one of cocamidopropyl betaine, Span and Tween.

[0010] Preferably, the anionic surfactant is sodium dodecylbenzene sulfonate and / or sodium dodecyl sulfate.

[0011] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0012] S1. Add nanocellulose and chitosan to water, perform ultrasonic treatment at 50-60°C for 5-15min, adjust the pH value of the system to 4-5, stir for 1-2h, add vinyl triethoxysilane and continue stirring for 1-3h, freeze at -40 to -60°C for 10-15h, freeze-dry, crush, add tributyrin and fatty acid mixture, perform ultrasonic treatment for 1-2h, add sodium alginate, hyperbranched polylysine and emulsifier, stir for 5-15min, and obtain preform a;

[0013] S2, adding sodium tripolyphosphate and anionic surfactant into deionized water and stirring evenly to obtain preform b;

[0014] S3, adding sodium carboxymethyl cellulose, calcium chloride, and anionic surfactant into deionized water and stirring evenly to obtain preform c;

[0015] S4. Add preform b dropwise to preform a and stir for 5-15 min at a stirring temperature of 5-15°C. Add the product dropwise to preform c and stir for 10-20 min at a stirring temperature of 40-50°C. Allow to stand for 5-10 h in an environment of 70-80°C and 65-75% RH, and spray dry.

[0016] Preferably, in S1, nanocellulose and chitosan are added to water and then ultrasonically treated, and the frequency of the ultrasonic treatment is 10-20 kHz.

[0017] Preferably, in S1, an aqueous acetic acid solution with a concentration of 1-2 mol / L is used to adjust the pH value of the system to 4-5.

[0018] Preferably, in S1, tributyrin and fatty acids are added and then mixed and ultrasonic treatment is performed. The frequency of the ultrasonic treatment is 5-15 kHz and the temperature of the ultrasonic treatment is 40-60°C.

[0019] Preferably, in S4, the feed rate of the spray drying is 500 mL / h, the inlet temperature is 150-160°C, and the outlet temperature is 70-80°C.

[0020] A feed additive, comprising: the above-mentioned tributyrin solid preparation.

[0021] Beneficial effects:

[0022] The present invention mixes nanocellulose and chitosan and performs acid treatment, so that the two have extremely high affinity and high mutual dispersion uniformity, and are further subjected to vinyl triethoxysilane lipophilic treatment, so that the loading capacity of tributyrin can be extremely high and the product can be highly dispersed uniformly in fatty acids.

[0023] The present invention disperses sodium tripolyphosphate and anionic surfactant in deionized water, drips them into preform a to form an oil-in-water microemulsion, and further drips them into preform c to form a water-in-oil-in-water system, wherein the temperature is controlled at 40-50° C. to promote cross-linking of the internal microemulsion interface and effectively enhance the stability of the internal microemulsion during the stirring process.

[0024] Since sodium carboxymethyl cellulose swells and tends to adsorb on the oil / water interface, the water-in-oil-in-water system not only has a spatial stabilizing effect, but the surface of hyperbranched polylysine contains amino groups, which can produce electrostatic adsorption with carboxymethyl cellulose, making the multiple emulsion system extremely stable, especially conducive to subsequent spray drying to obtain microcapsule preparations, improving the odor problem of tributyrin, making it easier for livestock and poultry to eat, and at the same time not easily decomposed by gastric acid, mainly decomposed in the hind intestine and improving the health of the intestine.

[0025] The content of tributyrin of the present invention can reach more than 65%, and the stability is extremely high, which greatly reduces the transportation and use costs, has stable flowability at room temperature, is easy to use, has no irritation and corrosive effects after being ingested by livestock and poultry, has no side effects, and has stable properties. After being ingested by livestock and poultry and entering the stomach, the microcapsule structure is transformed into fat-soluble soft particles, fatty acids are gradually absorbed in the intestine, and tributyrin is gradually dissociated and absorbed in the intestinal environment. The present invention has low production cost, simple process, cheap equipment, and is conducive to industrial production.

[0026] The experiment found that the present invention can be used for young animals, can significantly improve the imbalance of intestinal flora and antioxidant capacity of animals, can significantly enhance the digestion and absorption of nutrients in the diet, especially fat, can not only reduce the occurrence of inflammation, effectively increase production performance, and promote fat oxidation, but also can protect the liver very well. BRIEF DESCRIPTION OF THE DRAWINGS

[0027] Figure 1 It is a comparison chart of the embedding rates of the solid preparations of tributyrin obtained in Example 5 and Comparative Examples 1-2.

[0028] Figure 2The cumulative release rate curve of tributyrin in the artificial gastric juice and artificial intestinal juice digestion stages of the solid preparations of tributyrin obtained in Example 5 and Comparative Examples 1-2 is shown.

[0029] Figure 3 The cumulative release rate curve of butyric acid in the artificial intestinal fluid digestion stage of the solid preparation of tributyrin obtained in Example 5 and Comparative Examples 1-2.

[0030] Figure 4 It is a comparison chart of the antioxidant indexes of the piglets in Example 5 and Comparative Examples 1-2.

[0031] Figure 5 This is a comparison chart of the number of lactic acid bacteria and Escherichia coli in the rectal feces of piglets in Example 5 and Comparative Example 1-2 groups. DETAILED DESCRIPTION

[0032] The present invention will be further explained below in conjunction with specific embodiments.

[0033] The hyperbranched polylysine used below was purchased from Weihai Chenmu Molecular New Materials Co., Ltd.

[0034] Example 1

[0035] A tributyrin solid preparation, whose raw materials include: 500g of tributyrin, 25g of nanocellulose, 10g of chitosan, 10g of vinyltriethoxysilane, 100g of oleic acid, 10g of sodium alginate, 10g of 1.0 generation hyperbranched polylysine, 10g of cocamidopropyl betaine, 0.1g of sodium tripolyphosphate, 10g of sodium carboxymethyl cellulose, 10g of calcium chloride, 15g of sodium dodecyl sulfate and 15g of sodium dodecylbenzene sulfonate.

[0036] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0037] S1, adding nanocellulose and chitosan to 200g water, ultrasonically treating at a temperature of 50°C for 5min, the ultrasonic frequency is 10kHz, adjusting the pH value of the system to 4-5 with an acetic acid aqueous solution with a concentration of 1mol / L, stirring at a speed of 1000r / min for 1h, adding vinyl triethoxysilane and continuing stirring for 1h, freezing at -40°C for 10h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 1h, the ultrasonic frequency is 5kHz, the ultrasonic temperature is 40°C, adding sodium alginate, hyperbranched polylysine, and cocamidopropyl betaine, stirring at a speed of 1000r / min for 5min, and obtaining preform a;

[0038] S2, adding sodium tripolyphosphate and sodium dodecylbenzene sulfonate into 150 g of deionized water and stirring evenly to obtain preform b;

[0039] S3, adding sodium carboxymethyl cellulose, calcium chloride and sodium dodecyl sulfate to 300 g of deionized water and stirring evenly to obtain preform c;

[0040] S4. Add preform b dropwise into preform a, stir at 4000 r / min for 5 min, control the stirring temperature at 5°C, add the product dropwise into preform c, stir at 4000 r / min for 10 min, control the stirring temperature at 40°C, send into a constant temperature and humidity chamber, let stand for 5 h in an environment of 70°C and 65% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 150°C, and the outlet temperature is 70°C).

[0041] Example 2

[0042] A tributyrin solid preparation, whose raw materials include: 800g of tributyrin, 45g of nanocellulose, 15g of chitosan, 15g of vinyltriethoxysilane, 200g of oleic acid, 18g of sodium alginate, 20g of 3.0 generation hyperbranched polylysine, 18g of Span 60, 1g of sodium tripolyphosphate, 20g of sodium carboxymethyl cellulose, 18g of calcium chloride and 60g of sodium dodecylbenzene sulfonate.

[0043] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0044] S1, adding nanocellulose and chitosan to 300g water, ultrasonically treating at 60°C for 15min, the ultrasonic frequency is 20kHz, adjusting the pH value of the system to 4-5 with 2mol / L acetic acid aqueous solution, stirring at 2000r / min for 2h, adding vinyltriethoxysilane and continuing stirring for 3h, freezing at -60°C for 15h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 2h, the ultrasonic frequency is 15kHz, the ultrasonic temperature is 60°C, adding sodium alginate, hyperbranched polylysine, Span 60, stirring at 5000r / min for 15min, and obtaining preform a;

[0045] S2, adding sodium tripolyphosphate and 30 g of sodium dodecylbenzene sulfonate to 250 g of deionized water and stirring evenly to obtain preform b;

[0046] S3, adding sodium carboxymethyl cellulose, calcium chloride, and 30 g of sodium dodecylbenzene sulfonate to 400 g of deionized water and stirring evenly to obtain preform c;

[0047] S4. Add preform b dropwise into preform a, stir at a speed of 5000 r / min for 15 min, control the stirring temperature at 15°C, add the product dropwise into preform c, stir at a speed of 5000 r / min for 20 min, control the stirring temperature at 50°C, send into a constant temperature and humidity chamber, let stand for 10 h in an environment of 80°C and 75% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 160°C, and the outlet temperature is 80°C).

[0048] Example 3

[0049] A tributyrin solid preparation, whose raw materials include: 600g of tributyrin, 35g of nanocellulose, 13g of chitosan, 18g of vinyltriethoxysilane, 120g of oleic acid, 16g of sodium alginate, 13g of 2.0 generation hyperbranched polylysine, 16g of Tween 60, 0.3g of sodium tripolyphosphate, 17g of sodium carboxymethyl cellulose, 12g of calcium chloride and 48g of sodium dodecyl sulfate.

[0050] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0051] S1, adding nanocellulose and chitosan to 220g water, ultrasonically treating at a temperature of 58°C for 8min, the ultrasonic frequency is 18kHz, adjusting the pH value of the system to 4-5 with an acetic acid aqueous solution having a concentration of 1.2mol / L, stirring at a speed of 1700r / min for 80min, adding vinyltriethoxysilane and continuing stirring for 2.5h, freezing at -45°C for 13h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 80min, the ultrasonic frequency is 12kHz, the ultrasonic temperature is 45°C, adding sodium alginate, hyperbranched polylysine, Tween 60, stirring at a speed of 4000r / min for 8min, and obtaining preform a;

[0052] S2, adding sodium tripolyphosphate and 28 g of sodium dodecyl sulfate into 220 g of deionized water and stirring evenly to obtain preform b;

[0053] S3, adding sodium carboxymethyl cellulose, calcium chloride, and 20 g of sodium dodecyl sulfate to 330 g of deionized water and stirring evenly to obtain preform c;

[0054] S4. Add preform b dropwise into preform a, stir at 4800 r / min for 8 min, control the stirring temperature at 12°C, add the product dropwise into preform c, stir at 4300 r / min for 17 min, control the stirring temperature at 42°C, send into a constant temperature and humidity chamber, let stand for 9 h in an environment of 77°C and 68% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 155°C, and the outlet temperature is 75°C).

[0055] Example 4

[0056] A tributyrin solid preparation, whose raw materials include: 700g of tributyrin, 35g of nanocellulose, 17g of chitosan, 12g of vinyltriethoxysilane, 180g of oleic acid, 12g of sodium alginate, 17g of 2.0 generation hyperbranched polylysine, 14g of cocamidopropyl betaine, 0.7g of sodium tripolyphosphate, 13g of sodium carboxymethyl cellulose, 16g of calcium chloride and 55g of sodium lauryl sulfate.

[0057] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0058] S1, adding nanocellulose and chitosan to 280g water, ultrasonically treating at a temperature of 52°C for 12min, the ultrasonic frequency is 12kHz, adjusting the pH value of the system to 4-5 with an acetic acid aqueous solution having a concentration of 1.8mol / L, stirring at a speed of 1300r / min for 100min, adding vinyltriethoxysilane and continuing stirring for 1.5h, freezing at -55°C for 11h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 100min, the ultrasonic frequency is 6kHz, the ultrasonic temperature is 55°C, adding sodium alginate, hyperbranched polylysine, and cocamidopropyl betaine, stirring at a speed of 2000r / min for 12min, and obtaining preform a;

[0059] S2, adding sodium tripolyphosphate and 20 g of sodium dodecyl sulfate into 180 g of deionized water and stirring evenly to obtain preform b;

[0060] S3, adding sodium carboxymethyl cellulose, calcium chloride, and 35 g of sodium dodecyl sulfate to 370 g of deionized water and stirring evenly to obtain preform c;

[0061] S4. Add preform b dropwise into preform a, stir at 4200 r / min for 12 min, control the stirring temperature at 8°C, add the product dropwise into preform c, stir at 4700 r / min for 13 min, control the stirring temperature at 48°C, send into a constant temperature and humidity chamber, let stand for 7 h in an environment of 73°C and 72% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 155°C, and the outlet temperature is 75°C).

[0062] Example 5

[0063] A tributyrin solid preparation, whose raw materials include: 650g of tributyrin, 40g of nanocellulose, 15g of chitosan, 15g of vinyltriethoxysilane, 150g of oleic acid, 15g of sodium alginate, 15g of 2.0 generation hyperbranched polylysine, 15.5g of Tween 80, 0.5g of sodium tripolyphosphate, 15g of sodium carboxymethyl cellulose, 15g of calcium chloride and 54g of sodium dodecylbenzene sulfonate.

[0064] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0065] S1, adding nanocellulose and chitosan to 250g water, ultrasonically treating at a temperature of 55°C for 10min, the ultrasonic frequency is 15kHz, adjusting the pH value of the system to 4-5 with an acetic acid aqueous solution with a concentration of 1.5mol / L, stirring at a speed of 1500r / min for 90min, adding vinyltriethoxysilane and continuing stirring for 2h, freezing at -50°C for 12h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 90min, the ultrasonic frequency is 9kHz, the ultrasonic temperature is 50°C, adding sodium alginate, hyperbranched polylysine, Tween 80, stirring at a speed of 3000r / min for 10min, and obtaining preform a;

[0066] S2, adding sodium tripolyphosphate and 27g sodium dodecylbenzene sulfonate to 200g deionized water and stirring evenly to obtain preform b;

[0067] S3, adding sodium carboxymethyl cellulose, calcium chloride, and 27 g of sodium dodecylbenzene sulfonate to 350 g of deionized water and stirring evenly to obtain preform c;

[0068] S4. Add preform b dropwise into preform a, stir at 4500 r / min for 10 min, control the stirring temperature at 10°C, add the product dropwise into preform c, stir at 4500 r / min for 15 min, control the stirring temperature at 45°C, send into a constant temperature and humidity chamber, let stand for 8 h in an environment of 75°C and 70% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 155°C, and the outlet temperature is 75°C).

[0069] Comparative Example 1

[0070] A tributyrin solid preparation, whose raw materials include: 650g of tributyrin, 40g of nanocellulose, 15g of chitosan, 15g of vinyltriethoxysilane, 150g of oleic acid, 15g of sodium alginate, 15g of 2.0 generation hyperbranched polylysine, 15.5g of Tween 80, 0.5g of sodium tripolyphosphate and 27g of sodium dodecylbenzene sulfonate.

[0071] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0072] S1, adding nanocellulose and chitosan to 250g water, ultrasonically treating at a temperature of 55°C for 10min, the ultrasonic frequency is 15kHz, adjusting the pH value of the system to 4-5 with an acetic acid aqueous solution with a concentration of 1.5mol / L, stirring at a speed of 1500r / min for 90min, adding vinyltriethoxysilane and continuing stirring for 2h, freezing at -50°C for 12h, freeze drying, crushing, adding tributyrin and oleic acid to mix, ultrasonically treating for 90min, the ultrasonic frequency is 9kHz, the ultrasonic temperature is 50°C, adding sodium alginate, hyperbranched polylysine, Tween 80, stirring at a speed of 3000r / min for 10min, and obtaining preform a;

[0073] S2, adding sodium tripolyphosphate and 27g sodium dodecylbenzene sulfonate to 200g deionized water and stirring evenly to obtain preform b;

[0074] S3. Add preform b dropwise into preform a, stir at 4500 r / min for 10 min, control the stirring temperature at 10°C, send into a constant temperature and humidity chamber, let stand for 8 h in an environment of 75°C and 70% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 155°C, and the outlet temperature is 75°C).

[0075] Comparative Example 2

[0076] A tributyrin solid preparation, whose raw materials include: 650g of tributyrin, 40g of nanocellulose, 15g of chitosan, 150g of oleic acid, 15g of sodium alginate, 15g of 2.0 generation hyperbranched polylysine, 15.5g of Tween 80, 0.5g of sodium tripolyphosphate, 15g of sodium carboxymethyl cellulose, 15g of calcium chloride, and 54g of sodium dodecylbenzene sulfonate.

[0077] The preparation method of the above-mentioned tributyrin solid preparation comprises the following steps:

[0078] S1, adding nanocellulose and chitosan to tributyrin and oleic acid, mixing, ultrasonic treatment for 90 minutes, ultrasonic frequency of 9 kHz, ultrasonic temperature of 50 ° C, adding sodium alginate, hyperbranched polylysine, Tween 80, stirring at a speed of 3000 r / min for 10 minutes, to obtain preform a;

[0079] S2, adding sodium tripolyphosphate and 27g sodium dodecylbenzene sulfonate to 200g deionized water and stirring evenly to obtain preform b;

[0080] S3, adding sodium carboxymethyl cellulose, calcium chloride, and 27 g of sodium dodecylbenzene sulfonate to 350 g of deionized water and stirring evenly to obtain preform c;

[0081] S4. Add preform b dropwise into preform a, stir at 4500 r / min for 10 min, control the stirring temperature at 10°C, add the product dropwise into preform c, stir at 4500 r / min for 15 min, control the stirring temperature at 45°C, send into a constant temperature and humidity chamber, let stand for 8 h in an environment of 75°C and 70% RH, and spray dry (the feed rate of spray drying is 500 mL / h, the inlet temperature is 155°C, and the outlet temperature is 75°C).

[0082] The tributyrin contents in the solid tributyrin preparations of Example 5 and Comparative Examples 1-2 were measured, and the tributyrin contents of the three preparations were all >65%, which met the internal control quality standards of the applicant.

[0083] The embedding efficiency of the solid preparation of tributyrin obtained in Example 5 and Comparative Examples 1-2 was measured. Figure 1 As shown, the embedding rate of the solid preparation of tributyrin obtained in Example 5 was the highest, which was significantly better than that in Comparative Examples 1-2 (P < 0.05).

[0084] The tributyrin solid preparations obtained in Example 5 and Comparative Examples 1-2 were digested by a static digestion method, as follows:

[0085] Artificial gastric fluid: 0.514g / L KCl, 0.123g / L KH2PO4, 2.1g / L NaHCO3, 2.758g / L NaCl, 0.0203g / L MgCl2, 0.048g / L CaCl2 and pepsin (2000U / mL in the final digestion system), adjust the pH to 2.0 with hydrochloric acid solution, and prepare for use immediately.

[0086] Enzyme-free artificial intestinal fluid: 0.253g / LKCl, 0.054g / LKH2PO4, 3.57g / LNaHCO3, 1.12g / LNaCl, 0.335g / LMgCl2, 0.44g / L CaCl2, bile salt 10mM, prepared and used immediately.

[0087] Normal artificial intestinal fluid: 0.253g / LKCl, 0.054g / LKH2PO4, 3.57g / LNaHCO3, 1.12g / LNaCl, 0.335g / LMgCl2, 0.44g / L CaCl2, 10mM bile salt and pancreatic lipase (2000U / mL in the final digestion system), prepared and used immediately.

[0088] (1) 0.1 g of each group of tributyrin solid preparation samples were placed in 10 mL of artificial gastric juice and digested at 100 rpm / min in a constant temperature water bath shaker at 37±0.5°C for 2 h. Then, the samples were mixed with enzyme-free artificial intestinal juice at a volume ratio of 1:1, and the pH value of the system was adjusted to 7.5 with NaOH solution, and digestion was continued for 2 h.

[0089] During the artificial gastric juice and artificial intestinal juice digestion stages, samples were taken every 30 min. After adding 4-bromophenylboronic acid to the samples to inactivate the enzyme, tributyrin was extracted with 10 mL of n-hexane. The mixture was vortexed for 20 s and centrifuged at 17000g, 2°C for 20 min. The supernatant was collected and analyzed by gas chromatography.

[0090] like Figure 2 As shown, the solid preparations of tributyrin in each group did not rupture in the artificial gastric juice, and the cumulative release rate of tributyrin increased sharply after entering the artificial intestinal juice; while the cumulative release rate of tributyrin in the solid preparation of tributyrin obtained in Example 5 increased the slowest, which was lower than that of the solid preparation of tributyrin obtained in Comparative Examples 1-2 (P < 0.05).

[0091] (2) 0.1 g of each group of tributyrin solid preparation samples were placed in 10 mL of normal artificial intestinal fluid, and the pH value of the system was adjusted to 7.5 with NaOH solution. The samples were digested at 100 rpm / min for 2 h in a constant temperature water bath shaker at 37±0.5°C. 400 μL of the samples were taken every 30 min and placed in a centrifuge tube. 60 μL of 0.4% hydrochloric acid, 1 mL of methanol, and 0.5 g of anhydrous sodium sulfate were added. The samples were centrifuged at 17000 g, 2°C for 20 min, and the supernatant was collected for gas chromatography analysis.

[0092] like Figure 3 As shown, after each group of tributyrin solid preparations entered the artificial intestinal fluid, as tributyrin was continuously released, tributyrin was hydrolyzed by pancreatic lipase to produce butyric acid, thereby increasing the cumulative release rate of butyric acid; and the tributyrin solid preparation obtained in Example 5 had the slowest increasing rate of butyric acid cumulative release rate, which could effectively enable tributyrin to enter the colon and other areas.

[0093] A comparative test was conducted in a farm in Jiangxi Province, and 81 Duroc-Changda hybrid piglets weighing 18.9±1.3kg were selected and randomly divided into 3 groups, with 9 replicates in each group and 3 piglets in each replicate. Each group was fed with a corn-soybean meal type basic feed, and 2g / kg of the solid preparation of tributyrin obtained in Example 5 and Comparative Examples 1-2 was added to the basic feed, respectively, with a pre-feeding period of 1 week and a test period of 30 days.

[0094] All the experimental pigs were kept in the same pig house. The pig house was disinfected and isolated before feeding. They were allowed to eat and drink freely during feeding. The temperature of the pig house was controlled at around 25°C. The pig house was cleaned regularly to keep it clean. The status of the pigs was observed in time during feeding to identify any problems. Routine immunization of pigs was carried out according to the routine procedures of the pig farm.

[0095] On the 30th day of the experiment, 4 healthy piglets with a body weight close to the average body weight were randomly selected from each group, 5 mL of blood was collected from the anterior vena cava, the blood was placed in a 37°C water bath, and centrifuged at 3000 r / min for 10 min. The supernatant was used to measure the antioxidant indicators [total antioxidant capacity (T-AOC) and total superoxide dismutase (T-SOD) activity].

[0096] On the 30th day of the experiment, two healthy piglets with a body weight close to the average body weight were randomly selected from each replicate. After fasting for 12 hours, fresh rectal feces were collected in a sterile environment (live collection) and stored at 4°C for fecal flora analysis.

[0097] The plate count method was used to determine the lactic acid bacteria and Escherichia coli in rectal feces, and the test results were expressed as the logarithm of the total number of colonies per gram of feces, lgCFU / g.

[0098] like Figure 4 and Figure 5 As shown, the antioxidant capacity of the piglets in Example 5 was the best, the number of lactic acid bacteria was the highest, and the number of Escherichia coli was the lowest, which was better than that in the comparative examples 1-2 (P < 0.05).

[0099] The applicant believes that this is because the present invention uses nanocellulose and chitosan to mix and acid-treat, so that the two have extremely high affinity and high dispersion uniformity, and then vinyl triethoxysilane lipophilic treatment, which can not only make it have extremely high loading capacity for tributyrin, but also make the product have high dispersion uniformity in fatty acids. Sodium tripolyphosphate and anionic surfactant are then dispersed in deionized water, added dropwise to preform a to form an oil-in-water microemulsion, and further added dropwise to preform c to form a water-in-oil-in-water system, wherein the temperature is controlled at 40-50°C to promote cross-linking of the internal microemulsion interface, effectively enhancing the stability of the internal microemulsion during the stirring process. Since sodium carboxymethyl cellulose swells and tends to adsorb on the oil / water interface, the water-in-oil-in-water system not only has a spatial stabilizing effect, but the surface of hyperbranched polylysine contains amino groups, which can produce electrostatic adsorption with carboxymethyl cellulose, making the multiple emulsion system extremely stable, especially conducive to subsequent spray drying to obtain microcapsule preparations, improving the odor problem of tributyrin, making it easier for livestock and poultry to eat, and at the same time, it is not easily decomposed by gastric acid, and is mainly decomposed in the hind intestine to improve the health of the intestine.

[0100] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A solid preparation of tributyrin, characterized in that: The raw materials include, by mass, 50-80 parts of tributyrin, 2.5-4.5 parts of nanocellulose, 1-1.7 parts of chitosan, 1-1.8 parts of vinyl triethoxysilane, 10-20 parts of fatty acid, 1-1.8 parts of sodium alginate, 1-2 parts of hyperbranched polylysine, 1-1.8 parts of emulsifier, 0.01-0.1 parts of sodium tripolyphosphate, 1-2 parts of sodium carboxymethyl cellulose, 1-1.8 parts of calcium chloride and 3-6 parts of anionic surfactant.

2. The solid preparation of tributyrin according to claim 1, characterized in that: The number of generations of hyperbranched poly-lysine is 4.0-6.

0.

3. The solid preparation of tributyrin according to claim 1, characterized in that: The emulsifier is at least one of cocamidopropyl betaine, Span and Tween.

4. The solid preparation of tributyrin according to claim 1, characterized in that: The anionic surfactant is sodium dodecylbenzene sulfonate and / or sodium dodecyl sulfate.

5. A method for preparing the solid preparation of tributyrin according to any one of claims 1 to 4, characterized in that: The steps include: S1. Add nanocellulose and chitosan to water, perform ultrasonic treatment at 50-60°C for 5-15min, adjust the pH value of the system to 4-5, stir for 1-2h, add vinyl triethoxysilane and continue stirring for 1-3h, freeze at -40 to -60°C for 10-15h, freeze-dry, crush, add tributyrin and fatty acid mixture, perform ultrasonic treatment for 1-2h, add sodium alginate, hyperbranched polylysine and emulsifier, stir for 5-15min, and obtain preform a; S2, adding sodium tripolyphosphate and anionic surfactant into deionized water and stirring evenly to obtain prefabricated material b; S3, adding sodium carboxymethyl cellulose, calcium chloride, and anionic surfactant into deionized water and stirring evenly to obtain preform c; S4. Add preform b dropwise to preform a and stir for 5-15 min at a stirring temperature of 5-15°C. Add the product dropwise to preform c and stir for 10-20 min at a stirring temperature of 40-50°C. Allow to stand for 5-10 h in an environment of 70-80°C and 65-75% RH, and spray dry.

6. The method for preparing the solid preparation of tributyrin according to claim 5, characterized in that: In S1, nanocellulose and chitosan are added to water and then ultrasonically treated. The frequency of this ultrasonic treatment is 10-20 kHz.

7. The method for preparing the solid preparation of tributyrin according to claim 5, characterized in that: In S1, an acetic acid aqueous solution with a concentration of 1-2 mol / L is used to adjust the pH value of the system to 4-5.

8. The method for preparing the solid preparation of tributyrin according to claim 5, characterized in that: In S1, tributyrin and fatty acids are added and then ultrasonically treated. The frequency of the ultrasonic treatment is 5-15 kHz and the temperature of the ultrasonic treatment is 40-60°C.

9. The method for preparing the solid preparation of tributyrin according to claim 5, characterized in that: In S4, the feed rate of the spray drying is 500 mL / h, the inlet temperature is 150-160°C, and the outlet temperature is 70-80°C.

10. A feed additive, characterized in that: include: The tributyrin solid preparation according to any one of claims 1 to 4.

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