CN112641001B - Tianti-coating composite acidifier - Google Patents
Tianti-coating composite acidifier Download PDFInfo
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- CN112641001B CN112641001B CN202011475246.6A CN202011475246A CN112641001B CN 112641001 B CN112641001 B CN 112641001B CN 202011475246 A CN202011475246 A CN 202011475246A CN 112641001 B CN112641001 B CN 112641001B
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/30—Feeding-stuffs specially adapted for particular animals for swines
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/105—Aliphatic or alicyclic compounds
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/163—Sugars; Polysaccharides
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K40/00—Shaping or working-up of animal feeding-stuffs
- A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K50/00—Feeding-stuffs specially adapted for particular animals
- A23K50/60—Feeding-stuffs specially adapted for particular animals for weanlings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The composite acidifier is a combination of fumaric acid and potassium diformate, and comprises a pill-carrying core and an acid insoluble resin coating layer; the weight ratio of the fumaric acid to the potassium diformate is 6: (2-6). The coated compound acidulant can reduce the absorption rate of acidulant in stomach and improve the absorption uniformity in small intestine and large intestine.
Description
Technical Field
The invention belongs to the technical field of animal feed additives, and relates to a tie-coat compound acidifier.
Background
In recent years, the pig raising industry in China is in a situation of insufficient supply as a whole due to the influence of environmental protection, epidemic situation and cost of upstream raw feed. In order to maximize the reproductive performance of adult sows, a method for early weaning of piglets (3-4 weeks old) is generally adopted. However, since the digestive system of piglets is not yet developed, the nervous and endocrine regulation system is not yet fully established at this time.
Within 3-4 weeks after weaning, the lactic acid yield in the digestive tract of piglets is greatly reduced, and the endogenous gastric acid secretion is insufficient to compensate for the reduction of lactic acid; furthermore, part of gastric acid is easy to combine with feed raw materials. The pH value of the alimentary canal of the weaned piglets is higher than the level after weaning, and in addition, pathogenic microorganisms, inadaptation of feeding environment and other factors, the stress response of the piglets can be caused in the transition stage from the feeding of breast milk to the feeding of solid feed, including poor appetite, slow growth speed, diarrhea rate and death rate increase after weaning. These stress responses are collectively referred to as "early weaning stress syndrome".
In order to prevent and treat the above stress response of piglets, antibiotics are generally added to pig feed to control inflammatory response caused by various infections other than viral diseases. However, the use of antibiotics is twofold, brings great benefits, and also circulates into the human body through food intake, environmental residues and other modes, thereby endangering the health and environmental safety of the human body. Under such a large background, the world has been increasingly subjected to quite strict laws and regulations for the use of antibiotics in livestock and poultry farming. Taking the European Union as an example, the addition of antibiotic growth-promoting feed additives to animal-derived foods was completely prohibited in 2006. The national veterinary drug (antibacterial drug) comprehensive treatment five-year action scheme (2015-2019) of the export of China comprehensively prohibits the addition of antibiotics in the feed. Thus, there is an increasing demand for efficient and food-safe antibiotic alternatives (abbreviated as "tie") by livestock producers.
As antibiotic substitutes, more plant extracts (e.g., chinese herbal medicines and essential oils), microbial agents (e.g., enzyme preparations and probiotics), acidulants (e.g., inorganic and organic acids and salts thereof), and metal ion-based antibacterial agents (e.g., high zinc and high copper products), etc. are used.
Chinese patent CN107319131B discloses a preparation method and application of a natural anti-functional feed additive, the natural anti-functional feed additive is an amorphous powder solid preparation containing anti-drug-resistant bacteria and anti-inflammatory components, the amorphous powder solid preparation comprises the following components in weight ratio of 2:1, peony seed meal powder and soybean meal powder; wherein the peony seed meal contains 2.5-3.0% of anti-drug-resistant bacteria and anti-inflammatory components. The invention discloses a natural anti-G feed additive, which comprises the following raw materials in percentage by weight + Bacteria positive bacteria and simultaneously has bactericidal effect. The feed additive provided by the invention is used for livestock and even ruminants, can improve the growth performance, and has an antibiotic-like effect. However, the invention needs to squeeze oil from peony seed fruits and soybeans by screw squeezing, pulverize and screen the rest cake, mix, oven dry and sterilize to obtain amorphous powder solid preparation, the whole process is complex, and the process applicability is complex.
The Chinese patent application CN109511811A discloses a medium-short chain fatty acid essential oil preparation for a tiepiece and a preparation method and application thereof, wherein the medium-short chain fatty acid essential oil preparation for a tiepiece is mainly prepared from the following raw materials, by weight, 5-20 parts of formic acid, 5-20 parts of butyric acid, 1-5 parts of caproic acid, 1-5 parts of caprylic acid, 1-5 parts of capric acid, 5-20 parts of lauric acid, 3-10 parts of ammonia gas, 5-15 parts of glycerin, 1-5 parts of oregano oil and 20-40 parts of silicon dioxide, and the medium-short chain fatty acid essential oil preparation for a tiepiece can replace antibiotics to play a good role of sterilization and bacteriostasis, promote animal growth and avoid environmental pollution. However, the short-chain fatty acid essential oil preparation in the tiepin contains up to 6 acid types, and contains gas raw materials such as ammonia gas and solid raw materials of silicon dioxide, so that the formula stability is unsatisfactory.
In summary, acidulants are preferred antibiotic substitutes from the standpoint of the formulation stability and process suitability of the feed additives.
The acidulant includes organic acidulant and inorganic acidulant. The former is mainly citric acid, fumaric acid, lactic acid, formic acid, propionic acid, etc.; the organic acid has good flavor and can directly enter the tricarboxylic acid cycle in the body. The latter mainly comprises sulfuric acid, hydrochloric acid, phosphoric acid and the like; the inorganic acid has better pH value reduction and sterilization effects.
However, whatever acidulant is, it is corrosive and affects mineral metabolism in animals. In addition, the acidulant has the defect of unstable use effect, and mainly comprises the following components: the acidifier has high absorption speed in the stomach, and can inhibit gastric acid secretion and normal development of gastric functions; the acidulant only has a small part reaching the small intestine and the large intestine, can not effectively reduce the pH value in the small intestine, and is difficult to inhibit the growth of escherichia coli.
In view of the above-mentioned technical drawbacks, there is still a need to find a tiepiece coating acidulant which can not only reduce the absorption rate of acidulant in the stomach but also improve the absorption uniformity in the small and large intestines.
On the other hand, there are few complex acidulants in the prior art. The acidulant can realize broad-spectrum bacteriostasis and bacteriostasis function in a wider pH value range. Different kinds of acidulants have different effects on the palatability of the feed.
The inventor has found through scientific investigation that as a compound acidulant, a document report of a combination of both fumaric acid and potassium diformate has not yet been found. However, the addition of organic acid to the ration of weaned pigs is known to improve the productivity of the pigs; potassium diformate is the first non-antibiotic feed additive approved by the european union for replacement of antibiotics. Both have the functions of resisting bacterial infection, improving the nutrient digestibility of feed and the like, and have obvious growth promoting effect on piglets and growing-finishing pigs.
The inventor finds that the effect of the composite acidulant obtained by combining the two is better than that of a single acidulant in improving the production performance of animals.
In combination with the above two reasons, there is a need to find a coated composite acidulant for use as an anti-oxidant which can not only reduce the absorption rate of acidulant in the stomach but also improve the absorption uniformity in the small and large intestines.
Disclosure of Invention
The invention aims to provide an anti-coating compound acidifier. The tiepin coating compound acidifier can reduce the absorptivity of the acidifier in the stomach and improve the absorption uniformity in the small intestine and the large intestine. In particular, the absorption rate of the acidulant in the stomach is reduced to below 10%, while the absorption rates in the small intestine and the large intestine are both above 30%. The absorption characteristic can effectively reduce the pH value in the small intestine and inhibit the growth of escherichia coli.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a coated composite acidulant which is a combination of fumaric acid and potassium diformate, characterized in that the coated composite acidulant comprises a pill-carrying core and an acid insoluble resin coating.
The coated composite acidulant of the present invention, wherein the weight ratio of fumaric acid to potassium diformate is 6: (2-6).
Preferably, the weight ratio of fumaric acid to potassium diformate is 6: (3-5).
In a specific embodiment, the weight ratio of fumaric acid to potassium diformate is 3:2.
the coated composite acidulant of the invention, wherein the solid materials of the pellet-carrying core include composite acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose.
The coated composite acidulant of the invention, wherein the weight ratio of the composite acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose is (25-35): (25-35): (2-6): (6-10): (24-32).
Preferably, the weight ratio of the composite acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose is (20-30): (20-30): (3-5): (7-9): (26-30).
In a specific embodiment, the weight ratio of the compound acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose is 25:25:4:8:28.
the coated composite acidulant of the present invention, wherein the pellet-carrying core is prepared by mixing the solid raw materials and binder to prepare a soft mass and then performing an extrusion-spheronization operation.
The coated composite acidulant of the present invention, wherein the binder is selected from 0.5-4wt% hydroxypropyl methylcellulose (HPMC E3) aqueous solution; the addition amount is 20-50v% of the solid material volume.
Preferably, the binder is selected from 1-3wt% hpmc E3 in water; the addition amount is 30-40v% of the solid material volume.
In a specific embodiment, the binder is selected from the group consisting of 2wt% aqueous hpmc E3; the addition amount is one third of the volume of the solid material.
The coated composite acidulant of the present invention, wherein the acid insoluble resin is selected from acrylic resins that are insoluble at a pH of 5 or less.
Preferably, the acid-insoluble resin is selected from acrylic resins that are insoluble at a pH of 5.5 or less.
In a specific embodiment, the acid-insoluble resin is selected from acrylic resins that are insoluble at a pH of 6 or less.
The coated composite acidulant according to the present invention, wherein the acrylic resin is selected from the group consisting of Eudragit L100 and Eudragit S100; the weight ratio of the two is (4-8): (2-4).
Preferably, the acrylic resin is selected from the group consisting of Eudragit L100 and Eudragit S100 in combination; the weight ratio of the two is (5-7): (2.5-3.5).
In a specific embodiment, the acrylic resin is selected from the group consisting of Eudragit L100 and Eudragit S100; the weight ratio of the two is 2:1.
the coating compound acidifier of the invention, wherein the coating liquid of the acid insoluble resin coating layer is: 6-12 parts by weight of acrylic resin; 80-120 parts by weight of 90v% ethanol aqueous solution; 1-3 parts of talcum powder; 0.5 to 1.5 weight portions of triethyl citrate.
Preferably, the coating liquid of the acid-insoluble composite resin coating layer is: 8-10 parts of acrylic resin; 90-110 parts by weight of a 90v% ethanol aqueous solution; 1.5-2.5 parts of talcum powder; 0.8-1.2 parts by weight of triethyl citrate.
In a specific embodiment, the coating solution of the acid-insoluble resin coating layer is: 9 parts by weight of an acrylic resin; 100 parts by weight of a 90v% ethanol aqueous solution; 2 parts of talcum powder; 1 part by weight of triethyl citrate.
The coated composite acidulant of the present invention, wherein the acid insoluble resin coating has a weight gain of 18-26wt%.
Preferably, the acid insoluble resin coating weight gain is 20-24wt%.
In a specific embodiment, the acid insoluble resin coating weight gain is 22wt%.
The preparation method of the coating compound acidulant comprises the following steps:
mixing the solid raw materials with the adhesive to prepare a soft material, and performing extrusion-spheronization operation to prepare a pill carrying core;
and (3) using coating liquid to carry out bottom spray coating on the drug-loaded pellets to prepare the coated composite acidifier.
The preparation method of the invention, wherein the technological parameters of the rounding operation are as follows: the rolling speed is 300-700rpm, and the rolling time is 1-5min.
Preferably, the rounding speed is 400-600rpm and the rounding time is 2-4min.
In a specific embodiment, the spheronization speed is 500rpm and the spheronization time is 3 minutes.
The preparation method of the invention, wherein the technological parameters of the bottom spray coating are as follows: the air inlet temperature is 40-60 ℃, the material temperature is 35-55 ℃, the working frequency is 40-60Hz, the spraying pressure is 0.08-0.18MPa, and the spraying speed is 0.5-1.5mL/min.
Preferably, the air inlet temperature is 45-55 ℃, the material temperature is 40-50 ℃, the working frequency is 45-55Hz, the spraying pressure is 0.1-0.15MPa, and the spraying speed is 0.8-1.2mL/min.
In a specific embodiment, the air inlet temperature is 50 ℃, the material temperature is 45 ℃, the working frequency is 50Hz, the spraying pressure is 0.12MPa, and the spraying speed is 1mL/min.
The beneficial technical effects of the invention are as follows: the tiepiece coating compound acidulant can reduce the absorption rate of acidulant in stomach and improve the absorption uniformity in small intestine and large intestine; in particular, the absorption rate of the acidulant in the stomach is reduced to below 10%, while the absorption rates in the small intestine and the large intestine are both above 30%. The absorption characteristic can effectively reduce the pH value in the small intestine and inhibit the growth of escherichia coli.
Without wishing to be bound by any theory, the particular formulation of the pill-carrying core and coating layer produce a synergistic effect, thereby achieving the above-described effect.
Detailed Description
The examples are presented for better illustration of the present invention, but are not intended to limit the scope of the present invention to the examples.
Example 1
The weight ratio of the fumaric acid to the potassium diformate is 3:2, mixing to form the compound acidulant. According to 25:25:4:8:28, sieving a compound acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose through a 100-mesh sieve, uniformly mixing, and then adding a 2wt% hydroxypropyl methylcellulose (HPMC E3) aqueous solution with the volume of one third of the solid material to prepare a soft material. Placing the uniformly mixed soft material into an extrusion-spheronization machine, and extruding the soft material into a strip-shaped soft material through a screen with the aperture of 0.8mm at the rotating speed of 50 rpm; then rounding the strip-shaped soft material; the rolling rotation speed is 500rpm, and the rolling time is 3min; obtaining the drug-loaded pellets with high sphericity. And drying the drug-loaded pellets at 50 ℃ for 2 hours, and sieving and retaining the drug-loaded pellets with 20-30 meshes.
Taking 6 parts by weight and 3 parts by weight of Eudragit L100 and Eudragit S100 respectively, adding the 6 parts by weight and the 3 parts by weight into 100 parts by weight of 90v% ethanol water solution, and stirring the mixture to completely dissolve the mixture; and adding 2 parts by weight and 1 part by weight of talcum powder and triethyl citrate respectively, and uniformly mixing to obtain the coating liquid. And (3) placing the drug-loaded pellets into a fluidized bed granulating and coating machine for bottom spray coating, and controlling the weight gain of the coating to be 22wt%. The air inlet temperature is 50 ℃, the material temperature is 45 ℃, the working frequency is 50Hz, the spraying pressure is 0.12MPa, and the spraying speed is 1mL/min. The coating process is to continuously stir the coating solution, and the coating solution is dried for 10min at 50 ℃ after coating, so as to obtain the tianti-coating compound acidifier of the example 1.
Comparative example 1
Other conditions were the same as in example 1 except that Eudragit L100 was not used, and only Eudragit S100 parts by weight was taken.
Comparative example 2
Other conditions were the same as in example 1, except that the drug-loaded pellets were not subjected to the coating operation.
Digestion and absorption test
The invention firstly refers to Chen Liang et al (China agricultural science, 2013, 46 (15), 3199-3205) and evaluates the influence factors of the dry matter digestibility of the feed by a bionic method to prepare simulated pig gastric juice, pig small intestine juice and pig large intestine juice, pig gastric buffer, small intestine buffer and large intestine buffer. The digestibility of inventive example 1 and comparative examples 1-2 was then evaluated on a monogastric biomimetic digestive system SDS-2. After the digestion period of each stage is finished, 1mL of buffer solution is accurately sucked, and the buffer solution is placed in a 10mL volumetric flask, and the volume is fixed to the scale by using 0.4wt% phosphoric acid solution. 20. Mu.L of the solution was poured into the liquid chromatograph using a pipette. The chromatographic conditions are as follows: c18 silica gel column (250 mm. Times.4.6mm. Times.5 μm), 0.4wt% phosphoric acid solution-methanol (80:20), detection wavelength 210nm; the flow rate is 1mL/min; column temperature: 25 ℃. Calculating the absorptivity of the fumaric acid in the stomach, the small intestine and the large intestine of the pig by using a standard reference substance according to an external standard method; further, considering that potassium diformate has been largely decomposed into formic acid and potassium formate in the small intestine and large intestine, its absorption rate in the small intestine and large intestine is calculated by using respective controls of potassium diformate and potassium formate and then calculated by adding them.
The results are shown in Table 1.
TABLE 1
As a result, it can be seen that the tibetan coated composite acidulant according to example 1 of the present invention can not only reduce the absorption rate of acidulant in the stomach but also improve the absorption uniformity in the small and large intestines, as compared with comparative examples 1-2. The absorption characteristic can effectively reduce the pH value in the small intestine and inhibit the growth of escherichia coli.
It should be understood that the description of the specific embodiments is merely illustrative of the principles and spirit of the invention, and not in limitation thereof. Further, it should be understood that various changes, substitutions, omissions, modifications, or adaptations to the present invention may be made by those skilled in the art after having read the present disclosure, and such equivalent embodiments are within the scope of the present invention as defined in the appended claims.
Claims (1)
1. A coated composite acidulant which is a combination of fumaric acid and potassium diformate, characterized in that the coated composite acidulant consists of a pill-carrying core and an acid-insoluble resin coating layer;
wherein the weight ratio of the fumaric acid to the potassium diformate is 6: (2-6);
the solid raw materials of the pill carrying core comprise a compound acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose; the weight ratio of the composite acidulant, corn starch, sodium carboxymethyl starch, white carbon black and microcrystalline cellulose is (25-35): (25-35): (2-6): (6-10): (24-32);
the pill carrying core is prepared by mixing the solid raw materials and the adhesive to prepare a soft material and then performing extrusion-spheronization operation; the binder is selected from 0.5-4wt% hydroxypropyl methylcellulose HPMC E3 aqueous solution; the addition amount is 20-50% of the volume of the solid material;
the acid insoluble resin is selected from the group consisting of Eudragit L100 and Eudragit S100; the weight ratio of the two is (4-8): (2-4);
the coating liquid of the acid insoluble resin coating layer is as follows: 6-12 parts by weight of acrylic resin; 80-120 parts by weight of 90v% ethanol aqueous solution; 1-3 parts of talcum powder; 0.5-1.5 parts by weight of triethyl citrate; the weight gain of the acid insoluble resin coating layer is 18-26wt%.
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| CN112641001B true CN112641001B (en) | 2023-08-04 |
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| CN114431339B (en) * | 2022-02-14 | 2023-06-27 | 浙江汇能生物股份有限公司 | Low-additive stability-increasing microencapsulated potassium diformate feed additive and preparation method thereof |
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