Nano oxidized zinc preparation of a kind of enteric and preparation method thereof
Technical field
The invention belongs to feed addictive formulation art, relate to a kind of enteric sodium rice zinc oxide preparation and preparation technology thereof.
Background technology
Zinc is the indispensable element of animal, is the constituent of 40 various metals enzymes in body, the activity factor of more than 200 kind of enzyme, participates in nucleic acid and protein synthesis, energetic supersession, redox, cellular immunity and humoral immunity process.In addition, report is had to point out: zinc has the effect promoting lingual mucous membrane taste buds cell rapid regeneration, whet the appetite.
No. 1224th, Ministry of Agriculture bulletin " feed addictive safe handling specification " specifies: in sucking pig material, the most high-load of zinc must not more than 2250mg/kg, and this zinc must be the zinc derived from zinc oxide, the piglet of first 2 weeks after this high zinc dietary can only be used for weaning.The feed of other supplementary zinc is generally without zinc oxide.And concentration is no more than 150mg/kg.
Add zinc in early-weaned piglets daily ration and can reduce piglet white scour, improve daily gain, improve the price of deed.Because antibiotic use is more and more restricted, although zinc salt absorption rate is low, because it has good antibacterial and bacteriostasis, therefore cause the abuse of zinc aborning.It is reported, because high zinc is to the effect that to prevent diarrhea of weaned piglets from playing very large, present feed producer mostly uses high zinc in case piglet white scour diarrhoea in weanling pig daily ration, and its addition has exceeded animal normal needs more than 20 times, even higher.
At present, great majority research report is thought, only the high zinc in zinc oxide source has anti-diarrhea and growth promoting function, but report that the bioavailability of zinc oxide in various zinc source is minimum, weanling pig is about 5% ~ 10% simultaneously, wherein major part is discharged from excrement, be not utilized, severe contamination is caused to environment.Infer according to Japanese relevant expert, if zinc is all stayed in soil in all pig manures, Zn content will exceed standard in 17 years (120 milligrams every kilogram), and contaminated soil no longer will have arability.
Nano zine oxide is a kind of novel high function fine inorganic product geared to the 21st century.Its particle diameter is between 1nm ~ 100nm, and also known as ultra-fine zinc oxide, Product Activity is high, has the function of shielding infrared ray, ultraviolet and sterilization.In the sun, the electronegative electronics that especially energy disintegrate goes out to move freely under ultraviolet irradiation, leaves the hole of positively charged to nano-zinc oxide powder simultaneously.The oxygen that this hole can be activated in air becomes active oxygen, has extremely strong chemism, can with gas chromatography generation oxidation reaction (comprising the organic matter in bacterium), thus most germs and virus to be killed.Relevant quantitative test shows: when in 5min, nano oxidized zinc concentration is 1%, and the sterilizing rate of staphylococcus aureus is 98.86%, and colibacillary sterilizing rate is 99.93%.
Although nano zine oxide can improve bacteriostasis, and then there is the ability of stronger suppression diarrhoea, but, due to when nano zine oxide is by piggy gastric acid environment, can by pH lower than 3.5 gastric acid environment dissolve, generate zinc chloride and water, thus lose the original speciality of zinc oxide.Therefore, the antibacterial anti diar rhea performance how allowing nano zine oxide good really plays in enteron aisle, remains a very promising research direction.
Application number is the Chinese invention patent of 201310535833.3, disclose a kind of novel fodder additive and preparation method thereof, its technical scheme is specific as follows: this additive comprises enteric nano granular of zinc oxide, and this particle is respectively nano zine oxide core grain, too small enteric coating layer, the nano oxidized zinc layers in middle level from inside to outside and crosses stomach coatings; The constituent of described nano granular of zinc oxide is nano zine oxide, maltodextrin and HPMC; The constituent of described too small enteric coating layer is ethyl cellulose and Ac-Di-Sol; The constituent of the nano oxidized zinc layers in described middle level is nano zine oxide; The described constituent crossing stomach coatings is acrylic resin, Ac-Di-Sol and Hydroxypropyl methylcellulose.This technology protects nano zine oxide not by stomach acids destroy by double-layer coatings; divide two sections after entering enteron aisle to discharge; in small intestine (more than pH=5.5) release about 30%, in colon (more than pH=6.7) release about 70%, thus ensure the maximum service efficiency of nano zine oxide.The present inventor studies confirmation, and in this technical scheme, the final disintegration of enteric nano granular of zinc oxide may be influenced.
Summary of the invention
The present invention will solve the problems of the technologies described above, thus provides a kind of enteric nano oxidized zinc preparation, and it can not only protect microballoon ball core from the destruction of gastric juice, and can also ensure that microballoon ball core can disintegration in intestines.
The technical scheme that the present invention solves the problem is as follows:
The nano oxidized zinc preparation of a kind of enteric, comprises microballoon ball core, isolation coat layer, enteric coat layer from inside to outside successively; Described microballoon ball core is through throwing the 30-40 object spheric granules that circular knitting machine is made after being mixed with pharmaceutic adjuvant by Nano-class zinc oxide; Described isolation coat layer is made up when fluidized coating machine sprays described microballoon ball core of dextrin in aqueous solution; Described enteric coat layer by middle product 2 by the bottom of dressing spray system enteric coating is carried out to the microballoon ball core possessing isolation coat layer time make; Described middle product 2 are dissolved in food-grade alcohol are made by enteric resin 2, No. 3, enteric resin, talcum powder, PEG.
Preferred as technique scheme, described pharmaceutic adjuvant is one or more in sodium carboxymethyl starch, methylcellulose, Hydroxypropyl methylcellulose, hydroxypropyl cellulose; The mass ratio of described Nano-class zinc oxide and pharmaceutic adjuvant is 5 ~ 8:1.
Preferred as technique scheme, in raw material for the preparation of described middle product 2, composition and mass parts thereof are specially, enteric resin No. 22 ~ 4 parts, enteric resin No. 32 ~ 4 parts, talcum powder 2 ~ 4 parts, PEG6000 1 ~ 2 part, food-grade alcohol 90 ~ 100 parts.
Preferred as technique scheme, described pharmaceutic adjuvant is sodium carboxymethyl starch, and the mass ratio of described Nano-class zinc oxide and pharmaceutic adjuvant is 7:1; In raw material for the preparation of described middle product 2, composition and mass parts thereof are specially, enteric resin No. 23 parts, enteric resin No. 33 parts, talcum powder 3 parts, PEG6000 1 part, food-grade alcohol 90 parts.
Another object of the present invention is to provide the method for making of the nano oxidized zinc preparation of above-mentioned a kind of enteric.
Its technical scheme is specific as follows:
A preparation method for the nano oxidized zinc preparation of enteric, comprises pill, isolation coat and enteric coating operation; By pill, nano-zinc oxide powder is made to make circular microballoon ball core; By isolation coat, stop enteric coating liquid to contact with the direct of nano zine oxide raw material, avoid the disintegration affecting ball core; By the outer spray dressing of enteric coating liquid, manufactured goods are not dissolved in gastric juice, and effectively dissolve in intestinal environment, and all have good water-soluble owing to making microballoon ball core and isolation coat auxiliary material used, ball core can be discharged rapidly after dissolving in enteron aisle, nano zine oxide can be played one's part to the full in enteron aisle.
Preferred as technique scheme, comprises the following steps:
A) Nano-class zinc oxide is mixed with pharmaceutic adjuvant, obtain middle product 1;
B) enteric resin 2, No. 3, enteric resin, talcum powder, PEG are dissolved in food-grade alcohol, obtain middle product 2;
C) dextrin is soluble in water, product 3 in the middle of obtained;
D) appropriate middle product being added for 1 time in throwing circular knitting machine, by throwing circular knitting machine spray gun, purified water being added, until product formation 30-40 object spheric granules, sieve and to obtain product 4 in the middle of 30-40 order;
E) the middle product 4 after repeatedly throwing circle add in fluidized coating machine, and start seed-coating machine, air intake, carries out drying to middle product 4, and on-line period detects moisture content and is not more than 3%;
F) middle product 3 are passed through spray system at the bottom of dressing, isolation coat is carried out to dried middle product 4, until all spraying is complete; Continue fluidized drying 30-60 minute;
G) adjusting EAT is 45-50 degree, by middle product 2 by spray system at the bottom of dressing, carries out enteric coating to the above-mentioned middle product being isolated dressing drying; Dressing terminates, and adjustment EAT is 65-70 degree, carries out drying, obtains finished product.
As technique scheme further preferably, specifically comprise the following steps:
A) mixed with sodium carboxymethyl starch by Nano-class zinc oxide, the mass ratio of Nano-class zinc oxide and sodium carboxymethyl starch is 7:1, obtains middle product 1;
B) enteric resin No. 2 3%, enteric resin No. 3 3%, talcum powder 3%, PEG6000 1% are dissolved in 95% food-grade alcohol, obtain middle product 2;
C) dextrin is soluble in water, the mass ratio of dextrin and water is 1:2, product 3 in the middle of obtained;
D) start spherical throwing circular knitting machine, rotating speed is adjusted to 25-35 rev/min, is added for 1 time by appropriate middle product and throws in circular knitting machine, by throwing circular knitting machine spray gun, purified water being added, until product formation 30-40 object spheric granules, sieving and to obtain product 4 in the middle of 30-40 order;
E) the middle product 3 after throwing circle add in fluidized coating machine, and start seed-coating machine, air intake 80 DEG C, carries out drying 1 hour to middle product 4, and on-line period detects moisture content and is not more than 3%;
F) dextrin solution of middle product 3 is passed through spray system at the bottom of dressing, isolation coat is carried out to dried middle product 4, until all spraying is complete, continue fluidized drying 30-60 minute;
G) adjusting EAT is 45-50 DEG C, and by middle product 2 by spray system at the bottom of dressing, carry out enteric coating to the above-mentioned middle product being isolated dressing drying, dressing terminates, and adjustment EAT is 65-70 DEG C, carries out drying, obtains finished product.
The main feature of this technique is:
(1) with pill art for coating, enteric coating process is carried out to nano zine oxide, enable nano zine oxide have more than 80% by piggy gastric juice, reach small intestine disintegration;
(2) this product formulation technique comprises pill, isolation coat and enteric coating operation; By pill, nano-zinc oxide powder is made to make circular microballoon ball core; By isolation coat, stop enteric coating liquid to contact with the direct of nano zine oxide raw material, avoid the disintegration affecting ball core; By the outer spray dressing of enteric coating liquid, manufactured goods are not dissolved in gastric juice, and when pH is greater than 5.5, namely can effectively dissolve in intestinal environment, thus release ball core.Circular microballoon ball core and isolation coat material therefor all have well water-soluble, make ball core undergoes rapid expansion after chance water, thus realize the release of nano zine oxide, play one's part to the full at small intestine.
Detailed description of the invention
This detailed description of the invention is only explanation of the invention, is not limitation of the present invention.Any change that those skilled in the art are done after having read description of the present invention, as long as in the scope of claims, all will be subject to the protection of Patent Law.
embodiment: the preparation method of 70% nano zine oxide feed addictive preparation
Raw material and auxiliary material: 70 kg diet level nano zine oxide raw materials, 10 kilograms of CMSs are received, 10 kilograms of dextrin, enteric resin No. 23 kilograms, enteric resin No. 33 kilograms, talcum powder 3 kilograms, PEG6000 1 kilogram, 95% food-grade alcohol 90 kilograms and purified water some.
Capital equipment: spherical throwing circular knitting machine, fluidized coating machine.
The preparation first step, mixes above-mentioned Nano-class zinc oxide with sodium carboxymethyl starch, obtains middle product 1;
Prepare second step, above-mentioned No. 2,3 kilograms of enteric resins, 3 kilograms of enteric resins No. 3,3 kilograms talcum powder, 1 kilogram of PEG6000 are dissolved in 90 kilogram of 95% food-grade alcohol, obtain middle product 2;
Prepare the 3rd step, above-mentioned 10 kilograms of dextrin are dissolved in 20 kg of water, product 3 in the middle of obtained;
Prepare the 4th step, start spherical throwing circular knitting machine, rotating speed is adjusted to 25-35 rev/min, is added for 1 time by appropriate middle product and throws in circular knitting machine, (every batch of 5-10 kilogram, depending on throwing circular knitting machine production capacity); By throwing circular knitting machine spray gun, purified water added, until product formation 30-40 object spheric granules, sieve to obtain the middle product 4 of 30-40 order;
Prepare the 5th step, the middle product 4 after repeatedly throwing circle add in fluidized coating machine, and dosage is determined depending on equipment dressing ability; Start seed-coating machine, EAT 80 degree, carries out drying 1 hour to middle product 4, and on-line period detects moisture content and is not more than 3%;
Prepare the 6th step, by the dextrin solution of middle product 3 by spray system at the bottom of dressing, isolation coat is carried out to dried middle product 4, until all spraying is complete; Continue fluidized drying 30-60 minute;
Prepare the 7th step, adjustment EAT is 45-50 degree, by middle product 2 by spray system at the bottom of dressing, carries out enteric coating to the above-mentioned middle product being isolated dressing drying; Dressing terminates, and adjustment EAT is 65-70 degree, carries out drying, obtains finished product.
comparative example
By the enteric nano granular of zinc oxide (this particle is respectively nano zine oxide core grain, too small enteric coating layer, the nano oxidized zinc layers in middle level and mistake stomach coatings from inside to outside) of zinc oxide, nano zine oxide, the nano oxidized zinc preparation of enteric (embodiment) that the embodiment of the present invention is produced and comparative example, in simulation simulated gastric fluid and simulated intestinal fluid, carry out disintegration rate mensuration, result is as follows.
The dissolution determination result of the different zinc oxide formulation products of table 1 in gastro-intestinal Fluid
the application of enteric nano zine oxide on animal
Choose Du × length × large piglet 216 of 21 age in days wean, be divided into 3 processed group, each group 6 repetitions, each repetition 12, control group is for containing zinc oxide daily ration, the enteric nano zine oxide that test group is produced at feed respectively nano zine oxide and the present embodiment substitutes control group zinc oxide, 21 days experimental periods.Experimental session is observed each group of swinery diarrhea rate, is searched for food and drinking-water situation, record feed consumption rate, measures the wean body weight of latter 21 days, calculates average daily gain, average daily ingestion amount and feed-weight ratio;
Experimental result is as table 1:
The nano oxidized zinc preparation of table 1 enteric is on the impact of Growth Performance of Weaning Piglets
The result of table 1 shows: add the average daily gain that enteric nano zine oxide of the present invention can significantly improve weanling pig, reduce feed-weight ratio, the consumption of enteric nano zine oxide only has the 33%(of common zinc oxide and nano zine oxide with oximeter), but suppress the effect of diarrhoea to be better than common zinc oxide and nano zine oxide, illustrate by formulation treatment process of the present invention, the action effect of zinc oxide can be significantly improved, zinc oxide can be played a role at enteron aisle, reduce the addition of zinc oxide in feed, reduce zinc oxide to the pollution of environment, be conducive to the sustainable development of animal husbandry.