CN101168734B - Coating micro-pill phytase and preparation method thereof - Google Patents
Coating micro-pill phytase and preparation method thereof Download PDFInfo
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Abstract
The invention relates to coated micro-pellets phytase and the preparation method thereof. The coated micro-pellets phytase of the invention comprises micro-pellets phytase and a coating layer, the grain size of the coated micro-pellets phytase is about 30 to 60 meshes, the grains are dense, and the volume weight is feasible, wherein, the micro-pellets phytase comprises carriers and phytase in an effective amount, and all carrier components in the general carrier quantity have the proportion that corn starch is 30 to 50 wt percent, corn cob meal is 10 to 30 wt percent, marble dust is 5 to 15 wt percent, and lactose is 10 to 25 wt percent; the coating layer comprises hydroxypropyl emthylcellulose, hydroxypropyl cellulose, polyacrylic acid resin, and polyvinylpyrrolidone, and the proportion of the components is 10 to 30 wt percent:10 to 30 wt percent:30 to 50 wt percent:10 to 30 wt percent. The invention also discloses the preparation method of the coated micro-pellets phytase. The invention handpicks unique modeling palletizing and coating material, can keep the stability of the enzyme activity when the phytase products are used and stored, and increases the capacity of resisting bad external environments of high temperature, high humidity, etc.
Description
Technical field
The present invention relates to a kind of coating micro-pill phytase and preparation method thereof.
Background technology
Phosphorus is one of growth of animal, breeding, bone calcification and the necessary mineral element of metabolism.Because the vital role of phosphorus is very important so competent phosphorus is provided in the animal daily ration.Though contain a large amount of phosphorus in the vegetality feedstuff, but have 60～80%, exist with the form of phytate phosphorus, decompose the required enzyme of phytate phosphorus and in monogastric animal and aquatic products, lack, the utilization ratio of phosphorus only 0～30%, so need to add the deficiency that a large amount of inorganic phosphorus replenishes phosphorus in feed, this has promptly caused rolling up of feed cost, the phytate phosphorus in the feed can not be utilized by animal simultaneously, be excreted in a large number outside the animal body, cause severe contamination soil and water.
Phytase is a kind of fodder enzyme preparation that the phytate phosphorus hydrolysis in the feed can be become inorganic phosphorus and inositol, is one of global research focus.It has obtained approval widely to the feeding effect of monogastric animal.Can reduce by 50～70% inorganic phosphorus consumption after adding phytase in the feed, the utilization ratio of phosphorus in the plant feed own is brought up to more than 60%, the output of phosphorus reduces more than 30～40% in the ight soil, and reduce the anti-oxidant action of phytate greatly, raising herding productivity effect, reduction environmental pollution are had great importance.
But some present phytase products, undesirable in aspects such as resistance, temperature tolerance performances, effect is subjected to certain influence.On the one hand, in the product storage process, the influence that is subjected to extraneous undesirable element such as high temperature, high humidity easily makes enzyme decline alive; On the other hand, in the feed course of processing, particularly in the pelletization, be subjected to the pyritous influence and enzyme lived descending, even complete deactivation.At present phytase resistance, durothermic raising are mainly contained two approach, one is to realize by strain improvement, but the making little progress of this respect, and is also continuing in the middle of the development at present; Realize by special art breading exactly on the other hand, use micropill and coated micropill complete processing can improve the resistance and the temperature tolerance of phytase largely, make phytase be more suitable in feed, using.Simultaneously, because phytase is a kind of acid hydrolase, only competence exertion effect under the sour environment in the animal stomach, therefore the sfgd. of taking must guarantee that also phytase can discharge rapidly under one's belt.
CN 1981597A discloses a kind of preparation method of high-temperature-resisting micropellet enzyme feed, and this method is made uniform micropill with one or more feeding enzymes with the round as a ball method of extruding, wraps high-temperature-resistant layer on the micropill enzyme surface then, makes high temperature resistant micropill.Though this method has improved enzyme and has tolerated in the feed course of processing and to granulate and the high temperature of extruding and keep good enzyme to live, the solvability of not mentioned micropill enzyme obtained by this method, the stability under the normal temperature, and the avidity of feed, coating rate etc.
CN 1775067A discloses a kind of production method of coated granule phytase, coated granule phytase flowability, dispersiveness, the temperature tolerance of this method preparation are good, but this method has been used the enteric coatings material, be difficult to dissolving under one's belt, only in small intestine, could dissolve and play a role, and enteron aisle neutral and alkali environment is unfavorable for the performance of phytase effect; The dissolution time of coating material is 30 minutes in addition, and the time is longer, and it is slower to play a role; The 3rd this method uses ethanol as the enteric film dissolved material, is easy to generate the pollution to product and environment; The 4th feed granulating temperature much reaches more than 85 ℃, and CN 1775067A method only relates to 80 ℃ the rate that retains.
The inventor is devoted to the research of phytase, preparation technology to coating micro-pill phytase, adjust and improve in selection and concrete processing parameter, obtain 30～60 order epigranulars, the regular coating micro-pill phytase in surface, thereby improved phytase resistance and temperature tolerance.
Summary of the invention
Therefore, the object of the present invention is to provide a kind of epigranular, the surface is regular and have excellent resistance and durothermic coating micro-pill phytase; Another object of the present invention is to provide the preparation method of above-mentioned coating micro-pill phytase.
Coating micro-pill phytase of the present invention is made up of micro-pill phytase and coatings, this coating micro-pill phytase granular size is 30～60 orders, wherein, described micro-pill phytase is made of carrier and significant quantity phytase, and carrier is made of the W-Gum of the 30wt%～50wt% that accounts for the carrier total amount, the corn cob meal of 10wt%～30wt%, the marble dust of 5wt%～15wt% and the lactose of 10wt%～25wt%; Described coatings is formed in 10wt%～30wt%: 10wt%～30wt%: 30wt%～50wt%: 10wt%～30wt% ratio by Vltra tears, hydroxy propyl cellulose, polyacrylic resin and polyvinylpyrrolidone; Weight ratio between micro-pill phytase and the coatings is 40～100: 1.
In the present invention, methoxy content is 19wt%～24wt% in the Vltra tears that is adopted, and hydroxypropyl content is 4wt%～12wt%, and preferred viscosities is 20～30mPa.s; Propoxyl content 60wt%～66wt% in the hydroxy propyl cellulose that is adopted, preferred viscosities is 1500～2500mPa.s; The relative density 0.810～0.820 of the polyacrylic resin that is adopted, base number 162～198, preferred viscosities is 5～200mPa.s; And the nitrogen content of the polyvinylpyrrolidone that is adopted (PVP) is 11.5wt%～12.8wt%, and preferred K value is 27～32.
The invention provides the preparation method of above-mentioned coating micro-pill phytase, this method comprises the steps:
1. the preparation of micro-pill phytase
Mix as the phytase carrier accounting for the W-Gum of the 30wt%～50wt% of phytase carrier total amount, the corn cob meal of 10wt%～30wt%, the marble dust of 5wt%～15wt% and the lactose of 10wt%～25wt%.With the phytase carrier and the phytase fermented liquid thorough mixing that mix, wherein phytase carrier and phytase fermented liquid account for this total mixture ratio and are respectively 40wt%～60wt% and 40wt%～60wt% then.The phytase fermented liquid is phytase generating bacterial strain process liquid submerged fermentation, the liquid fermentation production that utilizes cultures such as glucose, sulfate of ammoniac to produce, and principal constituent is moisture and phytase albumen.
Above-mentioned phytase carrier that mixes and phytase fermented liquid mixture input are waved nodulizer, and by the physics extruding, material is made and is about 3～5mm, the cylindrical particle of the about 1～3mm of diameter.
Throw circle then, and, form micro-pill phytase in 70～90 ℃ of oven dry down of inlet temperature.
2. dressing
Vltra tears, hydroxy propyl cellulose, polyacrylic resin and polyvinylpyrrolidone are mixed with the aqueous solution of 2wt%～5wt% in 10wt%～30wt%: 10wt%～30wt%: 30wt%～50wt%: 10wt%～30wt% ratio, the micro-pill phytase that adopts gunite that step 1 is obtained then wraps by film forming, oven dry then, the coating micro-pill phytase of 30～60 order sizes is collected in screening.
Be described more specifically preparation method of the present invention below:
In the preparation of step 1 micro-pill phytase, specifically comprise:
(1) mixing and absorption
Equipment: mixing machine
Prescription: according to W-Gum 30wt%～50wt%, corn cob meal 10wt%～30wt%, marble dust 5wt%～15wt%, lactose 10wt%～25wt% mixed.With above-mentioned phytase carrier and phytase fermented liquid thorough mixing, wherein phytase carrier and phytase fermented liquid account for the total mixture ratio and are respectively 40wt%～60wt% and 40wt%～60wt%, wherein the phytase fermented liquid is phytase generating bacterial strain process liquid submerged fermentation, the liquid fermentation production that utilizes cultures such as glucose, sulfate of ammoniac to produce, principal constituent is moisture and phytase albumen.
Method: earlier with various solid materialss thorough mixing 5min in mixing machine, add a certain amount of phytase fermented liquid then, start to stir and continue to mix 10min.
(2) granulate
Equipment: wave nodulizer
Method: material is added in the hopper of nodulizer, starting outfit is made material and is about 3～5mm, the cylindrical particle of the about 1～3mm of diameter.
(3) throw circle
Equipment: the spherical circular knitting machine of throwing
Method: the cylindrical particle material input of making is thrown in the inner chamber of circular knitting machine, starting outfit, the adjustment rotating speed is 400～600rpm, discharging after cylindrical particle becomes circular granular.
(4) oven dry
Equipment: cyclone fluidized bed granulating coated machine
Method: 40wt%～60wt% round granular material is dropped in the drying tower, starting outfit, adjusting inlet temperature is 70～90 ℃, behind the oven dry 60min, stops oven dry.Drop into leftover materials again in drying tower, starting outfit keeps 70～90 ℃ of inlet temperature once more, until (water content is not higher than 6%, needs 70～90min) approximately with drying materials.
In step 2 dressing process, specifically comprise:
(1) dressing
Equipment: fluidized bed granulation dressing machine
Method: Vltra tears, hydroxy propyl cellulose, polyacrylic resin and polyvinylpyrrolidone are made into 2wt%～5wt% aqueous solution according to the ratio of 10wt%～30wt%: 10wt%～30wt%: 30wt%～50wt%: 10wt%～30wt%, are pressed in the machine spray gun.The round granular micro-pill phytase that step 1 is obtained drops in the drying tower, starting outfit, and adjusting inlet temperature is 70～90 ℃, opens spray gun simultaneously and wraps quilt, until with drying materials (water content is not higher than 6%, needs 2～3 hours approximately).
(2) screening
Equipment: vibrating screen classifier
Method: starting outfit, in the material input charging opening with drying, the particle of different-grain diameter is divided into Three Estate, collects the particle of 30～60 order sizes.
Beneficial effect
The moulding pill and the coating material of the selected uniqueness of the present invention can make the phytase product use, keep when storing enzyme alive stable, and the ability of poor environments such as opposing external high temperature, high humidity strengthens, and advantage of the present invention is as follows:
1, coating material used in the present invention is the gastric solubility material, can dissolve at once under one's belt to discharge phytase and play a role.The pH value that phytase used in the present invention plays a role is between 2.0～6.0, and the animal stomach is the environment of slant acidity, therefore can well play a role.
2, the used coating material of the present invention is a water-soluble material, with water dissolution, not with an organic solvent, not polluted product and environment, and cost is lower.
3, micro-pill phytase of the present invention and coating micro-pill phytase, dissolution time are 10 minutes, can dissolve rapidly in the animal stomach, have guaranteed the performance of its hydrolytic action.
4, micropill of the present invention and micropill dressing phytase granularity be at 30～60 orders, unit weight 0.6g/L, therefore, micropill and coating micro-pill phytase feed use or transport process in not classification, the diffusion good stability.
5, the coating material resistance to elevated temperatures is good, when pelleting temperature reaches 85 ℃, still can reach the rate that retains more than 90%.
6, the coating micro-pill phytase of the present invention's preparation is a microspheroidal, rounding, regular shape, epigranular.Reduce to greatest extent and extraneous bonded area, reduce the influence of unfavorable factor phytase activity.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
With the corn cob meal of 130kg W-Gum, 60kg, the marble dust of 40kg, the lactose of 70kg, amount to the 300kg material and in mixing machine, mix 5min, add 240kg phytase fermented liquid then, (this fermented liquid is phytase generating bacterial strain process deep fermentation, the liquid fermentation production that utilizes cultures such as glucose, sulfate of ammoniac to produce, principal constituent is moisture and phytase albumen, and enzyme is lived and is 10000U/g), continue to mix 10min.
The material that mixes added wave in the nodulizer hopper, starting outfit is made material and is about 3～5mm, the cylindrical particle of the about 1～3mm of diameter.The cylindrical particle material input of making is thrown the sphere of circular knitting machine and throw in the circular knitting machine inner chamber, starting outfit, the adjustment rotating speed is 400～600rpm, discharging after cylindrical particle becomes circular granular.
300kg round granular material is dropped in the drying tower, starting outfit, adjusting inlet temperature is 70 ℃, behind the oven dry 60min, stops oven dry.Drop into the 240kg material again in drying tower again, starting outfit keeps 90 ℃ of inlet temperature once more, and drying materials behind the 90min is made micro-pill phytase.
1kg Vltra tears, 1kg hydroxy propyl cellulose, 2kg polyacrylic resin and 1kg polyvinylpyrrolidone are made into 5% aqueous solution 100kg, are pressed in the machine spray gun.The round granular micro-pill phytase 200kg that step 1 is obtained drops in the drying tower, starting outfit, and adjusting inlet temperature is 90 ℃, opens spray gun simultaneously and wraps quilt, until with drying materials, dries in 2 hours.
Embodiment 2:
With the corn cob meal of 100kg W-Gum, 40kg, the marble dust of 20kg, the lactose of 40kg, amount to 200kg and in mixing machine, mix 5min, (this fermented liquid is phytase generating bacterial strain process liquid submerged fermentation to add the 300kg fermented liquid then, utilize cultures such as glucose, sulfate of ammoniac, the liquid fermentation production of producing, principal constituent is moisture and phytase albumen, and enzyme is lived and is 8000U/g), continue to mix 10min.
The material that mixes added wave in the nodulizer hopper, starting outfit is made material and is about 3～5mm, the cylindrical particle of the about 1～3mm of diameter.The cylindrical particle material input of making is thrown the sphere of circular knitting machine and throw in the circular knitting machine inner chamber, starting outfit, the adjustment rotating speed is 400～600rpm, discharging after cylindrical particle becomes circular granular.
300kg round granular material is dropped in the drying tower, starting outfit, adjusting inlet temperature is 70 ℃, behind the oven dry 60min, stops oven dry.Drop into the 200kg material again in drying tower, starting outfit keeps 90 ℃ of inlet temperature once more, and drying materials behind the 90min is made micro-pill phytase.
0.4kg Vltra tears, 0.4kg hydroxy propyl cellulose, 0.8kg polyacrylic resin and 0.4kg polyvinylpyrrolidone are made into 2% aqueous solution, are pressed in the machine spray gun.The round granular micro-pill phytase 200kg that step 1 is obtained drops in the drying tower, starting outfit, and adjusting inlet temperature is 90 ℃, opens spray gun simultaneously and wraps quilt, until with drying materials, dries in 2 hours.
Embodiment 3
Performance test
1, outward appearance: the sensory measurement, use magnifying glass microscopy particle roundness, uniformity coefficient.The coating micro-pill phytase of the present invention's preparation is a microspheroidal, rounding, regular shape, epigranular.
2, compactness: the sensory measurement, hand is twisted with the fingers does not have fragmentation.
3, enzyme uniformity coefficient alive: after a collection of products production comes out, get 10 samples in different sites, according to the mensuration-spectrophotometry of the feeding phytase activity of GB/T18634,, measure the phytase activity of each sample and measure the variation coefficient then in conjunction with the relevant instruction of national feeler mechanism.The coating micro-pill phytase enzyme of the present invention's preparation uniformity of dosage units height alive, the variation coefficient is less than 5%.
4, granularity: use the standard model sieve, take a sample test in the 1kg sample 30～60 purpose particle weight at random.Coating micro-pill phytase grain diameter of the present invention is suitable, and 30～60 orders account for more than 90%.
5, unit weight: get the 1L measuring tank, pour micro-pill phytase or coating micro-pill phytase into to 1L scale marks place in measuring tank, gravimetry, decrement tube heavily are the phytase weight of 1L, i.e. unit weight.Micro-pill phytase or coating micro-pill phytase unit weight are suitable, about 0.60kg/L, with feed avidity are preferably arranged, and not classification, do not play static.
6, dissolution rate: product is put into the aqueous solution with 1: 100 ratio, measure dissolution time.The coating material solvability is good, and dissolution time is 10 minutes fully in water.
7, stability: respectively product deposited, put into Preblend separately, put into concentrate feed, put into mixed feed and deposit certain hour, mensuration is deposited preceding and is deposited the back enzyme and live, measure the retention rate that enzyme is lived, enzyme activity determination is according to the mensuration-spectrophotometry of the feeding phytase activity of GB/T18634, carries out in conjunction with the relevant instruction of national feeler mechanism.6 months testing data of 25 ℃ of normal temperature preservations shows: the rate that retains of micro-pill phytase improves 9.2% than common phytase on the market when depositing separately, and the rate that retains of coating micro-pill phytase improves 11.1%; The rate that retains of micro-pill phytase improves 12.8% than common phytase when depositing in concentrate feed, and the rate that retains of coating micro-pill phytase improves 15.7%; The rate that retains of micro-pill phytase improves 23.5% than common phytase in Preblend, and the rate that retains of coating micro-pill phytase improves 26.9%.
8, temperature tolerance test:
Simulation test: phytase is mixed with Semen Maydis powder by a certain percentage, add moisture, make sample reach the simulation moisture condition of 18wt%～20wt%, make test sample, measure enzyme content alive, sample is put into baking oven, by the analog temperature of setting, simulated time heating, after the heating, after treating the sample cooling, test sample product enzyme is lived, and measures the rate that retains, the mensuration that enzyme is lived is according to the mensuration-spectrophotometry of the feeding phytase activity of GB/T18634, carries out in conjunction with the relevant instruction of national feeler mechanism.
Production test: phytase is added mixed feed by a certain percentage, at the pelleting temperature of setting with granulate under the time, getting particulate material mensuration enzyme after the granulation lives, mensuration retains rate, enzyme activity determination is according to the mensuration-spectrophotometry of the feeding phytase activity of GB/T18634, carries out in conjunction with the relevant instruction of national feeler mechanism.
Compare with common phytase, under 85 ℃ of conditions, the Retention of micro-pill phytase improves 24%; The coating micro-pill phytase Retention improves 35%.
Claims (4)
1. coating micro-pill phytase, it is made up of micro-pill phytase and coatings, it is characterized in that, this coating micro-pill phytase granular size is 30～60 orders, wherein, described micro-pill phytase is made of carrier and significant quantity phytase, and carrier is made up of the W-Gum of the 30wt%～50wt% that accounts for the carrier total amount, the corn cob meal of 10wt%～30wt%, the marble dust of 5wt%～15wt% and the lactose of 10wt%～25wt%; Described coatings is formed in 10wt%～30wt%: 10wt%～30wt%: 30wt%～50wt%: 10wt%～30wt% ratio by Vltra tears, hydroxy propyl cellulose, polyacrylic resin and polyvinylpyrrolidone; Weight ratio between micro-pill phytase and the coatings is 40～100: 1.
2. coating micro-pill phytase according to claim 1 is characterized in that, described Vltra tears, methoxy content wherein are 19wt%～24wt%, and hydroxypropyl content is 4wt%～12wt%, and viscosity is 20～30mPa.s; Described hydroxy propyl cellulose, propoxyl content 60wt%～66wt% wherein, viscosity is 1500～2500mPa.s; Described polyacrylic resin, its relative density are 0.810～0.820, and base number is 162～198, and viscosity is 5～200mPa.s; Described polyvinylpyrrolidone, its nitrogen content are 11.5wt%～12.8wt%, and the K value is 27～32.
3. method for preparing coating micro-pill phytase, the method comprising the steps of:
1) preparation of micro-pill phytase
Mix as phytase carrier and phytase fermented liquid accounting for the W-Gum of the 30wt%～50wt% of phytase carrier total amount, the corn cob meal of 10wt%～30wt%, the marble dust of 5wt%～15wt% and the lactose of 10wt%～25wt%, phytase carrier and phytase fermented liquid account for this total mixture ratio and are respectively 40wt%～60wt% and 40wt%～60wt%, wherein the phytase fermented liquid is the tunning of phytase generating bacterial strain through liquid submerged fermentation production, and principal constituent is moisture and phytase albumen;
The phytase carrier and the phytase fermented liquid mixture input that mix are waved nodulizer, and by the physics extruding, material is made and is about 3～5mm, the cylindrical particle of the about 1～3mm of diameter;
Throw circle then, and, form micro-pill phytase in 70～90 ℃ of oven dry down of inlet temperature;
2) dressing
Vltra tears, hydroxy propyl cellulose, polyacrylic resin and polyvinylpyrrolidone are mixed with the aqueous solution of 2wt%～5wt% in 10wt%～30wt%: 10wt%～30wt%: 30wt%～50wt%: 10wt%～30wt% ratio, the micro-pill phytase that adopts gunite that step 1 is obtained then wraps by film forming, oven dry then, the coating micro-pill phytase of 30～60 order sizes is collected in screening.
4. the method for preparing coating micro-pill phytase according to claim 3 is characterized in that, described Vltra tears, methoxy content wherein are 19wt%～24wt%, and hydroxypropyl content is 4wt%～12wt%, and viscosity is 20～30mPa.s; Described hydroxy propyl cellulose, propoxyl content 60wt%～66wt% wherein, viscosity is 1500～2500mPa.s; Described polyacrylic resin, its relative density are 0.810～0.820, and base number is 162～198, and viscosity is 5～200mPa.s; Described polyvinylpyrrolidone, its nitrogen content 11.5wt%～12.8wt%, the K value is 27～32.
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| CN101810253A (en) * | 2010-03-30 | 2010-08-25 | 浙江大学 | High temperature resistance diaphragm-controlled phytase pellets and preparation method thereof |
| CN102854158B (en) * | 2011-07-01 | 2016-01-20 | 北京昕大洋科技发展有限公司 | A kind of method of Fast Measurement phytase heat resistance |
| CN102362696B (en) * | 2011-08-23 | 2013-10-16 | 上海欧耐施生物技术有限公司 | Envelope production process for granzyme for temperature-resistant feed |
| CN102511665B (en) * | 2011-12-29 | 2013-06-05 | 青岛玛斯特生物技术有限公司 | Phytase-coated pellets and preparation method thereof |
| CN104152293A (en) * | 2014-07-28 | 2014-11-19 | 张洪山 | Whole set of production line for basic protein color particles for washing |
| CN107410710A (en) * | 2017-09-12 | 2017-12-01 | 昆明佰佳益康生物科技有限公司 | A kind of preparation method of phytase preparation |
| CN117535267A (en) | 2020-04-29 | 2024-02-09 | 南京百斯杰生物工程有限公司 | Parent phytase variant |
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