CN102106480A - B-complex crystal vitamin microcapsule and method for preparing microcapsules by utilizing spray drying method - Google Patents

B-complex crystal vitamin microcapsule and method for preparing microcapsules by utilizing spray drying method Download PDF

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CN102106480A
CN102106480A CN2011100286429A CN201110028642A CN102106480A CN 102106480 A CN102106480 A CN 102106480A CN 2011100286429 A CN2011100286429 A CN 2011100286429A CN 201110028642 A CN201110028642 A CN 201110028642A CN 102106480 A CN102106480 A CN 102106480A
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vitamin
wall material
crystal vitamin
group crystal
microcapsule
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CN102106480B (en
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曹俊明
黄燕华
蒋卫亮
王国霞
陈冰
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Guangzhou flying jubilt Biological Technology Co., Ltd.
Institute of Animal Husbandry, Guangdong Academy of Agricultural Sciences
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Guangdong Fishtech Fisheries Science & Technology Co ltd
Institute of Animal Science of Guangdong Academy of Agricultural Sciences
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Abstract

The invention discloses a B-complex crystal vitamin microcapsule and a method for preparing the microcapsule by utilizing a spray drying method. The method comprises the following steps: adding a wall material into water, controlling the water temperature to be between 60 and 70 DEG C, stirring to ensure the wall material is dissolved in the water; adding B-complex crystal vitamin, homogenizing to ensure the wall material and the B-complex crystal vitamin are uniformly dispersed in a solution; and carrying out spray drying on the solution, and controlling the temperature of intake air to be between 160 and 200 DEG C, the flow rate of compressed air to be between 560 and 800L/h and the feeding speed to be between 3.34 and 6.68ml/min to obtain the B-complex crystal vitamin microcapsule. In the method, the wall material comprises the following components in parts by weight: 30 to 50 parts of Arabic gum, 30 to 50 parts of malto dextrin, 3 to 7 parts of gelatin, and 10 to 13 parts of sucrose; in the solution, the mass ratio of the B-complex crystal vitamin to the wall material is (20-40):100; and in the solution, the total concentration of the B-complex crystal vitamin and wall material is 200 to 400g/L. The B-complex crystal vitamin microcapsule has the advantages of good sustained release effect and good stability.

Description

B group crystal vitamin microcapsule and utilize the method for these microcapsules of spray drying method for preparation
Technical field:
The invention belongs to field of animal feed, be specifically related to a kind of B group crystal vitamin microcapsule and utilize the method for these microcapsules of spray drying method for preparation.
Background technology:
In the raising fish and shrimp process, the main cause that fishes and shrimps can not make full use of B group crystal vitamin is at present: 1. fishes and shrimps are adopted and are raised food slowly, and B group crystal vitamin soluble in water in, be easy to from feed granules, ooze out, influence the additive effect of B group crystal vitamin.2. character and structure thereof were destroyed easily (as VB after some B group crystal vitamin contacted with external environment 1, VB 2, VB 6, folic acid).B group crystal vitamin and aquatic feeds are in storage process, and B group crystal vitamin contacts back character and destructurized with external environment, have influenced the additive effect of B group crystal vitamin.3. some B group crystal vitamin, non-refractory is (as VB 3, VB 7, folic acid).In preparation aquatic feeds process, temperature can reach 130 ℃, and crystal vitamin is destroyed easily under this temperature, has influenced the additive effect of B group crystal vitamin.
Summary of the invention:
The purpose of this invention is to provide a kind of method that has the B group crystal vitamin microcapsule of slow release effect, good stability and utilize these microcapsules of spray drying method for preparation.B group crystal vitamin microcapsule of the present invention has slow release effect, can slow down B group crystal vitamin in the fishes and shrimps body rate of release and in particulate material the dialysis amount in water, can also completely cut off contacting of B group crystal vitamin and external environment, avoid B group crystal vitamin to contact with external environment, and the character and the structure of destruction B group crystal vitamin, and further can also reduce the destruction of high temperature to crystal B family vitamin, thereby improve the additive effect of B group crystal vitamin greatly, and utilize the method for spray drying method for preparation B group crystal vitamin microcapsule to have simply, the advantage that cost is low can be produced on a large scale.
The method of utilizing spray drying method for preparation B group crystal vitamin microcapsule of the present invention is characterized in that, may further comprise the steps:
The wall material is added to the water, the control water temperature is 60～70 ℃, stirring is dissolved in the water wall material, add B group crystal vitamin again, homogeneous evenly spreads in the solution wall material and B group crystal vitamin, again this solution is carried out spray-drying, 160～200 ℃ of control EATs, compressed air require 560～800L/h, charging rate 3.34～6.68ml/min obtains B group crystal vitamin microcapsule;
Described wall material is pressed mass fraction, is made up of following component: Arabic gum 30～50, maltodextrin 30～50, gelatin 3～7, sucrose 10～13;
In the described solution, the mass ratio of B group crystal vitamin and wall material is 20～40: 100;
In the described solution, the total concentration of B group crystal vitamin and wall material is 200～400g/L.
Preferably, described homogeneous, its rotating speed are 200r/min～500r/min, and homogenizing time is 10min～30min.
Described B family vitamin is preferably Cobastab 1And Cobastab 6
The B group crystal vitamin microcapsule that utilizes the method for spray drying method for preparation B group crystal vitamin microcapsule of the present invention to prepare, its particle is little, crosses 80 mesh sieves.This B group crystal vitamin microcapsule has the good slow release effect, can slow down B group crystal vitamin in the fishes and shrimps body rate of release and in particulate material the dialysis amount in water; Can also completely cut off contacting of B group crystal vitamin and external environment, avoid B group crystal vitamin to contact, and destroy the character and the structure of B group crystal vitamin with external environment, good stability, under illumination condition, its photostability might as well; And further can also reduce the destruction of high temperature to B group crystal vitamin, high temperature is to the destruction of B group crystal vitamin, Heat stability is good in the process of reduction preparation aquatic feeds; Thereby improve the additive effect of B group crystal vitamin greatly, reduced the cost of feed, and simple, the suitable large-scale production of this preparation method, product is used for the fishes and shrimps feed, improves the culture benefit of fishes and shrimps greatly.
The specific embodiment:
Below be to further specify to of the present invention, rather than limitation of the present invention.
Embodiment 1:
Measure 100ml distilled water with beaker, in water-bath, be heated to 70 ℃ then, take by weighing wall material 25g, under the condition of stirring of limit, load weighted wall material is dissolved in the distilled water, wait wall material dissolving fully after, add the crystal Cobastab again 15g, homogeneous under the rotating speed of 400r/min then, homogeneous 15min.After homogeneous is intact, carry out spray-drying.160～200 ℃ of EATs, compressed air require 560～800L/h, charging rate 4.18ml/min makes B group crystal vitamin microcapsule, Cobastab in this B group crystal vitamin microcapsule 1Content can reach 18.07%, embedding rate can reach 86.26%, particle is little, crosses 80 sieves.
Described wall material is to be 30: 50: 3 by Arabic gum, maltodextrin, gelatin and sucrose according to mass ratio: what 13 ratio mixed forms.
Embodiment 2:
Measure 100ml distilled water with beaker, in water-bath, be heated to 70 ℃ then, take by weighing wall material 23.1g, under the condition of stirring of limit, load weighted wall material is dissolved in the distilled water, wait wall material dissolving fully after, add the crystal Cobastab again 66.9g, homogeneous under the rotating speed of 400r/min then, homogeneous 10min.After homogeneous is intact, carry out spray-drying.160～200 ℃ of EATs, compressed air require 560～800L/h, charging rate 5.85ml/min.Make B group crystal vitamin microcapsule, Cobastab in this B group crystal vitamine capsule 6Content can reach 27.65%, and embedding rate can reach 88.28%, and particle is little, crosses 80 sieves.
Described wall material is to be 50: 30: 7 by Arabic gum, maltodextrin, gelatin and sucrose according to mass ratio: what 10 ratio mixed forms.
Embodiment 3:
Measure 100ml distilled water with beaker, in water-bath, be heated to 70 ℃ then, take by weighing wall material 14.29g, under the condition of stirring of limit, load weighted wall material is dissolved in the distilled water, wait wall material dissolving fully after, add the crystal Cobastab again 15.71g, homogeneous under the rotating speed of 500r/min then, homogeneous 10min.After homogeneous is intact, carry out spray-drying.160～200 ℃ of EATs, compressed air require 560～800L/h, charging rate 3.34ml/min makes B group crystal vitamin microcapsule, Cobastab in this B group crystal vitamin microcapsule 1Content can reach 21.23%, embedding rate can reach 74.43%, particle is little, crosses 80 sieves.
Described wall material is to be 30: 30: 7 by Arabic gum, maltodextrin, gelatin and sucrose according to mass ratio: what 13 ratio mixed forms.
Embodiment 4:
Measure 100ml distilled water with beaker, in water-bath, be heated to 60 ℃ then, take by weighing wall material 33.33g, under the condition of stirring of limit, load weighted wall material is dissolved in the distilled water, wait wall material dissolving fully after, add crystal vitamin B1 6.67g again, homogeneous under the rotating speed of 200r/min then, homogeneous 30min.After homogeneous is intact, carry out spray-drying.160～200 ℃ of EATs, compressed air require 560～800L/h, charging rate 6.68ml/min, the B group crystal vitamin microcapsule that makes, Cobastab in this B group crystal vitamin microcapsule 1Content can reach 15.68%, embedding rate can reach 87.33%, particle is little, crosses 80 sieves.
Described wall material is to be 35: 35: 5 by Arabic gum, maltodextrin, gelatin and sucrose according to mass ratio: what 12 ratio mixed forms.
The performance measurement of B group crystal vitamin microcapsule:
B group crystal vitamin microcapsule for preparing with embodiment 1,2,3,4 and crystal vitamin B1, crystal vitamin B6 according to following method, are measured its character as sample.
(1) Study on Stability under the normal temperature laboratory condition of normal pressure
Sample thief 1.0g (every group get two parallel) is placed on indoorly, promptly is under the normal temperature and pressure conditions, gets sample weekly one time, the content of corresponding B family vitamin in the working sample, METHOD FOR CONTINUOUS DETERMINATION one month.
(2) Study on Stability under 130 ℃ of conditions
Sample thief 1.0g (every group get two parallel) is placed in 130 ℃ of baking ovens, respectively at 10min, and 20min, 30min, four time periods samplings of 60min, the content of corresponding B family vitamin in the working sample.
(3) Study on Stability under the solar radiation
Sample thief 1.0g (every group get two parallel) places irradiation in the sun, respectively at 1d, 3d, 7d and four time periods samplings of 14d, the content of corresponding B family vitamin in the working sample.
(4) rate of release in SGF
Sample thief 0.1g (every group get two parallel) puts into SGF, gets 5ml solution in 0min, 5min, 10min, 30min, five time periods of 60min respectively, measures the content of the corresponding B family vitamin in the solution.
(5) rate of release in fresh water
Sample thief 0.1g (every group get two parallel) puts into fresh water, gets 5ml solution in 0min, 5min, 10min, 30min, five time periods of 60min respectively, measures the content of the corresponding B family vitamin in the solution.
(6) rate of release in seawater
Sample thief 0.1g (every group get two parallel) puts into seawater, gets 5ml solution in 0min, 5min, 10min, 30min, five time periods of 60min respectively, measures the content of the corresponding B family vitamin in the solution.
B group crystal vitamin microcapsule that embodiment 1,2,3,4 prepares and crystal Cobastab 1, the crystal Cobastab 6Shown in the following tabulation of test result of sample:
Table 1: illumination is to the VB of sample 1Or VB 6Content influence (%)
Figure BDA0000045481960000061
Show under the 2:130 ℃ of temperature the VB in the sample 1Or VB 6Content influence (%)
Figure BDA0000045481960000062
Table 3: normal temperature and pressure is to the VB in the sample 1Or VB 6Content influence (%)
Figure BDA0000045481960000071
Table 4: the VB in the sample 1Or VB 6Rate of release in SGF (mg/L)
Figure BDA0000045481960000072
Table 5: the VB in the sample 1Or VB 6Rate of release in fresh water (mg/L)
Table 6: the VB in the sample 1Or VB 6Rate of release in seawater (mg/L)
Figure BDA0000045481960000082
The crystal Cobastab can be described by table 1 1And B 6After solar radiation, change of properties is very big, descended 16.11% and 23.44% after 14 days respectively, and the microcapsules that embodiment 1,2,3 and 4 makes has descended 2.49%, 2.51%, 11% and 0.87% respectively.Therefore can prove, crystal vitamin by embedding after, reduced the influence of illumination to its character, kept the original character of crystal vitamin, for crystal vitamin, stability is improved.
The crystal Cobastab can be described by table 2 1And B 6After 130 ℃ of high-temperature process, change of properties is very big, descended 29.36% and 36.59% respectively, and the microcapsules that embodiment 1,2,3 and 4 makes has descended 3.05%, 4.92%, 2.12% and 1.42% respectively.Therefore can prove, crystal vitamin by embedding after, reduced of the influence of 130 ℃ of high temperature to its character, kept the original character of crystal vitamin, help in the Aquatic Feed Processing process, keeping the character of crystal vitamin.For crystal vitamin, VB 1And VB 6Stability be improved.
The crystal Cobastab can be described by table 3 1And B 6Be placed in the normal temperature and pressure environment after one month, character has bigger variation, descended 8.87% and 10.27% respectively, and the microcapsules that embodiment 1,2,3 and 4 makes has descended about 0.89%, 1.47%, 0.72% and 0.41% respectively.Therefore can prove, crystal vitamin by embedding after, reduced the influence of external environment to its character, kept the original character of crystal vitamin.For crystal vitamin, VB 1And VB 6Stability be improved.
Can illustrate by table 4, crystal vitamin by embedding after, in SGF, still can discharge smoothly, therefore can prove that B group crystal vitamin microcapsule can discharge smoothly and in the fish body by the fish bulk absorption.
Can illustrate by table 5 and table 6, crystal vitamin by embedding after, for the rate of release of crystal vitamin, rate of release slows down at the rate of release in fresh water and the seawater, helps fish bulk absorption B family vitamin.
The assay method that the present invention is all:
(1) Cobastab 1The Determination on content method:
Cobastab 1The Determination on content method is according to GB GB/T 7295-2008.Take by weighing sample 0.05g (being accurate to 0.0002g), after adding water 50ml dissolving, add the 2ml concentrated hydrochloric acid, heating, add 4ml silico-tungstic acid (10g/100ml) after boiling, continue to boil 2min, be used in the core crucible suction filtration of 80 ℃ of dry constant weights, precipitation is earlier with the hydrochloric acid solution 20ml gradation washing of boiling, and then once with the washing of 10ml distilled water, use the acetone washed twice at last, each 5ml, sediment is dried to constant weight under 80 ℃.
W 1 = m 1 * 0.1939 * 100 M 2 * ( 1 - W 2 )
M 1=dry constant weight postprecipitation heavy (g)
0.1939-the thiamine hydrochloride tungstates is converted into the thiamine hydrochloride coefficient
M 2=sample quality (g)
W 2=sample drying weightlessness
(2) Cobastab 6The Determination on content method:
Method one: measure VB according to GB GB/T 7295-2006 6Content
VB 6Assay method according to GB GB/T 7295-2006.Take by weighing sample 0.15g (being accurate to 0.0002g), ice acetic acid 20ml and mass concentration are 5% mercuric acetate solution 5ml, after the damp and hot dissolving, put cold, add 1 of crystal violet indicator, with the perchloric acid standard titration solution titration of 0.1mol/l, result of the test is proofreaied and correct with blank test.
X = ( V 1 - V 2 ) * C * 205.6 * 100 M * 1000
V 1=perchloric acid consumption (ml)
V 2=blank group perchloric acid consumption (ml)
C=perchloric acid molar concentration (mol/l)
The quality of M=sample (g)
Method two: determined by ultraviolet spectrophotometry VB 6Content
VB 6Assay method with reference to the assay method of Chen Shuhua, in the 25ml volumetric flask, add a certain amount of VB successively 6Standard liquid, 10g/l sodium carbonate liquor 2.0ml, the amino peace of 4g/l 4-is replaced than quinoline solution 2.0ml and 10g/l peroxy-disulfuric acid ammonium salt solution 2.0ml, with distilled water be diluted to scale, shake up, static 20min, on 721 type spectrophotometers, in wavelength 394nm place, with the cuvette of 1cm, make reference with reagent blank, measure absorbance.
A＝0.01253C+0.005r＝0.999
C=VB 6Concentration
Annotate: the concentration of VB6 is: 2～40mg/l
(3) assay method of embedding rate:
Get the 1.0g sample and insert in the 200 purpose mesh bags, measure 30ml distilled water with graduated cylinder then, wash, wash three times, each 10ml wants slowly during flushing.After having washed, divide sucking-off water-in-bag with paper handkerchief at once, then low temperature drying.Behind dry the finishing, measure VB in the microcapsules 1Or VB 6Content.
The calculating of microcapsule embedded rate is formula as follows:
Figure BDA0000045481960000111
(4) computational methods of microcapsules retention rate:
Microcapsules owing to be subjected to Effect of Environmental, can cause degraded, the destruction of core in storage, the heaviest index of this change of stability situation is exactly the retention rate of core.
Cobastab 1Or B 6The computing formula of retention rate is:
Figure BDA0000045481960000112

Claims (4)

1. a method of utilizing spray drying method for preparation B group crystal vitamin microcapsule is characterized in that, may further comprise the steps:
The wall material is added to the water, the control water temperature is 60～70 ℃, stirring is dissolved in the water wall material, add B group crystal vitamin again, homogeneous evenly spreads in the solution wall material and B group crystal vitamin, again this solution is carried out spray-drying, 160～200 ℃ of control EATs, compressed air require 560～800L/h, charging rate 3.34～6.68ml/min obtains B group crystal vitamin microcapsule;
Described wall material is pressed mass fraction, is made up of following component: Arabic gum 30～50, maltodextrin 30～50, gelatin 3～7, sucrose 10～13;
In the described solution, the mass ratio of B group crystal vitamin and wall material is 20～40: 100;
In the described solution, the total concentration of B group crystal vitamin and wall material is 200～400g/L.
2. the method for utilizing spray drying method for preparation B group crystal vitamin microcapsule according to claim 1 is characterized in that described homogeneous, its rotating speed are 200r/min～500r/min, and homogenizing time is 10min～30min.
3. the method for utilizing spray drying method for preparation B group crystal vitamin microcapsule according to claim 1 is characterized in that described B family vitamin is a Cobastab 1And Cobastab 6
4. B group crystal vitamin microcapsule that the method for utilizing spray drying method for preparation B group crystal vitamin microcapsule according to claim 1 prepares.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103478710A (en) * 2013-08-30 2014-01-01 南京泛成生物化工有限公司 L-carnitine micro-capsule powder and preparation method thereof
CN105852133A (en) * 2016-06-25 2016-08-17 河北农业大学 Vitamin B microcapsule and preparation method thereof
CN106942498A (en) * 2017-04-28 2017-07-14 巴马原种香猪农牧实业有限公司 A kind of efficient BaMa miniature pig feed for pregnant sows
CN113730376A (en) * 2021-09-17 2021-12-03 华中药业股份有限公司 Thiamine nitrate sustained-release microcapsule and preparation method thereof

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CN101112400A (en) * 2007-07-25 2008-01-30 刘士峰 oral liquid and capsule for preventing and curing various diseases
CN101444495A (en) * 2008-12-31 2009-06-03 江南大学 Vitamin E microcapsule preparation method
CN101536993A (en) * 2009-04-21 2009-09-23 浙江花园生物高科股份有限公司 Vitamin D3 microcapsule and preparation method thereof
CN101703491A (en) * 2009-08-10 2010-05-12 北京市金康普食品添加剂科技有限公司 Vitamin a powder and preparation method thereof

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Publication number Priority date Publication date Assignee Title
CN101112400A (en) * 2007-07-25 2008-01-30 刘士峰 oral liquid and capsule for preventing and curing various diseases
CN101444495A (en) * 2008-12-31 2009-06-03 江南大学 Vitamin E microcapsule preparation method
CN101536993A (en) * 2009-04-21 2009-09-23 浙江花园生物高科股份有限公司 Vitamin D3 microcapsule and preparation method thereof
CN101703491A (en) * 2009-08-10 2010-05-12 北京市金康普食品添加剂科技有限公司 Vitamin a powder and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103478710A (en) * 2013-08-30 2014-01-01 南京泛成生物化工有限公司 L-carnitine micro-capsule powder and preparation method thereof
WO2015027565A1 (en) * 2013-08-30 2015-03-05 南京泛成生物化工有限公司 L-carnitine micro-capsule powder and preparation method thereof
CN103478710B (en) * 2013-08-30 2015-08-19 南京泛成生物化工有限公司 L-carnitine micro-capsule powder and preparation method thereof
CN105852133A (en) * 2016-06-25 2016-08-17 河北农业大学 Vitamin B microcapsule and preparation method thereof
CN106942498A (en) * 2017-04-28 2017-07-14 巴马原种香猪农牧实业有限公司 A kind of efficient BaMa miniature pig feed for pregnant sows
CN113730376A (en) * 2021-09-17 2021-12-03 华中药业股份有限公司 Thiamine nitrate sustained-release microcapsule and preparation method thereof
CN113730376B (en) * 2021-09-17 2023-10-10 华中药业股份有限公司 Thiamine nitrate slow-release microcapsule and preparation method thereof

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Address after: 510000 Dafeng street, No. 1, five mountain town, Tianhe District, Guangzhou, Guangdong

Co-patentee after: Guangzhou flying jubilt Biological Technology Co., Ltd.

Patentee after: Institute of Animal Husbandry, Guangdong Academy of Agricultural Sciences

Address before: 510000 Dafeng street, No. 1, five mountain town, Tianhe District, Guangzhou, Guangdong

Co-patentee before: Guangzhou Feixite Aquatic Technology Co., Ltd.

Patentee before: Institute of Animal Husbandry, Guangdong Academy of Agricultural Sciences