CN105031655A - Stable vitamin A preparation and preparation process thereof - Google Patents
Stable vitamin A preparation and preparation process thereof Download PDFInfo
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- CN105031655A CN105031655A CN201510249678.8A CN201510249678A CN105031655A CN 105031655 A CN105031655 A CN 105031655A CN 201510249678 A CN201510249678 A CN 201510249678A CN 105031655 A CN105031655 A CN 105031655A
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- attapulgite
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Abstract
The invention discloses a preparation method of a stable vitamin A preparation. The preparation method includes following steps: (1) activating attapulgite and performing high-temperature treatment to the attapulgite; and (2) adding the treated attapulgite in a vitamin A ethanol solution for adsorption. In the invention, the attapulgite is treated through acid and then treated at a high temperature to form activated attapulgite, and then the activated attapulgite is combined with vitamin A. The preparation is good in stability. The fat-soluble vitamin which is difficult to disperse is prepared into solid powder, so that the defect of vitamin A is overcome. The vitamin A preparation is convenient to use and is an excellent raw material for producing feeds without technical limit.
Description
Technical field
The invention belongs to veterinary drug and feed additive research field, be specifically related to the preparation method of a kind of attapulgite absorption vitamin A.
Background technology
Vitamin A keeps the sound and complete of epithelial tissue (skin and mucosa), promote growth and the regeneration of mucosa and skin, promote mucopolysaccharide synthesis in connective tissue, safeguard the complete of cell membrane and organelle membrane structure, surface of cell membrane albumen is mainly mucopolysaccharide albumen, research shows that vitamin A can by glycoprotein biosynthesis in the function influence epithelial cell of glycosyl transferase " during hypovitaminosis A; epithelial tissue squamous distortion keratinization, causes epithelial tissue drying and excessive keratinization.Vitamin A is also the necessary micronutrient element of animal body, due to the fat-soluble, oxidizable of vitamin A and the characteristic being vulnerable to ultraviolet impact, the feed formulation work of vitamin A is made to be difficult to carry out, feed formulation method was not at that time, not only can not reach the effect of nutritional intervention, harmful effect can be produced on the contrary, when adding vitamin A with stirring means in feedstuff, between each batch of feedstuff, content difference is very large, and vitamin A content in feedstuff is uneven, thus cause animal feed instability, be difficult to ensure quality of the fodder.
Attapulgite clay refers to attapulgite to be a kind of clay mineral of key component.Attapulgite crystal structure figure is see accompanying drawing 2.
Attapulgite is a kind of crystalloid hydrous magnesium aluminium silicate mineral, has unique layer chain structure feature, in its structure, there is crystal lattice, Na+, Ca2+, Fe3+, Al3+ containing non-quantitative in side crystal, and crystal is needle-like, threadiness or fiber collection shape.Attapulgite has unique dispersion, high temperature resistant, anti-good colloidal nature and the higher absorbability such as saline and alkaline.Due to the crystal structure of attapulgite uniqueness, make it that there is many special materializations and processing performance.Main physical and chemical performance and processing performance have: cation interchangeability, adsorptivity, adsorption bleaching, large specific surface area (9.6 ~ 36m2/g) and colloid index and expansion capacity.These character can make extend the time of contact of sterilization objects, and greatly decline to the corrosivity of metal etc., and its stability also strengthens greatly simultaneously.Therefore improve the effectiveness of its sterilization, along with the development of automatic cleaning system, corrosion-free, slow release, efficiently antibacterial have become desirable use object.
Summary of the invention
The technical problem to be solved in the present invention overcomes existing defect, provides the better vitamin A novel formulation of a kind of stability;
Another object of the present invention is to provide the preparation technology of said vitamin A novel formulation.
Object of the present invention carrys out specific implementation by the following technical programs:
A preparation for stabilizing vitamin A, described preparation is adsorb vitamin A by attapulgite to combine the powder formed.
Preferably, every 1000g attapulgite absorption 0.132g vitamin A.
The preparation method of the preparation of aforementioned stable vitamin A, first carries out activation processing to attapulgite, then carries out high-temperature process; Alcoholic solution attapulgite after process being placed in vitamin A again carries out adsorbing.
Concrete steps are as follows:
1) activation processing: by attapulgite supersound process 30min in sour water, then room temperature lower magnetic force stirs 4h;
2) high-temperature process: the attapulgite deionized water after activation processing is washed till without after chloride ion, calcines 5h at 200-600 DEG C, take out for subsequent use;
3) adsorb: to step 2) process after attapulgite mix with ethanol, vitamin A, vibrate under room temperature 12-24h, and sucking filtration solid, gets product.
Preferably, described sour water is the hydrochloric acid of 4-8M.The best is, described sour water is the hydrochloric acid of 8M
Preferably, described attapulgite: sour water: ethanol: vitamin A is 1000g:8000mL:100mL:0.135g.
Preferably, in described step 1), the revolution of magnetic agitation is 380r/min.
Preferably, described step 2) in, at 400 DEG C, calcine 5h.
The present invention is the preparation method that a kind of attapulgite and vitamin A combine, and it attapulgite is adsorbed vitamin A to combine formation powder, has the functions such as its stable in properties, slow release, persistent.The present invention adopts by acid and high-temperature process attapulgite, form active attapulgite stone, be combined with vitamin A again, its good stability, the fatsoluble vitamin of the liquid state of not easily disperseing is made pressed powder, overcome the shortcoming of vitamin A itself, take convenience, the unrestricted quality raw materials of feed processing technology.And can, according to different demands, can, by variable concentrations formula feed, adopt commercialization attapulgite and vitamin A to combine, prepare the preparation method of a kind of attapulgite absorption vitamin A, make its be more convenient for storage and application, facilitate the feed formulation in aquaculture, ensure the health of poultry.
Accompanying drawing explanation
Fig. 1 is the curve chart of vitamin A absorbing wavelength and absorbance in ethanol in the specific embodiment of the invention;
Fig. 2 is attapulgite crystal structure figure in background technology of the present invention.
Detailed description of the invention
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
Vitamin A adsorbs research on modified attapulgite
Vitamin A is all a kind of required nutrient substance to human body and animal, have and improve vision and promote the effect that normal growth is grown, but Excess free enthalpy can bring negative effect to health.Vitamin A is often added in animal feed to meet the nutritional need of animal.The present invention's static experiment method have studied the absorption property of vitamin A at modified attapulgite.
1, the adsorption experiment of vitamin A
1.1
retinol1:
The attapulgite taking 10g, in three-necked bottle, adds the hydrochloric acid of 100ml (8mol/L), ultrasonic 30min, and room temperature lower magnetic force stirs 4h(380r/min), then centrifugal, be washed till without chloride ion, after cold drying with deionized water.At 200 DEG C, calcine 5h, taking-up cooling is for subsequent use.Then add the vitamin A of 10ml ethanol and 0.0135g, at room temperature vibrate 12h, sucking filtration solid, measures the amount of the vitamin A in filtrate, then the amount that the amount of added vitamin A deducts in filtrate is the amount of absorption.
1.2
dehydroretinol:
The attapulgite taking 10g, in three-necked bottle, adds the hydrochloric acid of 100ml (8mol/L), ultrasonic 30min, and room temperature lower magnetic force stirs 4h(380r/min), then centrifugal, be washed till without chloride ion, after cold drying with deionized water.At 400 DEG C, calcine 5h, taking-up cooling is for subsequent use.Then add the vitamin A of 10ml ethanol and 0.0135g, at room temperature vibrate 18h, sucking filtration solid, measures the amount of the vitamin A in filtrate, then the amount that the amount of added vitamin A deducts in filtrate is the amount of absorption.
1.3
3-Hydroxyretinol:
The attapulgite taking 10g, in three-necked bottle, adds the hydrochloric acid of 100ml (8mol/L), ultrasonic 30min, and room temperature lower magnetic force stirs 4h(380r/min), then centrifugal, be washed till without chloride ion, after cold drying with deionized water.At 600 DEG C, calcine 5h, taking-up cooling is for subsequent use.Then add the vitamin A of 10ml ethanol and 0.0135g, at room temperature vibrate 24h, sucking filtration solid, measures the amount of the vitamin A in filtrate, then the amount that the amount of added vitamin A deducts in filtrate is the amount of absorption.
1.4 vitamin A contrasts
A certain amount of vitamin A is mixed with light flour, dosage with adsorb above modify after vitamin A consistent.
The selection of 1.5 maximum absorption wavelengths
Be that standard is blank with dehydrated alcohol, use 1cm quartz colorimetric utensil, with standard vitamin A ethyl ester solution, scan in 250 ~ 400nm wave-length coverage, as shown in Figure 1, vitamin A maximum absorption wavelength λ max is in ethanol 325nm (theoretical λ max=326nm), without other absworption peak in 250 ~ 400nm wave-length coverage.
The drafting of 1.6 standard working curves
1.6.1 recovery test
Get variable concentrations (1,2,3 μ gmL
-1) vitamin A standard solution carries out recovery test by method, acquired results is between 97.7% ~ 100.1%.
1.6.2 the drafting of standard curve
By test method, measure standard series, vitamin A concentration is at 0 ~ 12.0mgL
-1scope linear relationship is good, and regression equation C=16.899A+0.059, correlation coefficient is 0.9996.
1.6.3 the mensuration of vitamin A total amount
Sample thief appropriate (accurately to 0.0019) adds the petroleum ether of about 50ml in 65 in ground conical flask
0surname extraction 6h under C water bath condition, extracting solution cooling after by extracting solution standardize solution in the brown volumetric flask of 100ml, jolting mixes, lml solution standardize solution is pipetted again in the brown volumetric flask of 100ml from this volumetric flask, shake up mixing, from brown 100ml volumetric flask, pipette lml solution standardize solution in the brown volumetric flask of 100ml, shake up, finally measure absorbance with ultraviolet spectrophotometer at 325nm place.
2 results and discussion
2.1 stability test
According to the Ministry of Agriculture's " veterinary drug stability test technical specification (trying) " requirement, and affect this raw material stability factor, we select the condition such as different temperature, humidity, illumination to test, the projects such as appearance character, content, catabolite are examined or check, investigates the stability of this product.
This product three batches is placed in 40 DEG C, and relative humidity 75%(goes on the market packaging or simulation listing packaging) place six months under condition, monthly sample once, investigate related item, the results are shown in Table 1.
Adsorb vitamin A new product to modified attapulgite and contrast vitamin A (untreated), carry out the content detection of vitamin A ethyl ester at the product of 1,2,3,4,5,6 month, testing result is in table 1.Modified attapulgite absorption vitamin A(A1, A2, A3) content change very little in the storage process of six months, wherein A2 is the most stable, and contrasts poor stability.Therefore dehydroretinol can in feedstuff stable existence.Therefore, it is feasible for adsorbing the measure of vitamin A novel nourishing with modified attapulgite absorption vitamin A fortified feed exploitation modified attapulgite.
Table 1 accelerates test result experimental condition: temperature 40 DEG C of relative humiditys: 75%
。
2.2 pairs of light durability tests
Place ten days under this product three batch is placed in the condition of illumination 4500LX, timing sampling, investigates related item, the results are shown in Table 2.
Table 2 light durability test results test condition: illumination 4500LX
。
2.3 long term test
By this product three batch simulation listing packaging, temperature 25 DEG C, place 24 months under relative humidity 60% condition, regularly sample, investigate related item.
Result of the test is in table 3.
Table 3 long-term test results experimental condition: temperature 25 DEG C of relative humiditys: 60%
。
3 conclusions:
As can be seen from above stability test, the product stability prepared in the condition in dehydroretinol preparation method is best.
3.1 dehydroretinols are through 40 DEG C of relative humiditys 75%, and after being modified by absorption, its accelerated test six months, indices change is not obvious, shows that this product stablizes (table 1).And comparatively A1 and A3 is more stable.
3.2 this product were through sun exposure ten days, and appearance color is unchanged, after being modified by absorption, and its content and other index change not obvious (table 2).Show that this product stablizes (table 1).And comparatively A1 and A3 is more stable.
3.3 modified by absorption after, its this product long-term room-temperature keeps sample examination, has done 2 years at present, and indices, without significant change, shows that this product comparatively stablizes (table 3).Show that this product stablizes (table 1).And comparatively A1 and A3 is more stable.
3.4 contrast unstable chemcial properties, should not directly add in feedstuff.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (9)
1. a preparation for stabilizing vitamin A, is characterized in that: described preparation is adsorb vitamin A by attapulgite to combine the powder formed.
2. the preparation of stabilizing vitamin A according to claim 1, is characterized in that: every 1000g attapulgite absorption 0.132g vitamin A.
3. the preparation method of the preparation of stabilizing vitamin A according to claim 1 or 2, is characterized in that: first carry out activation processing to attapulgite, then carries out high-temperature process; Alcoholic solution attapulgite after process being placed in vitamin A again carries out adsorbing.
4. the preparation method of the preparation of stabilizing vitamin A according to claim 3, is characterized in that: concrete steps are as follows:
1) activation processing: by attapulgite supersound process 30min in sour water, then room temperature lower magnetic force stirs 4h;
2) high-temperature process: the attapulgite deionized water after activation processing is washed till without after chloride ion, calcines 5h at 200-600 DEG C, take out for subsequent use;
3) adsorb: to step 2) process after attapulgite mix with ethanol, vitamin A, vibrate under room temperature 12-24h, and sucking filtration solid, gets product.
5. the preparation method of the preparation of stabilizing vitamin A according to claim 4, is characterized in that: described sour water is the hydrochloric acid of 4-8M.
6. the preparation method of the preparation of stabilizing vitamin A according to claim 5, is characterized in that: described sour water is the hydrochloric acid of 8M.
7. the preparation method of the preparation of stabilizing vitamin A according to claim 4, is characterized in that: described attapulgite: sour water: ethanol: vitamin A is 1000g:8000mL:100mL:0.135g.
8. the preparation method of the preparation of stabilizing vitamin A according to claim 4, it is characterized in that: in described step 1), the revolution of magnetic agitation is 380r/min.
9. the preparation method of the preparation of stabilizing vitamin A according to claim 4, is characterized in that: described step 2) in, at 400 DEG C, calcine 5h.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5935623A (en) * | 1998-01-15 | 1999-08-10 | Milwhite, Inc. | Use of thermally treated clays in animal feeds |
| CN103416607A (en) * | 2012-05-24 | 2013-12-04 | 程会 | Chicken feed additive |
-
2015
- 2015-05-18 CN CN201510249678.8A patent/CN105031655A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5935623A (en) * | 1998-01-15 | 1999-08-10 | Milwhite, Inc. | Use of thermally treated clays in animal feeds |
| CN103416607A (en) * | 2012-05-24 | 2013-12-04 | 程会 | Chicken feed additive |
Non-Patent Citations (3)
| Title |
|---|
| C VISERAS,ET AL: "Current challenges in clay minerals for drug delivery", 《APPLIED CLAY SCIENCE》 * |
| 张乃峰等: "《猪饲料调制加工与配方集萃》", 31 January 2013, 中国农业科学技术出版社 * |
| 马冬梅等: "养鸡生产中维生素A缺乏症", 《畜牧与饲料科学》 * |
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