A 25-hydroxyvitamin d3 premix and its preparation method and application

Abstract

The application belongs to the technical field of feed additives, and particularly relates to a 25-hydroxyvitamin D3 premix, a preparation method and application thereof. The 25-hydroxyvitamin D3 premix comprises the following components by weight: 25-hydroxyvitamin D3 0.008%-0.08%, emulsifier 0.08%-0.7%, stabilizer 0.3%-1.2%, synergist 0.8%-1.7%, and diluent supplementing to 100%. The 25-hydroxyvitamin D3 premix coats non-water-soluble raw materials into water-soluble raw materials through emulsification, and has the advantages of simple process, uniform water dispersion, water solubility, better stability and the like. The additive has the effects of improving poultry bone density, reducing the incidence of abnormal eggs in the later stage of laying hens and the like.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of feed additives, and particularly relates to a 25-hydroxyvitamin D3 premix, a preparation method and application thereof. BACKGROUND

[0002] At present, China is the largest country in the world in terms of egg chicken breeding and consumption. With the increase of the age of egg chickens, the metabolism of vitamin D3 is disordered, which affects the absorption and deposition of calcium, and long-time egg production also affects the thickness and strength of egg shells. Calcium is the main component of egg shells, accounting for about 38%-40% of the weight of egg shells, and calcium deficiency in egg laying chickens can easily lead to reduced egg production and thin egg shells.

[0003] Vitamin D3 participates in the whole process of calcium and phosphorus metabolism in the body, is necessary for synthesizing calcium-binding egg proteins, activating bone calcium metabolism, and strengthening intestinal absorption of phosphorus metabolism, and is beneficial to adjusting the balance of calcium and phosphorus in the body.

[0004] 25-hydroxyvitamin D3 can directly enter the liver and then become active 1,25-2 hydroxyvitamin D3 in the kidney, promoting the absorption of calcium and the deposition in the egg shell. The bioavailability of 25-hydroxyvitamin D3 is 3-5 times that of ordinary vitamin D3.

[0005] At present, most of the commercially available products of 25-hydroxyvitamin D3 are liquid or water-insoluble powder products. The liquid products are prone to leakage and are unstable during transportation and storage. The water-insoluble products are inconvenient for farmers to add during on-site use, and the addition amount is low, which makes it difficult to uniformly disperse in the feed. Moreover, 25-hydroxy D3 is very sensitive to light and heat, and is easily oxidized and decomposed in the air, which can seriously affect the use of 25-hydroxyvitamin D3 products.

[0006] Therefore, it is necessary to develop a stable water-soluble 25-hydroxyvitamin D3 premix product as a feed additive for improving the quality of egg shells in the later egg production period and coping with high-temperature transportation and storage. SUMMARY

[0007] The present application aims to solve the technical problems in the prior art, and provides a 25-hydroxyvitamin D3 premix, a preparation method and application thereof.

[0008] To achieve the above purposes, the specific technical solutions of the present application are as follows:

[0009] In one aspect, the present application provides a 25-hydroxyvitamin D3 premix, the composition of the premix comprising: 25-hydroxyvitamin D3, an emulsifier, a stabilizer, a synergist, and a diluent.

[0010] The components and mass percentage in the premixing agent are: 25-hydroxy vitamin D3 0.008%-0.08%, emulsifier 0.08%-0.7%, stabilizer 0.3%-1.2%, synergist 0.8%-1.7%, and diluent supplementing to 100%.

[0011] Preferably, the components and mass percentage in the premixing agent are: 25-hydroxy vitamin D3 0.01%-0.06%, emulsifier 0.1%-0.5%, stabilizer 0.5%-1%, synergist 0.9%-1.3%, and diluent supplementing to 100%.

[0012] More preferably, the components and mass percentage in the premixing agent are: 25-hydroxy vitamin D3 0.03%, emulsifier 0.2%, stabilizer 0.8%, synergist 1.0%, and diluent supplementing to 100%.

[0013] The emulsifier is one or several of olive oil, Tween 80, tea oil, almond oil, glycerol, propylene glycol, glycerol monolaurate, preferably one or combination of olive oil and Tween 80, and more preferably olive oil.

[0014] The stabilizer is one or several of tea polyphenol, vitamin E, tert-butyl hydroquinone, ascorbic acid, glutathione, taurine, preferably one or combination of vitamin E and tert-butyl hydroquinone, and more preferably vitamin E.

[0015] The synergist is one or several of vitamin D3, vitamin A, vitamin B2, Eucommia ulmoides leaf extract, astragalus polysaccharide, lipoic acid, preferably one or combination of vitamin A, vitamin B2, Eucommia ulmoides leaf extract, and lipoic acid.

[0016] The diluent is one or several of sodium sulfate, sodium bicarbonate, lactose, malt dextrin, and anhydrous glucose, preferably one or combination of sodium bicarbonate and malt dextrin.

[0017] In another aspect of the present application, a preparation method of 25-hydroxy vitamin D3 premixing agent is provided, comprising the following steps:

[0018] (1) 25-hydroxy vitamin D3, emulsifier, stabilizer, synergist, and diluent are weighed according to the mass percentage respectively for standby;

[0019] (2) The stabilizer and emulsifier are heated to 50-90℃ for dissolution, then the 25-hydroxy vitamin D3 is added and stirred to become oil phase state;

[0020] (3) Put the reaction liquid obtained in step (2) into a homogenizer, add diluent and stir to mix evenly until it is moist. Then transfer it to a fluidized bed, blow in an airflow of 40℃-60℃, and continue to spray diluent to dry it, so as to obtain the powder to be used. The homogenization pressure is not less than 30MPa.

[0021] (4) The powder obtained in step (3) is passed through a 24-mesh sieve and mixed evenly with the synergist and the remaining diluent to obtain the final product.

[0022] In another aspect, the present invention provides an application of a 25-hydroxyvitamin D3 premix in improving the late-stage eggshell breakage rate, improving eggshell thickness, reducing the rate of soft-shelled eggs, and reducing the incidence of deformed eggs in the late-stage laying period of laying hens.

[0023] Preferably, the heating temperature in step (2) is 70°C.

[0024] The method of using the premix of this invention is as follows: Add 500g of this product per ton of feed when mixing with feed; add 250g of this product per ton of drinking water when adding drinking water. Long-term addition of this product will have better effects.

[0025] Beneficial effects:

[0026] 1. This invention prepares a water-soluble premix of 25-hydroxyvitamin D3 by emulsification and coating, forming an oil-in-water state in water, which not only has higher stability but also higher dispersibility, making it convenient for transportation and group administration.

[0027] 2. The premix obtained by this invention can withstand high temperature and light conditions in the air, and has higher stability under extreme conditions. It reduces the impact of high temperature environments during production, storage and transportation, and achieves a degradation rate far lower than that of commercially available products.

[0028] 3. This invention has a significant effect on improving the eggshell breakage rate, eggshell thickness, and soft-shelled eggs in the later stages of laying hens. Detailed Implementation

[0029] The above content will be further described in detail below through specific embodiments. However, this should not be construed as limiting the scope of the above subject matter to the following embodiments. All technologies implemented based on the content of this invention fall within the scope.

[0030] Example 1

[0031] A 25-hydroxyvitamin D3 premix contains 0.3g of 25-hydroxyvitamin D3, 2g of Tween 80, 8g of vitamin E, 2g of crude extract of Eucommia ulmoides leaves, 3g of alpha-lipoic acid, 4g of vitamin A, 1g of vitamin B2, 600g of sodium bicarbonate, and 379.7g of maltodextrin per 1kg of premix.

[0032] Example 2

[0033] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, tert-butyl hydroquinone 8g, Eucommia ulmoides leaf crude extract 2g, lipoic acid 3g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0034] Example 3

[0035] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, vitamin E 8g, Eucommia ulmoides leaf crude extract 2g, lipoic acid 3g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0036] Example 4

[0037] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, vitamin E 8g, Eucommia ulmoides leaf crude extract 2g, vitamin B2 1g, vitamin A 4g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0038] Example 5

[0039] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 1g, Tween 80 1g, vitamin E 8g, lipoic acid 4g, vitamin B2 1g, vitamin A 4g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0040] Example 6

[0041] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, vitamin E 8g, Eucommia ulmoides leaf crude extract 2g, lipoic acid 3g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0042] Example 7

[0043] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, vitamin E 8g, Astragalus polysaccharide 2g, lipoic acid 3g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of the premix agent.

[0044] Example 8

[0045] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.3g, olive oil 2g, ascorbic acid 8g, Eucommia ulmoides leaf extract 2g, lipoic acid 3g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 379.7g per 1kg of premix agent.

[0046] Example 9

[0047] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.1g, olive oil 1g, vitamin E 5g, Eucommia ulmoides leaf extract 2g, lipoic acid 2g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 384.9g per 1kg of premix agent.

[0048] Example 10

[0049] A 25-hydroxy vitamin D3 premix agent, containing 25-hydroxy vitamin D3 0.6g, olive oil 5g, vitamin E 10g, Eucommia ulmoides leaf extract 3g, lipoic acid 5g, vitamin A 4g, vitamin B2 1g, sodium bicarbonate 600g, malt dextrin 371.4g per 1kg of premix agent.

[0050] The preparation method of the 25-hydroxy vitamin D3 premix agent described in the above examples 1-10, comprising the following steps:

[0051] (1) 25-hydroxy vitamin D3, emulsifier, stabilizer, synergist, diluent are weighed according to the mass fraction respectively;

[0052] (2) The stabilizer and emulsifier are dissolved by heating to 70℃, then the 25-hydroxy vitamin D3 is added and stirred to form an oil phase state;

[0053] (3) The reaction liquid obtained in step (2) is put into a homogenizer, the diluent is added and stirred to mix uniformly to a wet state, then it is transferred into a fluidized bed, the airflow at 40-60℃ is blown in, and the diluent is continuously sprayed to dry it, obtaining a powder for use, the homogenization pressure is not less than 30MPa;

[0054] (4) The powder obtained in step (3) is passed through a 24 mesh screen and mixed uniformly with the synergist and the remaining diluent, and the 25-hydroxy vitamin D3 premix agent is obtained.

[0055] Comparative example 1

[0056] Referring to the composition and preparation process of example 1 of patent CN 107296152 A, an emulsion composition containing 25-hydroxy vitamin D3 is prepared.

[0057] Test example 1 25-hydroxy vitamin D3 water-soluble dispersion experiment

[0058] Experimental method:

[0059] Take 1000 g of the products of the above-mentioned Examples 1, 3, 5, 9, 10 and Comparative Example 1, dissolve them in 20 L of tap water at room temperature, and after dissolving, take 5 ml of the solution at 0, 8, 24 hours at three points of the upper, middle and lower parts of the solution, ultrasonic for 30 min, and then dilute to 50 ml with methanol, and filter with a 0.22 μm organic filter membrane, and then detect the content by liquid phase.

[0060] Liquid chromatography reference conditions:

[0061] a Chromatographic column: C18 column, 4.6 mm x 250 mm, particle size 5 μm or equivalent chromatographic column.

[0062] b Mobile phase: A phase is water phase, B phase is methanol, filtered with a 0.22 μm microporous organic filter membrane, and the gradient elution program is shown in Table 1.

[0063] c Flow rate: 1.0 mL / min.

[0064] d Column temperature: 40°C.

[0065] e Injection volume: 20 μL.

[0066] f Wavelength: 265 nm.

[0067] Table 1 Gradient elution program

[0068] Time, min Phase A, % Phase B, % 0.00 12 88 10.00 5 95 17.00 2 98 29.00 12 88 32.00 12 88

[0069] Determination:

[0070] Standard curve drawing

[0071] Accurately pipette the standard series solutions, and the concentration is from low to high, and then plot the standard curve with the concentration as the abscissa and the peak area as the ordinate.

[0072] Quantitative determination:

[0073] Inject the test sample solution into the liquid chromatograph, and then the result is substituted into the standard curve, and the content is calculated by the peak area according to the external standard method.

[0074] Result calculation:

[0075] The content of 25-hydroxyvitamin D3 in the sample is calculated according to the following formula:

[0076]

[0077] In the formula:

[0078] W - 25-hydroxyvitamin D3 in the sample, in milligrams per gram (mg / g);

[0079] c - concentration of 25-hydroxyvitamin D3 in the sample solution in micrograms per milliliter, converted to milligrams per milliliter (mg / mL) based on the dilution factor, as derived from the standard curve;

[0080] V - final volume of the sample solution in milliliters (mL);

[0081] m - mass of the sample in grams (g);

[0082] The calculation result is rounded to three significant figures, and the absolute difference between two independent measurement results obtained under repeatability conditions should not exceed 10% of the arithmetic mean.

[0083] 1.2 Experimental results:

[0084] Table 2 Water-soluble dispersibility test

[0085]

[0086] From the above table, it can be seen that the average decrease of 25-hydroxyvitamin D3 in Examples 3, 5, 9 and 10 of the present application is relatively advantageous, all being less than 1%. In particular, the decrease in Examples 3, 9 and 10 is the smallest, being 0.22%, 0.67% and 0.22% respectively. This can meet the limitation of the maximum use time on site. In addition, the content difference between the upper layer and the lower layer in Example 3 is 0.01 mg / kg, which is much better than 0.76 mg / kg of Comparative Example 1. This can indicate that the process examples 3, 9 and 10 of the present application can be uniformly dispersed in water after standing for 24 hours, meeting the water line use on site.

[0087] Test Example 2 Comparison of stability of each embodiment of the present application

[0088] Experimental method: The products of Examples 1-3, 8-10 and Comparative Example 1 and commercially available 25-hydroxyvitamin D3 powder (having the same content as Example 3) were placed in a 60°C oven, and the content was detected on the 5th day and the 10th day to verify the stability comparison between each example and Comparative Example 1.

[0089] Experimental records:

[0090] Table 3 Stability test

[0091]

[0092]

[0093] From the above experimental results, it can be seen that the examples of the present application are relatively stable at 60°C for 5 days, and no obvious degradation occurs, and the degradation rate is not more than 30% on the 10th day. The degradation rate of Example 3 is the lowest, which is 13.3%, followed by Example 9 and Example 10, which are 20% and 15%, respectively. However, the commercial product and Comparative Example 1 both show obvious degradation on the 5th day, and the degradation rate is particularly obvious on the 10th day. It can be seen that the process of the present application can improve the influence of 25-hydroxy D3 at high temperature, and has more advantages than the commercial product.

[0094] Clinical application experiment of test example 3

[0095] Experimental animals and grouping:

[0096] In this experiment, 540-day-old Hyline Brown egg-laying chickens were selected, about 40,500, which were randomly divided into 8 groups. The first to seventh groups were given the products prepared by Examples 3-7, 9 and 10 of the present application, mixed with water, and 50g of the product of the present application was added per ton of water, and used for 21 days. The eighth group was a blank control group, which was fed according to the normal feeding procedure, and the external environment of each group was the same.

[0097] Detection index:

[0098] Observation of egg production rate and broken egg rate

[0099] Experimental records and analysis:

[0100] Table 4 Improvement of the additive of the present application on eggshell

[0101]

[0102]

[0103] From the above table, it can be seen that the examples of the present application have no obvious improvement effect on the improvement of egg production rate, but can also maintain the stable egg production rate compared with the blank control group. However, there are relatively obvious effects on the broken egg rate. Among them, the broken egg rate of Example 3 group, Example 9 group and Example 10 group is reduced by 49.6%, 35.9% and 47.1% respectively after 14 days of use, and the broken egg rate of Examples 4-7 is reduced by 4.2%, 0.7%, 4.6% and 16.4% respectively, and the egg production rate and broken egg rate of the blank control group are not improved.

[0104] Clinical comparison test of eggshell improvement effect of test example 4

[0105] Experimental method: select a 540 days old sea lane brown egg chicken and divide it into 6 groups randomly, the first-3 groups are the premix prepared in example 3, example 9, example 10, the 4th group is the commercial product 1, the 5th group is the commercial product 2, the main component of the experimental group is 25-hydroxy vitamin D3, the 6th group is the control group, give normal diet. The experimental period is 30 days, the dosages of each experimental group are consistent, record the dead rate, soft broken shell egg rate and feed egg ratio before and after the experiment.

[0106] Table 5 improvement of the additive of the application to the egg shell

[0107] Group Dead rate, % Soft broken shell egg rate, % Feed egg ratio 1st group 1.95 ± 0.5 ** ]] 3.93 ± 0.27 ** ]] 2.31 ± 1.46 * ]] 2nd group 2.01 ± 0.2 * ]] 4.12 ± 0.35 * ]] 2.38±1.28 3rd group 1.96 ± 0.6 ** ]] 4.02 ± 0.26 * ]] 2.37±1.62 4th group 2.01 ± 0.4 * ]] 4.44±0.47 2.39±1.33 5th group 2.21±0.1 4.35 ± 0.36 * ]] 2.39±1.56 6th group 2.52±1.2 5.25±0.42 2.49±1.62

[0108] Note: * indicates that the difference between the same column data is significant (P<0.05), ** indicates that the difference between the same column data is extremely significant (P<0.01)

[0109] Experimental conclusion:

[0110] From the above table, the first three experimental groups have more advantages in dead rate, soft broken shell egg rate and feed egg ratio than the blank control group, and the three indicators corresponding to the premix prepared in example 3, example 9, example 10 (experimental group 1-3) are significantly different (P<0.05) compared with other groups, which shows that the product of the application is better than the commercial product group, and can effectively reduce the dead rate and feed egg ratio.

[0111] The above is only the preferred embodiment of the application, it should be pointed out that for ordinary skilled in the art, without departing from the technical principles of the application, can make a number of improvements and refinements, these improvements and refinements should also be considered as the protection scope of the application.

Claims

1. A 25-hydroxyvitamin D3 premix characterized in that, The components and mass percentage in the premix are: 25-hydroxy vitamin D3 0.01%-0.06%, emulsifier 0.1%-0.5%, stabilizer 0.5%-1%, synergist 0.9%-1.3%, diluent to 100%; the emulsifier is olive oil; the stabilizer is vitamin E; the synergist is vitamin A, vitamin B2, crude extract of Eucommia ulmoides leaf, thioctic acid; the diluent is sodium bicarbonate and maltodextrin.

2. The 25-hydroxyvitamin D3 premix according to claim 1, characterized in that, The components and mass percentage in the premix are: 25-hydroxy vitamin D3 0.03%, emulsifier 0.2%, stabilizer 0.8%, synergist 1.0%, diluent to 100%.

3. A process for the preparation of a 25-hydroxyvitamin D3 premix as claimed in any one of claims 1-2, characterized in that, The method comprises the following steps: (1) 25-hydroxy vitamin D3, emulsifier, stabilizer, synergist and diluent are weighed according to the mass percentage respectively for standby; (2) the stabilizer and emulsifier are heated to 50-90℃ to dissolve, then 25-hydroxy vitamin D3 is added to stir to become oil phase state; (3) the reaction liquid obtained in step (2) is put into a homogenizer, diluent is added to stir to mix uniformly to a moist state, then it is transferred into a fluidized bed, 40-60℃ air flow is blown in, diluent is continuously sprayed to dry, to obtain standby powder, the homogenization pressure is not less than 30MPa; (4) the powder obtained in step (3) is passed through a 24 mesh screen, mixed with synergist and the remaining diluent uniformly, to obtain the product.

4. The use of 25-hydroxy vitamin D3 premix as claimed in any one of claims 1-2 in improving the late-stage eggshell breaking rate of poultry, improving eggshell thickness, reducing soft-shell egg rate, and reducing the incidence of abnormal eggs in the late stage of laying hens.

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