Feed additive of egg shell improver for laying hens as well as preparation method and application of feed additive

Abstract

The invention relates to the technical field of feed additives, and provides a feed additive of a laying hen eggshell improver as well as a preparation method and application of the feed additive. The feed additive of the egg shell improver for the laying hens comprises the following raw materials: glutathione, vitamin E, calcium acetate, potassium chloride, organic selenium and a caulis spatholobi extract, and a preparation method of the caulis spatholobi extract comprises the following steps: crushing and sieving caulis spatholobi to obtain caulis spatholobi powder; adding the caulis spatholobi powder into water, performing ultrasonic extraction, and filtering to obtain a first extracting solution and first filter residues; adding the first filter residue into a mixed extracting agent, performing reflux extraction, and filtering to obtain a second extracting solution and a second filter residue; mixing the first extracting solution and the second extracting solution, and performing extraction, vacuum concentration and drying to obtain a caulis spatholobi extract; the mixed extracting agent consists of ethanol and propylene glycol in a mass ratio of (6-7): 3. According to the technical scheme, the problem that the eggshell quality improvement effect of an eggshell improver in a feed additive in the related technology is poor is solved.

Description

Technical Field

[0001] This invention relates to the field of feed additive technology, specifically to a feed additive that is an eggshell improver, its preparation method, and its application. Background Technology

[0002] Eggshell quality is a key indicator for evaluating the profitability of egg-laying hen farming, directly affecting the commercial value, storage stability, and transportation safety of eggs. Its quality level has a decisive impact on the economic benefits of the egg-laying hen industry. According to industry statistics, the economic losses caused by eggshell quality problems in my country's egg-laying hen industry reach 2-3 billion yuan annually. Taking a large-scale farm with 100,000 egg-laying hens as an example, the loss due to eggshell quality problems alone can reach 1.33 million yuan in a single breeding cycle, accounting for as much as 8% of total losses.

[0003] To improve eggshell quality, various eggshell improvers have been developed and applied in laying hen farming. Their core technologies primarily focus on directly supplementing trace elements such as calcium and phosphorus, or adding vitamin D3 to enhance calcium metabolism regulation. However, practical applications have shown that these improvers have insufficient effectiveness. When eggshells are thin, brittle, or easily broken, the pass rate of marketable eggs drops significantly, and broken eggs cannot be sold normally, directly leading to wasted production at the farming end. Insufficient eggshell density allows for easy loss of internal moisture and leakage of carbon dioxide, resulting in a shortened shelf life and increased risk of spoilage during storage. Weak eggshells are also more susceptible to compression and impact during transportation and handling, causing a surge in breakage rates and increasing logistics losses and after-sales dispute costs.

[0004] Therefore, it is very necessary to develop a feed additive that can effectively improve the quality of eggshells. Summary of the Invention

[0005] This invention proposes a feed additive for improving eggshell quality, its preparation method, and its application, which solves the problem that eggshell improvers in feed additives are not effective in improving eggshell quality in related technologies.

[0006] The technical solution of this invention is as follows: This invention proposes a feed additive for improving eggshell quality, comprising the following components by weight: 20-30 parts glutathione, 15-25 parts vitamin E, 90-100 parts calcium acetate, 20-30 parts potassium chloride, 10-20 parts organic selenium, and 15-25 parts chicken blood vine extract. The preparation method of the chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine into powder, sieve it, and obtain chicken blood vine powder; S2. Add the chicken blood vine powder to water, extract with ultrasound, and then filter to obtain the first extract and the first filter residue. S3. Add the first filter residue to the mixed extractant, reflux extract and filter to obtain the second extract and the second filter residue. S4. The first extract and the second extract are mixed to obtain a mixed extract. The mixed extract is then extracted, concentrated under reduced pressure and dried to obtain the chicken blood vine extract. The mixed extractant consists of ethanol and propylene glycol in a mass ratio of 6-7:3.

[0007] As a further technical solution, in step S1, the particle size of the chicken blood vine powder is 30-40 mesh.

[0008] As a further technical solution, in step S2, the mass ratio of water to chicken blood vine powder is 10~12:1.

[0009] As a further technical solution, in step S2, the ultrasonic extraction time is 20~35 min, the ultrasonic extraction temperature is 50~60℃, and the ultrasonic extraction power is 200~250W.

[0010] As a further technical solution, in step S3, the mass ratio of the mixed extractant to the first filter residue is 12~15:1.

[0011] As a further technical solution, in step S3, the temperature of the reflux extraction is 50~60℃, and the reflux extraction time is 20~30min.

[0012] As a further technical solution, in step S4, the extraction, vacuum concentration and drying includes the following steps: adding the mixed extract to the first extractant, extracting to obtain an organic phase and an aqueous phase, collecting the organic phase, dehydrating to obtain the first extract, adding the aqueous phase to the second extractant, extracting to obtain the organic phase, dehydrating to obtain the second extract, mixing the first extract and the second extract, concentrating and drying under vacuum to obtain the chicken blood vine extract.

[0013] As a further technical solution, the first extractant is ethyl acetate, and the second extractant is composed of n-butanol and ethyl acetate in a mass ratio of 7~9:1.

[0014] In the feed additive of this invention, during the preparation of *Spatholobus suberectus* extract, the first extractant is ethyl acetate, which has high selectivity for fat-soluble flavonoids and lignans in *Spatholobus suberectus*. This allows for precise separation of fat-soluble blood-activating and blood-tonifying active ingredients and estrogen-like active ingredients from the mixed extract, avoiding mixing with water-soluble impurities. The second extractant is a mixture of n-butanol and ethyl acetate in a mass ratio of 7-9:1. This utilizes the high solubility of n-butanol for moderately polar active ingredients, while the small amount of ethyl acetate fine-tunes the solvent polarity, forming a gentle polarity gradient with the preceding ethyl acetate extraction system. This reduces component residue and helps the *Spatholobus suberectus* extract function effectively in the feed additive, improving eggshell quality.

[0015] As a further technical solution, the volume ratio of the first extractant to the mixed extract is 1:1.

[0016] As a further technical solution, the volume ratio of the aqueous phase to the second extractant is 1:1.

[0017] This invention also proposes a method for preparing an eggshell improver feed additive, which includes the following steps: D1. Mix the glutathione, vitamin E and chicken blood vine extract to obtain preparation A; D2. Mix the calcium acetate, potassium chloride, and organoselenium to obtain formulation B; D3. Mix the formulation A and the formulation B to obtain the eggshell improver as a feed additive.

[0018] As a further technical solution, in step D1, the mixing time is 15 minutes; in step D2, the mixing time is 7 minutes; and in step D3, the mixing time is 7 minutes.

[0019] The present invention also proposes the application of the eggshell improver feed additive prepared by the method of preparing the eggshell improver feed additive to improve eggshell quality.

[0020] The working principle and beneficial effects of this invention are as follows: 1. In this feed additive, a highly efficient liver protection and antioxidant network is constructed through the triple synergy of glutathione, vitamin E, and organic selenium. The liver, as the core organ for vitamin D3 activation and calcium metabolism regulation, directly determines eggshell quality. Glutathione, as an endogenous antioxidant, can directly scavenge reactive oxygen species within liver cells; vitamin E, as a fat-soluble antioxidant, targets and protects the integrity of liver cell membrane structures, reducing oxidative damage; organic selenium not only possesses antioxidant activity itself, but more importantly, as an essential component of glutathione peroxidase, it can significantly improve the bioavailability and antioxidant activity of glutathione. Calcium acetate, as a high-quality soluble calcium source, can directly provide easily absorbed calcium raw materials for eggshell formation; potassium chloride, by regulating the osmotic pressure and ion balance of the hen's body fluids, creates a suitable physiological environment for the absorption of calcium ions by intestinal mucosal cells, while simultaneously activating the activity of intestinal calcium transport proteins; and vitamin D3, efficiently activated by the liver, can further promote the active transport of calcium acetate in the intestine under the suitable environment created by potassium chloride. The blood-activating and blood-tonifying effects of chicken blood vine extract can improve blood circulation in the shell gland area, accelerate the transport rate of calcium ions to the shell gland, and ensure timely deposition of calcium carbonate. The synergistic effect of the six components effectively improves the quality of eggshells.

[0021] 2. In the extraction process of the chicken blood vine extract of the present invention, a step-by-step extraction method is adopted. The first extraction uses water, and the second extraction uses a mixed solution composed of ethanol and propylene glycol. The combination of the two extractions covers both water-soluble and fat-soluble core active ingredients in chicken blood vine, which greatly improves the comprehensiveness of extraction and helps chicken blood vine extract play a role in feed additives and improve the quality of eggshells. Detailed Implementation

[0022] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0023] Example 1 A feed additive for improving eggshell quality, comprising the following components in parts by weight: 20 parts glutathione, 15 parts vitamin E, 90 parts calcium acetate, 20 parts potassium chloride, 10 parts organic selenium, and 15 parts chicken blood vine extract. The preparation method of chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine, sieve it, and obtain chicken blood vine powder with a particle size of 30 mesh; S2. Add chicken blood vine powder to water, with a mass ratio of water to chicken blood vine powder of 10:1. Extract with ultrasound at 50℃ and 200W power for 35 minutes, then filter to obtain the first extract and the first filter residue. S3. Add the first filter residue to the mixed extractant, with a mass ratio of the mixed extractant to the first filter residue of 12:1. Reflux at 50℃ for 30 min and then filter to obtain the second extract and the second filter residue. The mixed extractant consists of ethanol and propylene glycol in a mass ratio of 2:1. S4. The first extract and the second extract are mixed to obtain a mixed extract. The mixed extract is extracted twice with ethyl acetate (the volume ratio of ethyl acetate to the mixed extract is 1:1). The organic phases are combined, concentrated and dried under reduced pressure to obtain chicken blood vine extract. A method for preparing a feed additive containing eggshell conditioner includes the following steps: D1. Mix glutathione, vitamin E and chicken blood vine extract for 15 minutes to obtain preparation A; D2. Mix calcium acetate, potassium chloride and organoselenium for 7 minutes to obtain preparation B; D3. Mix formulation A and formulation B for 7 minutes to obtain the eggshell improver feed additive.

[0024] Example 2 A feed additive for improving eggshell quality, comprising the following components in parts by weight: 25 parts glutathione, 20 parts vitamin E, 95 parts calcium acetate, 25 parts potassium chloride, 15 parts organic selenium, and 20 parts chicken blood vine extract. The preparation method of chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine, sieve it, and obtain chicken blood vine powder with a particle size of 30 mesh; S2. Add chicken blood vine powder to water, with a mass ratio of water to chicken blood vine powder of 11:1. Extract with ultrasound at 55℃ and 200W power for 25 minutes, then filter to obtain the first extract and the first filter residue. S3. Add the first filter residue to the mixed extractant, with a mass ratio of the mixed extractant to the first filter residue of 13:1. Reflux at 55℃ for 25 min and then filter to obtain the second extract and the second filter residue. The mixed extractant consists of ethanol and propylene glycol in a mass ratio of 2:1. S4. The first extract and the second extract are mixed to obtain a mixed extract. The mixed extract is extracted twice with ethyl acetate (the volume ratio of ethyl acetate to the mixed extract is 1:1). The organic phases are combined, concentrated and dried under reduced pressure to obtain chicken blood vine extract. A method for preparing a feed additive containing eggshell conditioner includes the following steps: D1. Mix glutathione, vitamin E and chicken blood vine extract for 15 minutes to obtain preparation A; D2. Mix calcium acetate, potassium chloride and organoselenium for 7 minutes to obtain preparation B; D3. Mix formulation A and formulation B for 7 minutes to obtain the eggshell improver feed additive.

[0025] Example 3 A feed additive for improving eggshell quality, comprising the following components in parts by weight: 30 parts glutathione, 25 parts vitamin E, 100 parts calcium acetate, 30 parts potassium chloride, 20 parts organic selenium, and 25 parts chicken blood vine extract. The preparation method of chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine, sieve it, and obtain chicken blood vine powder with a particle size of 30 mesh; S2. Add chicken blood vine powder to water, with a mass ratio of water to chicken blood vine powder of 12:1. Extract with ultrasound at 60℃ and 250W power for 20 minutes, then filter to obtain the first extract and the first filter residue. S3. Add the first filter residue to the mixed extractant, with a mass ratio of the mixed extractant to the first filter residue of 15:1. Reflux at 60℃ for 20 min and then filter to obtain the second extract and the second filter residue. The mixed extractant consists of ethanol and propylene glycol in a mass ratio of 2:1. S4. The first extract and the second extract are mixed to obtain a mixed extract. The mixed extract is extracted twice with ethyl acetate (the volume ratio of ethyl acetate to the mixed extract is 1:1). The organic phases are combined, concentrated and dried under reduced pressure to obtain chicken blood vine extract. A method for preparing a feed additive containing eggshell conditioner includes the following steps: D1. Mix glutathione, vitamin E and chicken blood vine extract for 15 minutes to obtain preparation A; D2. Mix calcium acetate, potassium chloride and organoselenium for 7 minutes to obtain preparation B; D3. Mix formulation A and formulation B for 7 minutes to obtain the eggshell improver feed additive.

[0026] Example 4 The difference between Example 4 and Example 2 is that the mixed extractant consists of ethanol and propylene glycol in a mass ratio of 7:3.

[0027] Example 5 The difference between Example 5 and Example 4 is that ethyl acetate in the extraction process is replaced with n-butanol.

[0028] Example 6 Compared with Example 4, the difference in Example 6 is that step S4 in the preparation method of the chicken blood vine extract in this example includes the following steps: mixing the first extract and the second extract to obtain a mixed extract; adding the mixed extract to ethyl acetate (the volume ratio of ethyl acetate to the mixed extract is 1:1); extracting to obtain an organic phase and an aqueous phase; collecting the organic phase; dehydrating to obtain the first extract; adding the aqueous phase to the second extractant (the volume ratio of the second extractant to the mixed extract is 1:1); extracting to obtain the organic phase; dehydrating to obtain the second extract; mixing the first extract and the second extract; concentrating and drying under reduced pressure to obtain the chicken blood vine extract, wherein the second extractant is composed of n-butanol and ethyl acetate in a mass ratio of 7:1.

[0029] Example 7 The difference between Example 7 and Example 4 is that the second extractant consists of n-butanol and ethyl acetate in a mass ratio of 9:1.

[0030] Comparative Example 1 Compared with Example 2, Comparative Example 1 differs in that the preparation method of the chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine, sieve it, and obtain chicken blood vine powder with a particle size of 30 mesh; S2. Add chicken blood vine powder to water, with a mass ratio of water to chicken blood vine powder of 11:1. Extract with ultrasound at 55℃ and 200W power for 25 minutes, then filter to obtain extract and filter residue. S3. The extract was extracted twice with ethyl acetate (the volume ratio of ethyl acetate to extract was 1:1), the organic phases were combined, concentrated and dried under reduced pressure to obtain the chicken blood vine extract.

[0031] Comparative Example 2 Compared with Example 2, the difference of Comparative Example 2 is that in the preparation method of Chicken Blood Vine Extract, the mixing extractant in step S3 is only ethanol.

[0032] Experimental Example 1 For the *Spatholobus suberectus* extracts obtained in Examples 1-7 and Comparative Examples 1-2, the NaNO2-Al(NO3)3 colorimetric method was used to plot rutin standard curves at a wavelength of 510 nm, and linear regression was performed to obtain the equation. The *Spatholobus suberectus* extracts from each group were dissolved in 95% ethanol and diluted to volume with distilled water to obtain extract samples. The extract samples from each group were then subjected to color development and testing under the same conditions. Substituting the results into the regression equation, the total flavonoid content in each group of *Spatholobus suberectus* extracts could be calculated, and thus the total flavonoid yield could be calculated.

[0033] The test results are shown in Table 1: Table 1 Performance test results of Examples 1-7 and Comparative Examples 1-2

[0034] As shown in Table 1, the yield of total flavonoids in the chicken blood vine extract can be increased when a two-stage extraction process of water extraction followed by a mixture of ethanol and propylene glycol is adopted. When the second extractant is composed of n-butanol and ethyl acetate, the yield of total flavonoids in the chicken blood vine extract is even higher.

[0035] Experiment Example 2 Five hundred 390-day-old Jingfen No. 6 chickens were randomly divided into two groups: experimental group A and control group B, with 250 chickens in each group. The experimental group was fed the feed additive containing 100 kg of eggshell improver per ton of feed for 30 consecutive days. The control group was fed normally. After 30 days, 20 eggs were randomly selected from each group, and the eggshell gloss, color, thickness, strength, deformation value, and dark spots were measured. Eggshell gloss was measured using a Nove-Gloss Flex60 instrument, eggshell color using a QCR instrument, eggshell thickness using an ETG-1061A instrument, eggshell strength using an FGX-5R instrument, and dark spots were observed by candling.

[0036] The test results are shown in Table 2: Table 2 Performance test results of the experimental group and the control group

[0037] Experimental Example 3 Five hundred Hy-Line Brown chickens aged 360 days were randomly divided into two groups: experimental group C and control group D, with 250 chickens in each group. The experimental group was fed a feed additive containing 100 kg of eggshell improver per ton of feed for 30 consecutive days. The control group was fed normally. After 30 days, 20 eggs were randomly selected from each group, and the eggshell gloss, color, thickness, strength, deformation value, and dark spots were measured. Eggshell gloss was measured using a Nove-Gloss Flex60 instrument, eggshell color using a QCR instrument, eggshell thickness using an ETG-1061A instrument, eggshell strength using an FGX-5R instrument, and dark spots were observed by candling.

[0038] The test results are shown in Table 3: Table 3 Performance test results of the experimental group and the control group

[0039] As shown in Tables 2 and 3, the eggshell improver prepared by this invention has good feed additive effects. It can improve the gloss, thickness and strength of the eggshell, significantly improve the color and uniformity of the eggshell, and reduce the number of eggs with dark spots. It has significant economic benefits and application prospects.

[0040] The above are merely preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A feed additive containing an eggshell improver, characterized in that, The raw materials include the following components in parts by weight: glutathione 20-30 parts, vitamin E 15-25 parts, calcium acetate 90-100 parts, potassium chloride 20-30 parts, organic selenium 10-20 parts, and chicken blood vine extract 15-25 parts. The preparation method of the chicken blood vine extract includes the following steps: S1. Crush the chicken blood vine into powder, sieve it, and obtain chicken blood vine powder; S2. Add the chicken blood vine powder to water, extract with ultrasound, and then filter to obtain the first extract and the first filter residue. S3. Add the first filter residue to the mixed extractant, reflux extract and filter to obtain the second extract and the second filter residue. S4. The first extract and the second extract are mixed to obtain a mixed extract. The mixed extract is then extracted, concentrated under reduced pressure and dried to obtain the chicken blood vine extract. The mixed extractant consists of ethanol and propylene glycol in a mass ratio of 6-7:

3.

2. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S1, the particle size of the chicken blood vine powder is 30-40 mesh.

3. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S2, the mass ratio of water to chicken blood vine powder is 10~12:

1.

4. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S2, the ultrasonic extraction time is 20-35 minutes, the ultrasonic extraction temperature is 50-60°C, and the ultrasonic extraction power is 200-250W.

5. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S3, the mass ratio of the mixed extractant to the first filter residue is 12~15:

1.

6. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S3, the reflux extraction temperature is 50~60℃, and the reflux extraction time is 20~30min.

7. The feed additive of eggshell conditioner according to claim 1, characterized in that, In step S4, the extraction, concentration and drying include the following steps: adding the mixed extract to the first extractant, extracting to obtain an organic phase and an aqueous phase, collecting the organic phase, dehydrating to obtain the first extract, adding the aqueous phase to the second extractant, extracting to obtain the organic phase, dehydrating to obtain the second extract, mixing the first extract and the second extract, concentrating and drying under reduced pressure to obtain the chicken blood vine extract.

8. The feed additive of eggshell conditioner according to claim 7, characterized in that, The first extractant is ethyl acetate, and the second extractant is composed of n-butanol and ethyl acetate in a mass ratio of 7 to 9:

1.

9. A method for preparing a feed additive containing an eggshell improver, used to prepare a feed additive containing an eggshell improver as described in any one of claims 1 to 8, characterized in that, Includes the following steps: D1. Mix the glutathione, vitamin E and chicken blood vine extract to obtain preparation A; D2. Mix the calcium acetate, potassium chloride, and organoselenium to obtain formulation B; D3. Mix the formulation A and the formulation B to obtain the eggshell improver as a feed additive.

10. The feed additive for improving eggshell quality prepared by the method of preparing an eggshell improver according to any one of claims 1 to 8 or claim 9, and its application in improving eggshell quality.

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