CN102524521A - Preparation method of eggshell hydrolysate, as well as product and application of eggshell hydrolysate - Google Patents
Preparation method of eggshell hydrolysate, as well as product and application of eggshell hydrolysate Download PDFInfo
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Abstract
The invention discloses a preparation method of eggshell hydrolysate. The preparation method comprises the following specific steps of: collecting eggshells, and washing the collected eggshells to obtain the clean eggshells; placing the washed eggshells into an electrolyte solution prepared by a mixed solution of sodium chloride and hydrochloric acid for sterilization; collecting the sterilized eggshells, then drying and smashing the sterilized eggshells; and adding hydrochloric acid or acetic acid for carrying out acidolysis till the eggshells react with the hydrochloric acid or the acetic acid completely, filtering, collecting a filtrate, and obtaining the eggshell hydrolysate. The preparation method is simple, is low in cost, does not need any special equipment or reagent; and the prepared eggshell hydrolysate contains elements such as calcium, phosphorus, magnesium, and zinc, and can be used for improving the laying rate of poultry in later egg-laying period.
Description
Technical field
The present invention relates to chemical field, particularly the preparation method of eggshell hydrolyzate also relates to eggshell hydrolyzate obtained by this method and application thereof.
Background technology
Poultry (for example: egg duck, laying hen etc.) has egg-laying peak in the process of laying eggs; In case crossed egg-laying peak, laying rate can significantly descend, and the quality of eggshell also can descend simultaneously; Improve, produce soft-shelled egg, husky shell egg etc. like breakage rate, had a strong impact on economic benefit.Nutrition is the key factor that influences laying rate and eggshell quality, to a certain extent laying rate is had improvement to a certain degree through replenishing elements such as an amount of calcium, phosphorus, magnesium, zinc.If but the ratio of adding element is inappropriate, can produce a series of side effect, too much as adding calcium in the feed, can cause the hypefcalcipexy of eggshell and egg shell membrane, can make the eggshell color thin out, the tone variation; Too much can influence the acid-base balance in the poultry body like phosphorus, influence eggshell quality.Contain multiple elements such as calcium, phosphorus, magnesium, zinc in the eggshell itself, content is higher, and balanced in nutrition, is the natural material that improves eggshell quality.The a large amount of eggshells that produce behind hatching back or the processing egg based foodstuff are at present mostly abandoned and are underutilized as rubbish, and resource is underutilized on the one hand, brings very big pressure to environmental improvement on the other hand.
Therefore, be badly in need of a kind of preparation method of eggshell hydrolyzate, the preparation method is simple, and non-environmental-pollution is with low cost.
Summary of the invention
In view of this, one of the object of the invention is to provide a kind of preparation method of eggshell hydrolyzate, and this method is simple to operate, does not need special installation, and production cost is low.
For realizing above-mentioned technical purpose, technical scheme is:
The preparation method of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect eggshell, the eggshell of collecting is cleaned, obtain clean egg shell, subsequent use;
B. sterilization
With carrying out disinfection in the electrolyte of step a gained eggshell adding by the mixed solution preparation of sodium chloride and hydrochloric acid, collect eggshell, oven dry is pulverized, and gets egg-shell meal, and is subsequent use;
C. acidolysis
Step b gained egg-shell meal is added the pH value be not less than 3 hydrochloric acid, acidolysis at least 1.5 hours; Add concentration again and be not less than the hydrochloric acid of 5mol/L, acidolysis at least 2 hours, the eggshell hydrolyzate;
Or be equivalent to egg-shell meal weight 1-1.5 acetic acid doubly with adding in the step b gained egg-shell meal, acidolysis 1-2 hour, add again and be equivalent to egg-shell meal weight 2-3 acetic acid doubly, acidolysis at least 5 hours.
Further, said step a is with the eggshell water ultrasonic cleaning of collecting 20-30 minute, and water cleans 3-5 time again.
Further, said step b adds to be equivalent to eggshell volume 2-5 electrolyte doubly, sterilizes 10-60 minute.
Further, among the said step b, the available chlorine content of said electrolyte is for being not less than 80ppm.
Further, the preparation method of electrolyte that available chlorine content is not less than 80ppm does, is that 0.085-0.85mol/L, concentration of hydrochloric acid are the mixed solution of 0.01-0.1mol/L with sodium chloride concentration, under the 220V voltage conditions, makes in electrolysis 1-2 hour.
Further, the preparation method of electrolyte that said available chlorine content is not less than 80ppm does, is that 0.5mol/L, concentration of hydrochloric acid are the mixed solution of 0.05mol/L with sodium chloride concentration, and electrolysis made in 1 hour under the 220V voltage conditions.
Further, said step c adds step b gained egg-shell meal to be equivalent to the hydrochloric acid of egg-shell meal weight 6-8 pH value doubly for 3-4, acidolysis 1-2 hour; Adding and being equivalent to egg-shell meal weight 0.5-5 concentration doubly is the hydrochloric acid of 5-10mol/L, acidolysis 2-3 hour.
The little pioneer E2 type sterilizing machine that the instrument that electrolysis is used among the present invention is produced as the Beijing XinnHuiChang Biology Safety Technology Co., Ltd.
Two of the object of the invention is to provide the eggshell hydrolyzate of above-mentioned preparation method's preparation, and eggshell hydrolyzate kind contains calcium, phosphorus, and manganese, elements such as magnesium and zinc, and the eggshell hydrolyzate prepares process and passes through sterilisation step, can avoid the risk of transmission.
For solving above-mentioned purpose, technical scheme is:
Utilize the eggshell hydrolyzate of preparation method's preparation of said eggshell hydrolyzate.
Three of the object of the invention is to provide the application of eggshell hydrolyzate in the raising poultry is laid eggs the later stage laying rate, and balanced in nutrition, technical scheme is:
The application of said eggshell hydrolyzate in improving the poultry laying rate.
Further, said poultry is a duck.
Beneficial effect of the present invention is: the invention discloses the preparation method of eggshell hydrolyzate, its preparation method is simple, and cost is low, does not need special installation; Adopt electrolyte to carry out disinfection in the preparation process, sterilization is thorough, and sterilization method is simple, does not produce harmful substance after the sterilization, can not pollute environment; In the acidolysis process, the substep acid hydrolyzation is adopted in acidolysis, the control reaction speed; Main hydrochloric acid and acetic acid and egg-shell meal reaction produce a large amount of hydrogen; The hydrochloric acid or a part of acetic acid that add low concentration earlier after reaction a period of time, add the hydrochloric acid or the remaining acetic acid of high concentration again; Avoid reaction too violent, prevent to splash; The invention also discloses eggshell hydrolyzate obtained by this method, in the eggshell hydrolyzate in the eggshell hydrolyzate nutriment abundant, comprise calcium, phosphorus, manganese, magnesium, zinc etc.; And content is high; Be respectively calcium 15.50mg/ml, phosphorus 0.084 mg/ml, manganese 0.31 μ g/ml; Magnesium 38.78 μ g/ml, zinc 2.93 μ g/ml; Also disclose the application of eggshell hydrolyzate, feeding lays eggs can obviously improve the laying rate in egg duck later stage behind the egg duck in later stage, and it is about 10% that laying rate improves, and eggshell quality is good, and therefore no calcium deposition can increase economic efficiency.
The specific embodiment
Below will combine embodiment that the present invention is carried out detailed description.The experimental technique of unreceipted actual conditions in the preferred embodiment is usually according to normal condition.
Embodiment 1
The preparation of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect egg shell, water ultrasonic cleaning 20 minutes, water cleans 5 times again, obtains clean egg shell, and is subsequent use;
B. sterilization
Step a gained eggshell is added the electrolyte that is equivalent to 5 times of eggshell volumes, sterilized 30 minutes, collect eggshell then, eggshell is dried under 100 ℃ of conditions, pulverize, get egg-shell meal, subsequent use; Wherein electrolyte is to be that sodium chloride and the electrolysis under the 220V condition of 0.05mol/L hydrochloric acid of 0.5mol/L made in 1 hour with concentration, and effective chlorine density is 800ppm in the electrolyte that makes, and is subsequent use.
C. acidolysis
In step b gained egg-shell meal, add 10 times pH value being equivalent to egg-shell meal weight and be 3 hydrochloric acid solution, do not stop stirring, acidolysis 1.5 hours; In reactant liquor, adding the concentration that is equivalent to 0.5 times of egg-shell meal weight again is the hydrochloric acid of 10mol/L, does not stop to stir, and acidolysis 2 hours is filtered, and collects filtrating, promptly gets the eggshell hydrolyzate.
The eggshell hydrolyzate pH value of present embodiment preparation is 6, and calcium, phosphorus, manganese, magnesium, zinc concentration are respectively calcium 15.50mg/mL in the eggshell hydrolyzate, phosphorus 0.084 mg/mL, manganese 0.31 μ g/mL, magnesium 38.78 μ g/mL, zinc 2.93 μ g/mL.
Embodiment 2
The preparation of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect Ovum Anas domestica putamina, water ultrasonic cleaning 30 minutes, water cleans 3 times again, obtains clean egg shell, and is subsequent use;
B. sterilization
Step a gained eggshell is added the electrolyte that is equivalent to 3 times of eggshell volumes, sterilized 45 minutes, collect eggshell then, eggshell is dried under 80 ℃ of conditions, pulverize, get egg-shell meal, subsequent use; Wherein electrolyte is to be that sodium chloride and the electrolysis under the 220V condition of 0.01mol/L hydrochloric acid of 0.85mol/L made in 2 hours with concentration, and effective chlorine density is 1200ppm in the electrolyte that makes, and is diluted to effective chlorine density and is 80ppm, and is subsequent use.
C. acidolysis
In step b gained egg-shell meal, add the pH value be equivalent to 6 times of egg-shell meal quality and be 4 hydrochloric acid solution, do not stop stirring, acidolysis 2 hours; In reactant liquor, adding the concentration that is equivalent to 5 times of egg-shell meal weight again is the hydrochloric acid of 5mol/L; Do not stop to stir, acidolysis 2.5 hours is filtered; Collect filtrating, promptly get the eggshell hydrolyzate.
The eggshell hydrolyzate pH value that present embodiment makes is 6, and calcium, phosphorus, manganese, magnesium, zinc concentration are respectively calcium 14.29mg/ml in the eggshell hydrolyzate, phosphorus 0.075 mg/ml, manganese 0.37 μ g/ml, magnesium 35.48 μ g/ml, zinc 2.76 μ g/ml.
Embodiment 3
The preparation of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect goose egg-shell, water ultrasonic cleaning 30 minutes, water cleans 3 times again, obtains clean egg shell, and is subsequent use;
B. sterilization
Step a gained eggshell is added the electrolyte that is equivalent to 4 times of eggshell volumes, sterilized 10 minutes, collect eggshell then, eggshell is dried under 80 ℃ of conditions, pulverize, get egg-shell meal, subsequent use; Wherein electrolyte is to be that sodium chloride and the electrolysis under the 220V condition of 0.1mol/L hydrochloric acid of 0.085mol/L made in 2 hours with concentration, and effective chlorine density is 250ppm in the electrolyte that makes, and is subsequent use.
C. acidolysis
In step b gained egg-shell meal, add the pH value be equivalent to 8 times of egg-shell meal quality and be 3.5 hydrochloric acid solution, do not stop stirring, acidolysis 1 hour; In reactant liquor, adding the concentration that is equivalent to 3 times of egg-shell meal weight again is the hydrochloric acid of 8mol/L; Do not stop to stir, acidolysis 3 hours is filtered; Collect filtrating, promptly get the eggshell hydrolyzate.
The eggshell hydrolyzate pH value that present embodiment makes is 6, and calcium, phosphorus, manganese, magnesium, zinc concentration are respectively calcium 15.17mg/ml in the eggshell hydrolyzate, phosphorus 0.091 mg/ml, manganese 0.33 μ g/ml, magnesium 36.27 μ g/ml, zinc 2.51 μ g/ml.
Embodiment 4
The preparation of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect Ovum Anas domestica putamina, water ultrasonic cleaning 30 minutes, water cleans 3 times again, obtains clean egg shell, and is subsequent use;
B. sterilization
Step a gained eggshell is added the electrolyte that is equivalent to 2 times of eggshell volumes, sterilized 60 minutes, collect eggshell then, eggshell is dried under 60 ℃ of conditions, pulverize, get egg-shell meal, subsequent use; Wherein electrolyte is to be that sodium chloride and the electrolysis under the 220V condition of 0.025mol/L hydrochloric acid of 0.8mol/L made in 1.5 hours with concentration, and effective chlorine density is 1150ppm in the electrolyte that makes, and is diluted to effective chlorine density and is 80ppm, and is subsequent use;
C. acidolysis
In step b gained egg-shell meal, add the acetic acid that is equivalent to 1 times of egg-shell meal weight, do not stop to stir, acidolysis 2 hours, and then add the acetic acid that is equivalent to 2 times of egg-shell meal weight, acidolysis 5 hours is filtered, and collects filtrating, promptly gets the eggshell hydrolyzate.
The eggshell hydrolyzate pH value that present embodiment makes is 6, and calcium, phosphorus, manganese, magnesium, zinc concentration are respectively calcium 6.9mg/mL in the eggshell hydrolyzate, phosphorus 0.058mg/mL, manganese 0.16 μ g/mL, magnesium 13.23 μ g/mL, zinc 0.54 μ g/mL.
Embodiment 5
The preparation of eggshell hydrolyzate, concrete steps are following:
A. preliminary treatment
Collect Ovum Anas domestica putamina, water ultrasonic cleaning 25 minutes, water cleans 4 times again, obtains clean egg shell, and is subsequent use;
B. sterilization
Step a gained eggshell is added the electrolyte that is equivalent to 2 times of eggshell volumes, sterilized 60 minutes, collect eggshell then, eggshell is dried under 60 ℃ of conditions, pulverize, get egg-shell meal, subsequent use; Wherein electrolyte is to be that sodium chloride and the electrolysis under the 220V condition of 0.05mol/L hydrochloric acid of 0.2mol/L made in 1 hour with concentration, and effective chlorine density is 700ppm in the electrolyte that makes, and is subsequent use.
C. acidolysis
In step b gained egg-shell meal, add the acetic acid that is equivalent to 1.5 times of egg-shell meal weight, do not stop to stir, acidolysis 1 hour adds the acetic acid that is equivalent to 3 times of egg-shell meal weight again, does not stop to stir, and acidolysis 6 hours is filtered, and collects filtrating, promptly gets the eggshell hydrolyzate.
The eggshell hydrolyzate pH value that present embodiment makes is 6, and calcium, phosphorus, manganese, magnesium, zinc concentration are respectively calcium 7.2mg/mL in the eggshell hydrolyzate, phosphorus 0.032mg/mL, manganese 0.27 μ g/mL, magnesium 23.43 μ g/mL, zinc 1.58 μ g/mL.
Embodiment 6
The laying rate test
Cherry paddy egg duck to lay eggs more than 1 year is an experimental subjects, and Hechuan District Rong Xing agricultural cooperative society carries out egg duck field in the Chongqing City in test, and test period is that on August 6th, 2011 was to September 20; Wherein on August 6th, 2011 to August 20, the mass fraction of crude protein was 18.0% in the preparatory stage feeding feed stuff in order to raise the preparatory stage in advance in totally 15 days, and the mass fraction of crude fat is 1.5%; Coarse-fibred mass fraction is 8.0%; The mass fraction of coarse ash is 15%, and the mass fraction of calcium is 2.7%, and the mass fraction of phosphorus is 0.5%; The mass fraction of salt is 0.8%, and feed by 400g every every day.To test duck and be divided into two groups at random, 10 of every group of drakes, 50 of ducks.Wherein the A group is as control group, and feeding method is with raising the preparatory stage, and the B group is experimental group, and the method for feeding feed stuff is identical with the A group, and in addition every egg duck is drunk the eggshell hydrolyzate 50ml of embodiment 1 ~ 5 preparation every day.Measured the duck's egg index in the 7th day, the 14th day, the 21st day, the 28th day after record is fed, determination data adopts the single factor variance statistical analysis software of SPSS13.0 to handle, and makes multiple ratio with the LSD method, and data are represented with (mean+SD).Measure the influence of eggshell hydrolyzate to egg duck egg laying performance, the result is as shown in table 1:
Table 1. eggshell hydrolyzate is to the influence of egg duck production performance
| Group | Lay eggs sum (piece) | Laying rate (%) | Egg size (g) |
| The A group | 570 | 30.5±4.9A | 85.5±3.7 |
| The B group | 779 | 41.9±7.4B | 84.0±3.6 |
Annotate: different capitalizations are represented difference extremely significantly (p < 0.01)
Can know from table 1; Control group A group laying rate is 30.5 ± 4.9%, and after experimental group B group was added the eggshell hydrolyzate, laying rate was 41.9 ± 7.4%; Compare laying rate with control group and improved approximately 11.4%, the result shows that the eggshell hydrolysis fluid power of feeding significantly improves the egg laying performance of the later stage egg duck of laying eggs.
The eggshell quality of egg duck behind the determination experiment is studied the influence of eggshell hydrolyzate to the eggshell quality of egg duck respectively, and the result is as shown in table 2:
Table 2. eggshell hydrolyzate is to the influence of quality of egg
| Group | Shell thickness (mm) | Eggshell heavy (g) | Eggshell phase counterweight (%) | Eggshell strength (g/cm 2） |
| The A group | 0.33±0.03 | 8.6±0.7 | 9.9±0.5 | 4341.35±1295.62 |
| The B group | 0.34±0.03 | 8.5±0.5 | 9.7±0.2 | 4197.78±909.21 |
Can be known that by table 2 control group A group and experimental group B group is compared, shell thickness, eggshell weight, eggshell phase counterweight and eggshell strength difference are not remarkable, show behind the eggshell hydrolyzate of feeding less to shell thickness, eggshell weight, eggshell phase counterweight and eggshell strength influence.
The quality of egg duck's egg that duck produces behind the determination experiment is measured egg shape index, eggshell color, yolk colorimetric, egg yolk weight, albumen height and Hough unit's index of duck's egg respectively, and the result is as shown in table 3:
Table 3. eggshell hydrolyzate is to the influence of duck's egg quality
| Group | Egg shape index | The eggshell color | The yolk colorimetric | Egg yolk weight (g) | Albumen height (mm) | Hough unit |
| The A group | 1.45±0.08 | 39.7±3.08 | 6.87±1.22 | 30.66±4.21 | 6.23±1.31 | 68.35±10.99 |
| The B group | 1.40±0.06 | 38.67±3.34 | 6.87±0.69 | 31.02±2.95 | 6.14±1.28 | 66.82±13.37 |
Annotate: different capitalizations are represented difference extremely significantly (p < 0.01)
Can know that by table 3 the control group A group is compared with experimental group B group, index there was no significant differences such as egg shape index, eggshell color, yolk colorimetric, egg yolk weight, albumen height and Hough unit, so the interpolation of eggshell hydrolyzate can not influence other quality of duck's egg.
In sum; Utilize the eggshell hydrolyzate of method disclosed by the invention preparation can obviously improve the lay eggs egg laying performance in later stage of egg duck; And can not influence the quality of duck's egg and the quality of eggshell thereof, therefore can use as additive for a long time, the egg duck is had no side effect.Eggshell hydrolyzate disclosed by the invention not only is used to improve the laying rate of egg duck, can also be used for other poultry, like laying poultries such as chicken, geese.
Explanation is at last; Above embodiment is only unrestricted in order to technical scheme of the present invention to be described; Although through invention has been described with reference to the preferred embodiments of the present invention; But those of ordinary skill in the art should be appreciated that and can make various changes to it in form with on the details, and the spirit and scope of the present invention that do not depart from appended claims and limited.
Claims (10)
1. the preparation method of eggshell hydrolyzate is characterized in that, concrete steps are following:
A. preliminary treatment
Collect eggshell, the eggshell of collecting is cleaned, obtain clean egg shell, subsequent use;
B. sterilization
With carrying out disinfection in the electrolyte of step a gained eggshell adding by sodium chloride and hydrochloric acid mixed solution preparation, collect eggshell, oven dry is pulverized, and gets egg-shell meal, and is subsequent use;
C. acidolysis
Step b gained egg-shell meal is added the pH value be not less than 3 hydrochloric acid, acidolysis at least 1.5 hours; Add concentration again and be not less than the hydrochloric acid of 5mol/L, acidolysis at least 2 hours, the eggshell hydrolyzate;
Or be equivalent to egg-shell meal weight 1-1.5 acetic acid doubly with adding in the step b gained egg-shell meal, acidolysis 1-2 hour, add again and be equivalent to egg-shell meal weight 2-3 acetic acid doubly, acidolysis at least 5 hours.
2. preparation method according to claim 1 is characterized in that: said step a is with the eggshell water ultrasonic cleaning of collecting 20-30 minute, and water cleans 3-5 time again.
3. preparation method according to claim 1 is characterized in that: said step b adds to be equivalent to eggshell volume 2-5 electrolyte doubly, sterilizes 10-60 minute.
4. preparation method according to claim 3 is characterized in that: among the said step b, the available chlorine content of said electrolyte is for being not less than 80ppm.
5. preparation method according to claim 4; It is characterized in that: the preparation method of electrolyte that said available chlorine content is not less than 80ppm does; With sodium chloride concentration is that 0.085-0.85mol/L, concentration of hydrochloric acid are the mixed solution of 0.01-0.1mol/L, under the 220V voltage conditions, makes in electrolysis 1-2 hour.
6. preparation method according to claim 5; It is characterized in that: the preparation method of electrolyte that said available chlorine content is not less than 80ppm does; With sodium chloride concentration is that 0.5mol/L, concentration of hydrochloric acid are the mixed solution of 0.05mol/L, and electrolysis made in 1 hour under the 220V voltage conditions.
7. preparation method according to claim 1 is characterized in that: said step c adds step b gained egg-shell meal to be equivalent to the hydrochloric acid of egg-shell meal weight 6-8 pH value doubly for 3-4, acidolysis 1-2 hour; Adding and being equivalent to egg-shell meal weight 0.5-5 concentration doubly is the hydrochloric acid of 5-10mol/L, acidolysis 2-3 hour.
8. the eggshell hydrolyzate that makes of the preparation method of each said eggshell hydrolyzate of claim 1-7.
9. the application of the said eggshell hydrolyzate of claim 8 in improving the poultry laying rate.
10. application according to claim 9 is characterized in that: said poultry is a duck.
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| CN103302081A (en) * | 2013-06-27 | 2013-09-18 | 北京二商健力食品科技有限公司 | Preparation method of eggshell powder and processing device |
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| CN103316896A (en) * | 2013-06-27 | 2013-09-25 | 北京二商健力食品科技有限公司 | Processing method of eggshell powder |
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| CN103302081B (en) * | 2013-06-27 | 2016-01-27 | 北京二商健力食品科技有限公司 | A kind of preparation method of egg-shell meal and process equipment |
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| CN104824711A (en) * | 2015-05-21 | 2015-08-12 | 贵州梦润鹌鹑有限公司 | Preparation method of quail egg nutrition powder |
| CN106935415A (en) * | 2017-05-03 | 2017-07-07 | 王馨瑜 | The method for improving specific capacity of double-layer capacitor |
| CN115215363A (en) * | 2022-05-25 | 2022-10-21 | 华中农业大学 | Method for efficiently preparing eggshell source fine calcium carbonate and application thereof |
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