CN102442871A - Preparation method of composite calcium amino acid chelate by hems of shells and scallops as raw materials - Google Patents
Preparation method of composite calcium amino acid chelate by hems of shells and scallops as raw materials Download PDFInfo
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- CN102442871A CN102442871A CN2010105121023A CN201010512102A CN102442871A CN 102442871 A CN102442871 A CN 102442871A CN 2010105121023 A CN2010105121023 A CN 2010105121023A CN 201010512102 A CN201010512102 A CN 201010512102A CN 102442871 A CN102442871 A CN 102442871A
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Abstract
The invention relates to a preparation method of composite calcium amino acid chelate by hems of shells and scallops as raw materials, comprising the steps of using 0.05 M of hydrochloric acid to soak shells, drying and crushing the shells, treating the shells powder by water-refining method, obtaining calcium-based shell powder; using neutral protease, papain and acid protease to perform enzymolysis for hems of fresh scallops, obtaining composite amino acid solution; mixing the composite amino acid and the shell powder according to the mol ratio of 2: (1.0-1.2) (based on 92% of calcium content in the calcium carbonate; performing chelating in a gradient manner at pH of 5, pH of 8 and pH of 11 in turn; maintaining the temperature for 2 h under every pH gradient; condensing the mixture solution to be paste, adding absolute ethyl alcohol to precipitate; performing low-temperature re-crystallizing and drying by absolute ethyl alcohol, and obtaining composite calcium amino acid chelate. The method is simple and convenient and can process wastes such as hems of shells and scallops in a high value manner.
Description
Technical field:
The present invention relates to a kind of shellfish processing waste (oyster shells, scallop shell etc.) that utilizes and be the calcium source; With the scallop body is the compounded amino acid source; Through high-valued, clean process step, realize the process method that compound amino acid chelate calcium is produced in the shellfish processing waste comprehensive utilization.
Background technology:
The raising of calcium contents is to solve one of main path of calcium deficiency problem in the food.
At present, widely used calcium-supplementing preparation majority is a calcium salt in the food, like calcium phosphate, lime carbonate, calglucon, calcium acetate, lactic acid ca etc., but shortcoming such as the ubiquity specific absorption is low.And calcium amino acid chelate because of be easy to absorb, toxicity is little more and more receives extensive attention.
In recent years, kind, the quantity of China's sea farming are advanced by leaps and bounds, wherein, sea farming output be shellfish more than 75%.Show that according to Food and Agricultural Organization of the United Nations's report China's shellfish culture industry size and output occupied first place in the world in continuous 18 years.And a large amount of waste oyster shellss, scallop shell, scallop body that shellfish processing produces still remain high-valued Application and Development.The present invention is conceived to the higher value application of shellfish processing waste, utilizes shell to make compound amino acid source as calcium source, scallop body and prepares the high purity compound amino acid chelate calcium, turns waste into wealth, and is also significant to the protection environment simultaneously.
Summary of the invention:
The object of the present invention is to provide a kind of is calcium source, scallop body are produced compound amino acid chelate calcium for the compounded amino acid source novel method with the shell.
To achieve these goals, main process of the present invention comprises shell pre-treatment, scallop body enzymolysis, synthetic, refining, the stoving process step of compound amino acid chelate calcium, wherein:
Shell pre-treatment: shell is scrubbed adsorptives such as removing shell surface silt with 0.05M salt soak after 1 hour, through 100 ℃ of oven dry, pulverized 60 mesh sieves, promptly get through the processing of tap water flying method again and synthesize compound amino acid chelate calcium with calcium source oyster shell whiting;
The scallop body enzymolysis: the fresh scallops shirt rim adds same weight tap water, is heated to 50 ℃, transfers pH6.5, adds to account for fresh scallops shirt rim weight 0.5 ‰ mixed enzyme (neutral protease: papoid=1: 1, w: w) enzymolysis 5h; Enzymolysis solution adds the aspartic protease enzymolysis 5.5h that accounts for fresh scallops shirt rim weight 0.5 ‰ again under 45 ℃, pH2.5 condition after inactivation treatment.Enzymolysis solution through deactivation, centrifugal, is discarded insolubles and obtains compositing acid solution, and wherein the mole number of aminoacids complex is obtained with FTM;
Synthetic: as earlier oyster shell whiting (calcium carbonate content is in 92%) to be added hydrochloric acid according to stoichiometric relation and be converted into calcium chloride; Be 2: 1.0～1.2 adding scallop body compositing acid solutions by aminoacids complex and calcium chloride mol ratio again, stir and be heated to 70～75 ℃.Adopt pH gradient adjusting method to carry out chelatropic reaction.PH5, pH8 and pH11 totally 3 pH gradients are set sequentially; Under each pH gradient, be incubated chelatropic reaction 2h; Altogether after the chelatropic reaction 6h, add the absolute ethyl alcohol deposition after mixture solution is concentrated into paste, promptly get the compound amino acid chelate calcium bullion through suction filtration again;
Refining: as above-mentioned gained bullion to be added the less water dissolving, add absolute ethyl alcohol again, stir stand at low temperature recrystallization, suction filtration;
Oven dry: the vacuum-drying of above-mentioned gained recrystallization is promptly got the compound amino acid chelate calcium product.
The present invention compared with prior art; Its technological process is simple, and shell need not calcining, and building-up process only depends on conditioned reaction liquid pH gradient; Can make that the calcareous chelating of aminoacids complex more than 92% and shell source is converted into compound amino acid chelate calcium in the scallop body enzymolysis solution; Products obtained therefrom quality good (faint yellow, easy to be molten, chelation percent is up to more than 95%).
Embodiment:
Through instance the present invention is done further elaboration below:
Instance 1: 1.2 kilograms of oyster shellss are soaked in the 0.05M hydrochloric acid soln scrub adsorptives such as removing shell surface silt after 1 hour; Through 100 ℃ of oven dry, pulverized 60 mesh sieves; Handle promptly to get through the tap water flying method again and synthesize compound amino acid chelate calcium, add hydrochloric acid according to stoichiometric relation and be converted into 1 liter in 9.2M calcium chloride with 1 kilogram of calcium source oyster shell whiting; 1 kilogram of fresh scallops shirt rim adds the homogenate of same weight tap water, is heated to 50 ℃, transfers pH6.5, adds each 0.25 gram enzymolysis 5h of neutral protease and papoid; Enzymolysis solution adds 0.5 gram aspartic protease enzymolysis 5.5h again under 45 ℃, pH2.5 condition after inactivation treatment.Enzymolysis solution through deactivation, centrifugal, is discarded insolubles and obtains compositing acid solution.The above-mentioned calcium chloride solution that obtains is mixed, stirs with compositing acid solution and is heated to 70 ℃; Reaction solution pH5, pH8 and pH11 totally 3 pH gradients are set sequentially; Under each pH gradient, be incubated chelatropic reaction 2h; Altogether after the chelatropic reaction 6h, mixture solution is concentrated into adds 3 liters of absolute ethyl alcohols behind the paste and make the product deposition, suction filtration promptly gets the compound amino acid chelate calcium bullion;
Purifying: above-mentioned bullion is added the less water dissolving, add 3 liters of absolute ethyl alcohols again, stir, leave standstill 3 hours recrystallizations, suction filtration in 4 ℃;
Oven dry:, promptly get about 1.8 kilograms of compound amino acid chelate calcium product with above-mentioned gained recrystallization vacuum-drying 6 hours.
Instance 2: step and method are with instance 1, and raw material is chosen scallop shell or CONCHA MERETRICID SEU CYCLINAE, and the quality of its preparation compound amino acid chelate calcium product is identical with the oyster shells raw material.
Claims (5)
1. main process of the present invention comprises shell pre-treatment, scallop body enzymolysis, synthetic, refining, the stoving process step of compound amino acid chelate calcium; Wherein: oyster shell whiting (calcium carbonate content is in 92%) is added hydrochloric acid according to stoichiometric relation be converted into calcium chloride; Be 2: 1.0～1.2 adding scallop body compositing acid solutions by aminoacids complex and calcium chloride mol ratio again, stir and be heated to 70～75 ℃.Adopt pH gradient adjusting method to carry out chelatropic reaction.PH5, pH8 and pH11 totally 3 pH gradients are set sequentially; Under each pH gradient, be incubated chelatropic reaction 2h; Altogether after the chelatropic reaction 6h, add the absolute ethyl alcohol deposition after mixture solution is concentrated into paste, promptly get the compound amino acid chelate calcium bullion through suction filtration again; Above-mentioned gained bullion is added the less water dissolving, add absolute ethyl alcohol again, stir stand at low temperature recrystallization, suction filtration; The vacuum-drying of above-mentioned gained recrystallization is promptly got the compound amino acid chelate calcium product.
2. as claimed in claim 1 is the preparation method of the compound amino acid chelate calcium of raw material with shell and scallop body, it is characterized in that the calcareous chelating of aminoacids complex and shell adopts pH gradient chelating method;
3. as claimed in claim 1 is the preparation method of the compound amino acid chelate calcium of raw material with shell and scallop body, it is characterized in that the separation of compound amino acid chelate calcium, refining employing absolute ethyl alcohol are precipitation agent;
4. as claimed in claim 1 is the preparation method of the compound amino acid chelate calcium of raw material with shell and scallop body, it is characterized in that the preparation of compound amino acid chelate calcium makes full use of shellfish processing waste-scallop body and shell;
5. as claimed in claim 1 is the preparation method of the compound amino acid chelate calcium of raw material with shell and scallop body, it is characterized in that its calcareous source shell comprises shellfish processing wastes such as oyster shells, scallop shell, CONCHA MERETRICID SEU CYCLINAE.
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Cited By (8)
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| CN103710403A (en) * | 2013-12-09 | 2014-04-09 | 广东环西生物科技股份有限公司 | Efficient cleaning production process of compound amino acid chelated calcium |
| CN104905256A (en) * | 2015-05-21 | 2015-09-16 | 北海富安源生物科技有限公司 | Composite amino acid chelated calcium prepared by using oysters as raw materials |
| CN105433300A (en) * | 2015-12-29 | 2016-03-30 | 广西钦州市绿源天然食品加工有限公司 | Processing method for producing active calcium from oyster shells |
| CN105567775A (en) * | 2016-03-03 | 2016-05-11 | 集美大学 | Production method of fish collagen peptide chelated calcium |
| CN108477619A (en) * | 2018-03-16 | 2018-09-04 | 青岛大学 | A kind of preparation method of compound amino acid chelate calcium |
| CN110256267A (en) * | 2019-07-08 | 2019-09-20 | 中国海洋大学 | It is a kind of to chelate calcium preparation method by the L-Aspartic acid of calcium source of Pacific Ocean oyster shell |
| CN114190469A (en) * | 2021-12-27 | 2022-03-18 | 南通励成生物工程有限公司 | Hydrolyzed whey protein composite amino acid chelate as well as preparation method and application thereof |
| CN117586067A (en) * | 2023-12-07 | 2024-02-23 | 峨眉山市龙腾生物科技有限公司 | Amino acid chelated organic fertilizer and production process thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104905256A (en) * | 2015-05-21 | 2015-09-16 | 北海富安源生物科技有限公司 | Composite amino acid chelated calcium prepared by using oysters as raw materials |
| CN105433300A (en) * | 2015-12-29 | 2016-03-30 | 广西钦州市绿源天然食品加工有限公司 | Processing method for producing active calcium from oyster shells |
| CN105567775A (en) * | 2016-03-03 | 2016-05-11 | 集美大学 | Production method of fish collagen peptide chelated calcium |
| CN108477619A (en) * | 2018-03-16 | 2018-09-04 | 青岛大学 | A kind of preparation method of compound amino acid chelate calcium |
| CN110256267A (en) * | 2019-07-08 | 2019-09-20 | 中国海洋大学 | It is a kind of to chelate calcium preparation method by the L-Aspartic acid of calcium source of Pacific Ocean oyster shell |
| CN114190469A (en) * | 2021-12-27 | 2022-03-18 | 南通励成生物工程有限公司 | Hydrolyzed whey protein composite amino acid chelate as well as preparation method and application thereof |
| CN114190469B (en) * | 2021-12-27 | 2024-03-15 | 南通励成生物工程有限公司 | Hydrolyzed whey protein composite amino acid chelate as well as preparation method and application thereof |
| CN117586067A (en) * | 2023-12-07 | 2024-02-23 | 峨眉山市龙腾生物科技有限公司 | Amino acid chelated organic fertilizer and production process thereof |
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Application publication date: 20120509 |