CN102731614A - Collagen tripeptide chelated calcium and its preparation method - Google Patents
Collagen tripeptide chelated calcium and its preparation method Download PDFInfo
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Abstract
Relating to health food and preparation methods, the invention provides collagen tripeptide chelated calcium and its preparation method. The collagen tripeptide chelated calcium is a product obtained by mixing of calcium hydroxide and collagen tripeptide in a weight ratio of 7:0.5-7:4, deodorization treatment, vacuum filtration, concentration, and drying. The preparation method comprises the following steps of: (1) adding equivalent collagen tripeptide in twice into calcium hydroxide and mixing them uniformly, keeping the materials and a liquid in a weight ratio of 6:10-6:400, controlling the temperature of the process at 40DEG C-100DEG C and the reaction time at 90 minutes; (2) conducting vacuum filtration and deodorization treatment to the mixed solution, and collecting the filtrate for concentration; and (3) carrying out drying so as to obtain the product. With the invention, the chelating ability of collagen tripeptide and calcium is substantially enhanced. The preparation process of collagen tripeptide chelated calcium of the invention simplifies equipment, shortens the preparation time, and simplifies the process, thus saving manpower, material resources and time, and reducing the production cost.
Description
Technical field
The present invention relates to protective foods and preparation method, particularly relate to the method for a kind of collagen tripeptide chelating calcium and preparation thereof.
Background technology
Calcium is one of maximum mineral element of people's in-vivo content, also is one of most active element in the body.Calcium has multiple important physical function; Participate in the normal function of the histoorgan of each system of conciliation; And in body, play an important role with multiple histocyte, biomacromolecule level; Calcium is to keep the normal excited necessary composition of N&M, also is to guarantee bone growth and keep the necessary material of sclerotin hardness.Yet calcium deficiency belongs to global health problem, and especially in special populations such as the elderly, children, women, even in Japan and many wests industrialized country, calcium deficiency is ubiquity too.Implement planned replenishing the calcium, body constitution and the health level that improves the crowd is had very important significance.
Exist a feast for the eyesly at present on the market, miscellaneous product of replenishing the calcium, first-generation calcium-supplementing preparation are inorganic calciums such as lime carbonate; It is higher to contain calcium concn; But solvability is relatively poor, need consume hydrochloric acid in gastric juice in the intravital absorption of machine, and needs the interior involved enzyme of consumption human body and make carrier through VITAMINs just can be absorbed; So specific absorption is low, this type calsium supplement can increase the burden of kidney simultaneously.Second on behalf of organic calcium, is calcium ion, but the inhalation effects factor is many, and spinoff is big, mainly has the low and toxicity problem in various degree of calcium contents.The third generation is a calcium amino acid chelate; The whole molecule of calcium and organic group thereof complete by intestinal absorption; It is stable to have chemical property, and the biological value advantages of higher the more important thing is VITAMINs; The influence of unsaturated fatty acids isoreactivity composition is less, can reduce the antagonism with other trace element and major element in vivo.Wherein small-peptide chelated calcium is identical with the normal physiological calcium absorption, more is prone to absorb than calcium amino acid chelate.
At present, calcium amino acid chelate needs absolute ethyl alcohol deposition and recrystallizing technology to carry out the purifying of calcium amino acid chelate in process of production, and man-hour is long, and cost is high.Small-peptide chelated calcium prepares often selects for use calcium chloride as the calcium source in the process, need the artificial pH of adjusting value, introduces non-active ingredients, and for improving purity, must separate chelating calcium and ionized calcium, complex process by alcohol precipitation.
Collagen tripeptide is called for short CTP (Collagen tripeptide), by the small-molecular peptides of molecular weight about 200～500Dalt that three amino acid are formed, the about 280Dalt of molecular-weight average.Research shows: tripeptides need not to decompose and can be absorbed by the body, because the interaction between its three amino acid compositions makes it have the activity stronger than single amino acids; Collagen tripeptide can infiltrate in keratoderma, epidermal area, skin corium and the hair/hair follicle, have promote that collagen and mucinase are synthetic, inhibition melanochrome generates, preserve moisture, multiple functions such as slim, skin moisten, preventing osteoporosis.
Collagen mainly is from animal tissuess such as ox and pig, to extract for a long time.The people that make of mad cow disease and foot and mouth disease begin to consider to use the substitute of ox, pig collagen in recent years.To be that the collagen tripeptide of feedstock production has safe, the cell agglutinating value(of coal) is good, transparent, odorless and characteristics such as non-stimulated with free of contamination fish-skin.
Chinese patent number be 200910151023.1 and the patent No. be 200910063282.9 to disclose the method for preparing calcium amino acid chelate respectively, but aforesaid method exists shortcoming to be: need absolute ethyl alcohol deposition and recrystallizing technology, production unit is complicated, and preparation time is long.Chinese patent numbers 200610036501.0 discloses glutathione calcium chelate preparation technology, in the preparation process, needs the artificial pH of adjusting; Need alcohol precipitation to separate chelating calcium and ionized calcium.
At present, the research to collagen both at home and abroad obtains very big progress, but the someone proposes collagen tripeptide is combined with calcium-supplementing preparation to produce a kind of thinking and method of high efficiency calcium-enriching preparation of brand-new biologically active as yet.
Summary of the invention
The purpose of this invention is to provide a kind of collagen tripeptide chelating calcium and preparation method thereof; The high efficiency calcium-enriching preparation that the present invention provides a kind of collagen tripeptide to combine to produce a kind of brand-new biologically active with calcium-supplementing preparation, the present invention also provides a kind of preparation technology of high-efficient calcium replenishing agent of brand-new biologically active.
A kind of collagen tripeptide chelating calcium of the present invention, with calcium hydroxide and collagen tripeptide with 7: 0.5～7: 4 proportionings of weight ratio, through mix, take off flavor processing, vacuum filtration, concentrate, dry made product.
The chelated calcium preparation method of a kind of collagen tripeptide of the present invention, operate according to following steps:
(1) be raw material with calcium hydroxide and collagen tripeptide, the weight ratio of collagen tripeptide and calcium hydroxide is 7: 0.5～7: 4, and collagen tripeptide equivalent adding at twice mixes mixing with calcium hydroxide; With water is liquid, and above-mentioned raw materials adds in the liquid, and the feed liquid weight ratio is 6: 10～6: 400; The said process controlled temperature is at 40 ℃～100 ℃, and the reaction times is 90 minutes;
(2) above-mentioned mixed solution is carried out vacuum filtration, the suction filtration condition is 0.04MPa; Collect filtrating, under 40 ℃ of temperature, water-bath 30 minutes is taken off flavor and is handled with 30% gac; To take off the filtrating of flavor processing then and carry out vacuum filtration, the suction filtration condition is 0.04Mpa; Collect filtrating concentrating;
(3) above-mentioned liquid concentrator is carried out drying, obtain product.
In the vacuum concentration condition described in (two) step is 40 ℃～50 ℃.
Can be vacuum-drying or spraying drying in drying described in (three) step.
The collagen tripeptide chelating calcium that designed of invention be with small molecules fish skin collagen tripeptides and calcium hydroxide under given conditions chelating form.
The present invention and the patent No. be 200910151023.1 and the patent No. be 200910063282.9 prepare calcium amino acid chelate method compare, maximum difference do not need to be absolute ethyl alcohol deposition and recrystallizing technology, has simplified corresponding production unit, has shortened preparation time.The present invention compares with the patent No. 200610036501.0 glutathione calcium chelate preparation technologies and existing peptide chelating calcium preparation technology, selects calcium hydroxide to prepare collagen tripeptide chelating calcium as the calcium source, in the preparation process, need not artificially to regulate pH; Need not alcohol precipitation and separate chelating calcium and ionized calcium; Equivalent adds collagen tripeptide at twice, makes collagen tripeptide and calcium sequestration capacity promote greatly.Collagen tripeptide chelating calcium preparation technology of the present invention has simplified equipment, shortens preparation time, has saved human and material resources and time thereby simplify technology, reduces preparation cost.
Description of drawings
Fig. 1 is the impact effect synoptic diagram of collagen tripeptide chelating calcium to the mouse femur calcium contents.
Annotate: * representes relatively have the significance of difference with blank control group, P＜0.05 among the figure
* * representes relatively have difference utmost point significance, P＜0.01 with blank control group among the figure
Embodiment
With illustrated embodiments the present invention is done detailed explanation below.
Embodiment 1:
Is to mix at 7: 2 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 40, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 5.75% in the collagen tripeptide chelating calcium at this moment.
Calcium described in all embodiment is calcium hydroxide.
Embodiment 2:
Is to mix at 7: 2 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 120, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 6.48% in the collagen tripeptide chelating calcium at this moment.
Embodiment 3:
Is to mix at 7: 2 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 400, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 9.34% in the collagen tripeptide chelating calcium at this moment.
Embodiment 4:
Is to mix at 7: 3 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 40, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 6.40% in the collagen tripeptide chelating calcium at this moment.
Embodiment 5:
Is to mix at 7: 3 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 120, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 7.70% in the collagen tripeptide chelating calcium at this moment.
Embodiment 6:
Is to mix at 7: 3 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 400, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 13.00% in the collagen tripeptide chelating calcium at this moment.
Embodiment 7:
Is to mix at 7: 4 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 40, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 5.98% in the collagen tripeptide chelating calcium at this moment.
Embodiment 8:
Is to mix at 7: 4 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 120, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 7.75% in the collagen tripeptide chelating calcium at this moment.
Embodiment 9:
Is to mix at 7: 4 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 400, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 13.27% in the collagen tripeptide chelating calcium at this moment.
Embodiment 10:
Is to mix at 7: 3 collagen tripeptide and calcium according to mass ratio, and solid-liquid ratio is 6: 400, and controlled temperature is 60 ℃, and the reaction times is 90min.Fully after the reaction, control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and adding 30% is that 4% sodium hydroxide solution and concentration are 4% hydrochloric acid soln activated particles gac through concentration, in 40 ℃, and water-bath 30min.Control pressure is that 0.04MPa carries out vacuum filtration, collects filtrating, and vacuum concentration places 70 ℃ with liquid concentrator, and vacuum-drying 1～2h promptly obtains collagen tripeptide chelating calcium.Calcium contents is 14.42% in the collagen tripeptide chelating calcium at this moment.
Collagen tripeptide chelating calcium of the present invention according to " protective foods function assessment assessment process and method of inspection standard ", is laboratory animal with the kunming mice; Male and female half and half adopt the maximum stomach amount method (MTD) of irritating to experimentize, and dosage is designed to 10.0g/kg.bw; Irritate stomach 3 times in 24 hours, observed for two weeks continuously.Mouse does not all have death, and body weight increases to some extent, compares there was no significant difference with the blank group.So the true border of collagen tripeptide chelating calcium of the present invention is nontoxic.
Collagen tripeptide chelating calcium of the present invention is a kind of stable water-soluble calcium inner complex, belongs to little peptide binding substances, and specific absorption is high, and the form with small-peptide chelated calcium in small intestine absorbs, avoid with food in oxalic acid, phytic acid etc. combine and influence absorption.Collagen tripeptide chelating calcium is absorbed by transhipment in human body; Supplement calcium and collagen nutrition; And collagen tripeptide also can be brought into play distinctive biological activity in vivo; Make the product of the present invention can high efficiency calcium-enriching, can bring into play the distinctive physiological function of collagen tripeptide again simultaneously, can be used as protective foods and additive etc. and be widely used in and produce and live.
Weaning 20 days, 12～15g, kunming mice is an animal subject, is divided into the normal control group; Model group, experimental group is removed the normal control group conventional feed of feeding, all the other each groups low calcium feed of all feeding; To cause the calcium deficiency model, normal control group, model group are comforted with filling stomach zero(ppm) water and are handled; Experimental group is irritated stomach collagen tripeptide chelating calcium 2.4mg/g, and display model group femur calcium contents is starkly lower than the normal control group and has the significance of difference as a result, shows the modeling success.Experimental group femur calcium contents is higher than model group and normal control group, carries out statistical study with the normal control group, and its result shows that difference has utmost point significance.Specifically see accompanying drawing 1.The femur calcium contents is high, explain that collagen tripeptide chelating calcium not only is prone to absorb, and the calcium utilization that absorbs is higher, can be deposited on the bone, makes bone strong.Normal control group in the experimentation, model group, experimental group do not have the significance of difference aspect body weight.It is thus clear that the effect that collagen tripeptide chelating calcium of the present invention has tangible supplement calcium.
Select 50～70 years old, get rid of and take oestrogenic hormon above 154 of the women more than 10 years climacteric; Steroid hormone, anticonvulsant drug, thiazine hydragog(ue) or other influence the people of the medicine of calcium metabolism; 127 experimenters get into data statistics; Be divided into control group and intervention group, intervention group is taken 1.2g collagen tripeptide chelating calcium every day, and control group is taken placebo.The DPX-L type dual intensity X line borne densitometers that adopts U.S. GE Lunar company to produce is measured the 1st～4 lumbar spine bmd, and through the tracing observation in 1 year, the result was as shown in table 1.Intervention group is close with the control group bone density before the research, finds that through the follow-up study in 1 year its lumbar spine bmd of menopausal women of taking collagen tripeptide chelating calcium group every day will be apparently higher than the lumbar spine bmd of the control group menopausal women of taking placebo.This research experimenter be climacteric the women more than 10 years as research object; Because its body inner estrogen level obviously descends; Calcium content of bone runs off more obvious; With collagen tripeptide chelating calcium it is intervened, its bone density loss degree is starkly lower than control group after 1 year, compares with control group to have the significance of difference.It is thus clear that the effect that collagen tripeptide chelating calcium of the present invention has supplement calcium.
Table 1127 experimenter's lumbar spine bmd (BMD) is followed the tracks of detected result
Above embodiment is more preferably embodiment a kind of of the present invention, and common variation that those skilled in the art carry out in present technique scheme scope and replacement should be included in protection scope of the present invention.
Claims (4)
1. a collagen tripeptide chelating calcium is characterized in that, with calcium hydroxide and collagen tripeptide with 7: 0.5～7: 4 proportionings of weight ratio, through mix, take off flavor processing, vacuum filtration, concentrate, dry made product.
2. the chelated calcium preparation method of collagen tripeptide is characterized in that, operates according to following steps:
(1) be raw material with calcium hydroxide and collagen tripeptide, the weight ratio of collagen tripeptide and calcium hydroxide is 7: 0.5～7: 4, and collagen tripeptide equivalent adding at twice mixes mixing with calcium hydroxide; With water is liquid, and above-mentioned raw materials adds in the liquid, and the feed liquid weight ratio is 6: 10～6: 400; The said process controlled temperature is at 40 ℃～100 ℃, and the reaction times is 90 minutes;
(2) above-mentioned mixed solution is carried out vacuum filtration, the suction filtration condition is 0.04MPa; Collect filtrating, under 40 ℃ of temperature, water-bath 30 minutes is taken off flavor and is handled with 30% gac; To take off the filtrating of flavor processing then and carry out vacuum filtration, the suction filtration condition is 0.04Mpa; Collect filtrating concentrating;
(3) above-mentioned liquid concentrator is carried out drying, obtain product.
3. the chelated calcium preparation method of a kind of according to claim 1 collagen tripeptide is characterized in that, is 40 ℃～50 ℃ in the vacuum concentration condition described in (two) step.
4. the chelated calcium preparation method of a kind of according to claim 1 collagen tripeptide is characterized in that, can be vacuum-drying or spraying drying in drying described in (three) step.
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Cited By (3)
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| CN107712910A (en) * | 2017-09-22 | 2018-02-23 | 西安交通大学 | A kind of gelatin small peptide or collagen tripeptide chelating calcium and magnesium and preparation method thereof |
| CN111990649A (en) * | 2020-08-13 | 2020-11-27 | 自然资源部第三海洋研究所 | Preparation method of water-soluble melanin chelated calcium salt of squid |
| CN117946207A (en) * | 2024-03-26 | 2024-04-30 | 北京青颜博识健康管理有限公司 | Mineral-containing high-purity collagen tripeptide and preparation method thereof |
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| CN107712910A (en) * | 2017-09-22 | 2018-02-23 | 西安交通大学 | A kind of gelatin small peptide or collagen tripeptide chelating calcium and magnesium and preparation method thereof |
| CN111990649A (en) * | 2020-08-13 | 2020-11-27 | 自然资源部第三海洋研究所 | Preparation method of water-soluble melanin chelated calcium salt of squid |
| CN117946207A (en) * | 2024-03-26 | 2024-04-30 | 北京青颜博识健康管理有限公司 | Mineral-containing high-purity collagen tripeptide and preparation method thereof |
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