CN102178228A - Collagen-calcium chelate and preparation method thereof - Google Patents
Collagen-calcium chelate and preparation method thereof Download PDFInfo
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- CN102178228A CN102178228A CN2011100960765A CN201110096076A CN102178228A CN 102178228 A CN102178228 A CN 102178228A CN 2011100960765 A CN2011100960765 A CN 2011100960765A CN 201110096076 A CN201110096076 A CN 201110096076A CN 102178228 A CN102178228 A CN 102178228A
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Abstract
The invention relates to a collagen-calcium chelate and a preparation method thereof. In traditional calcium preparations, the calcium preparation mainly including inorganic salts and organic salts has low absorption and utilization rates; the amino acid chelated calcium can not supplement collagen and calcium simultaneously; the collagen chelated calcium mainly comprises acid soluble collagen from animal cartilage or skin tissue, and the application of the heterogeneous and xenogenous collagen in human bodies has the risks of high infection rate and high rejection rate. The collagen-calcium chelate provided by the invention is a functional food manufactured by combining calcium elementa with collagen and is prepared from animal-based collagen or humanlike collagen and soluble calcium salts as raw materials through the water system synthesis method. The collagen-calcium chelate has the advantages of good stability and high biological value and can be directly absorbed by the intestinal mucosa to actually realize high absorption, calcium is deposited in the bones under the adhesion of collagen, and the purpose of enhancing the flexibility and the hardness of the bones is finally achieved.
Description
Technical field
The present invention relates to a kind of collagen-calcium chelate and preparation method thereof.
Background technology
Calcium is one of maximum mineral element of people's in-vivo content, and the total amount in human body reaches 1300g, is about the 1.5-2.0% of body weight, and wherein 99% is present in bone and the tooth.Calcium in bone in the mode of hydroxyapatite deposition, be that adhesive is fixed up with the ossein.Not having ossein just not to be called bone in the bone, is the accumulation of many hydroxyapatite molecules and particle; Not having ossein enough and that carrying out eubolism in the bone, will be not hard and unsound.Therefore, prevent and improve osteoporosis, scientific methods is supplement calcium and collagen simultaneously.Like this, calcium could be in the bonding deposit of collagen in bone, thereby strengthens the toughness and the hardness of bone.
Following three developing stage have been gone through in the development of calcium preparation: first generation product is based on inorganic salts, as animal fresh bone, shell, calcium carbonate mineral etc.; Second generation product is based on traditional organic salt, as calcium lactate, calcium acetate, calcium gluconae etc.More than two series products all have the low defective of absorption rate, and have antagonism between the mineral element, therefore can not fully satisfy the needs of body.Third generation product amino acid chelated calcium has also obtained exploitation to a certain degree as a kind of good calcium-supplementing preparation, though overcome the shortcoming of inorganic calcium and organic calcium, it also can not accomplish that collagen and calcium are with mending.
Summary of the invention
The purpose of this invention is to provide a kind of collagen-calcium chelate and preparation method thereof, make novel functional food closely-related with health, that calcium constituent and collagen are combined.
The technical solution adopted in the present invention is:
A kind of preparation method of collagen-calcium chelate is characterized in that: realized by following steps:
Step 1: with collagen and soluble calcium salt is raw material, the mass ratio of collagen and soluble calcium salt is 10:1～4, reaction temperature is 20～50 ℃, react 1.5～5h under stirring condition, the alkali lye that adds molar concentration simultaneously and be 0.5～2mol/L is 4.0～5.5 with the pH value of control reactant liquor;
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Collagen described in the step 1 is animal sources collagen or human-like collagen.
Soluble calcium salt described in the step 1 is calcium chloride or calcium acetate.
Alkali lye described in the step 1 is sodium hydroxide solution, potassium hydroxide solution or barium hydroxide solution.
Collagen-calcium chelate that a kind of preparation method as claimed in claim 1 makes.The present invention has the following advantages:
A kind of collagen-calcium chelate involved in the present invention is that calcium constituent and collagen are combined the functional food of making, with animal sources collagen or human-like collagen and soluble calcium salt is raw material, adopt the aqueous systems synthetic method to make, thereby have and have good stability, the biological value height, can be directly be absorbed the real high advantage that absorbs that realizes by intestinal mucosa, and make calcium in the bonding deposit of collagen in bone, finally reach the toughness that strengthens bone and the purpose of hardness.
Description of drawings
Fig. 1 is the ultraviolet spectrogram of collagen-calcium chelate, and transverse axis is wavelength (nm) among the figure, and the longitudinal axis is absorbance (A), and dotted line is the collagen curve, and solid line is collagen-calcium chelate curve.
Fig. 2 is the infrared spectrogram of collagen-calcium chelate, and transverse axis is wave number (cm among the figure
-1), the longitudinal axis is transmissivity (%), and No. 1 curve is the collagen curve, and No. 2 curves are collagen-calcium chelate curve.
Fig. 3 is the differential thermal analysis curve of collagen-calcium chelate, and transverse axis is temperature (℃), the longitudinal axis is DSC(mW/mg) among the figure, and solid line is the collagen curve, and dotted line is collagen-calcium chelate curve.
Fig. 4 is the thermogravimetric analysis figure of collagen-calcium chelate, among the figure transverse axis be temperature (℃), the longitudinal axis is weight-loss ratio (%), dotted line is the collagen curve, solid line is collagen-calcium chelate curve.
The specific embodiment
The present invention will be described in detail below in conjunction with the specific embodiment.
A kind of collagen-calcium chelate involved in the present invention is a raw material with collagen and soluble calcium salt, adopts the aqueous systems synthetic method to carry out, and reaction adding alkali lye is controlled to be acidity with reactant liquor under stirring condition.Reaction with the reactant liquor vacuum freeze drying, obtains collagen-calcium chelate after finishing; Or after reaction finishes, reactant liquor is taked dialysis or hyperfiltration treatment, and carry out the operation of vacuum freeze drying again, prepare collagen-calcium chelate product.
The human-like collagen that can select common animal sources collagen in the raw material for use or produce by genetic engineering bacterium BL21 high density fermentation, the collagen that adopts the human-like collagen animal sources to extract is compared, it has water-soluble better, virus-free hidden danger, low rejection, structure and the extremely approaching remarkable advantage of human body self collagen, show effect of supplemented calcium significantly, stay in grade, the advantage definite, safety non-toxic of tiring, thereby can be used as a kind of good functional nutrient food applications in human body.
Embodiment one:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is that 10mg/mL, volume are the calcium chloride solution of 1mL, reaction temperature is 20 ℃, reaction is 1.5 hours under stirring condition, adding the sodium hydroxide solution that molar concentration is 0.5mol/L simultaneously, is 4.0 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment two:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is that 10mg/mL, volume are the calcium chloride solution of 1.5mL, reaction temperature is 25 ℃, reaction is 2 hours under stirring condition, adding the sodium hydroxide solution that molar concentration is 0.5mol/L simultaneously, is 4.0 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment three:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is that 10mg/mL, volume are the calcium chloride solution of 1.5mL, reaction temperature is 25 ℃, reaction is 2.5 hours under stirring condition, adding the sodium hydroxide solution that molar concentration is 0.5mol/L simultaneously, is 4.0 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment four:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is that 10mg/mL, volume are the calcium chloride solution of 2mL, reaction temperature is 30 ℃, reaction is 2.5 hours under stirring condition, adding the sodium hydroxide solution that molar concentration is 1mol/L simultaneously, is 4.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment five:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is the calcium chloride solution of 10mg/mL, volume 2mL, reaction temperature is 30 ℃, reaction is 3 hours under stirring condition, adding the potassium hydroxide solution that molar concentration is 1mol/L simultaneously, is 4.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment six:
Step 1: take by weighing animal sources collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in the animal sources collagen solution is that 10mg/mL, volume are the calcium chloride solution of 2.5mL, reaction temperature is 35 ℃, reaction is 3 hours under stirring condition, adding the potassium hydroxide solution that molar concentration is 1mol/L simultaneously, is 4.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, obtain collagen-calcium chelate.
Embodiment seven:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 2.5mL, reaction temperature is 35 ℃, reaction is 3.5 hours under stirring condition, adding the potassium hydroxide solution that molar concentration is 1.5mol/L simultaneously, is 5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Embodiment eight:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 3mL, reaction temperature is 40 ℃, reaction is 3.5 hours under stirring condition, adding the potassium hydroxide solution that molar concentration is 1.5mol/L simultaneously, is 5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Embodiment nine:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 3mL, reaction temperature is 40 ℃, reaction is 4 hours under stirring condition, adding the barium hydroxide solution that molar concentration is 1.5mol/L simultaneously, is 5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Embodiment ten:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 3.5mL, reaction temperature is 45 ℃, reaction is 4 hours under stirring condition, adding the barium hydroxide solution that molar concentration is 2mol/L simultaneously, is 5.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Embodiment 11:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 3.5mL, reaction temperature is 45 ℃, reaction is 4.5 hours under stirring condition, adding the barium hydroxide solution that molar concentration is 2mol/L simultaneously, is 5.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Embodiment 12:
Step 1: take by weighing human-like collagen 100mg, be dissolved in the 10mL distilled water, adding volumetric concentration then in human-like collagen solution is that 10mg/mL, volume are the calcium chloride solution of 4mL, reaction temperature is 50 ℃, reaction is 5 hours under stirring condition, adding the barium hydroxide solution that molar concentration is 2mol/L simultaneously, is 5.5 with the pH value of controlling reactant liquor.
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
Product to above embodiment carries out ultraviolet spectral analysis, infrared spectrum analysis, differential thermal analysis and thermogravimetric analysis, and its analysis result is as follows:
1, the ultraviolet spectral analysis of collagen-calcium chelate:
Show among Fig. 1, with the maximum absorption band (λ of pure collagen
Max=206nm) compare the maximum absorption band (λ of collagen-calcium chelate
Max=223nm) moved 17nm to the long wave direction, and the height of maximum absorption band obviously increases.
2, the infrared spectrum analysis of collagen-calcium chelate is made a concrete analysis of result such as table 1 as shown in Figure 2.
3, the differential thermal analysis of collagen-calcium chelate is made a concrete analysis of result such as table 2 as shown in Figure 3.
4, the thermogravimetric analysis of collagen-calcium chelate is made a concrete analysis of result such as table 3 as shown in Figure 4.
The zoopery result that collagen-calcium chelate that the present invention makes is used for adult female ICR mouse shows: compare with the calcium carbonate with same calcium concentration, can improve bone density 4.7%, improve bone strength 10.5%.
Claims (5)
1. the preparation method of a collagen-calcium chelate is characterized in that: realized by following steps:
Step 1: with collagen and soluble calcium salt is raw material, the mass ratio of collagen and soluble calcium salt is 10:1～4, reaction temperature is 20～50 ℃, react 1.5～5h under stirring condition, the alkali lye that adds molar concentration simultaneously and be 0.5～2mol/L is 4.0～5.5 with the pH value of control reactant liquor;
Step 2: after above reaction finishes, reactant liquor is carried out vacuum freeze drying handle, perhaps reactant liquor is taked to carry out the vacuum freeze drying processing again after dialysis or the ultrafiltration, obtain collagen-calcium chelate.
2. the preparation method of a kind of collagen-calcium chelate according to claim 1, it is characterized in that: the collagen described in the step 1 is animal sources collagen or human-like collagen.
3. the preparation method of a kind of collagen-calcium chelate according to claim 1, it is characterized in that: the soluble calcium salt described in the step 1 is calcium chloride or calcium acetate.
4. the preparation method of a kind of collagen-calcium chelate according to claim 1, it is characterized in that: the alkali lye described in the step 1 is sodium hydroxide solution, potassium hydroxide solution or barium hydroxide solution.
5. collagen-calcium chelate that preparation method as claimed in claim 1 makes.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232538A (en) * | 2013-04-27 | 2013-08-07 | 西北大学 | Sulfhydrylation modified collagen calcium compound |
| CN106579459A (en) * | 2016-12-09 | 2017-04-26 | 阿布加提·阿力甫斯巴依 | Preparation method of calcium caseinate |
| CN107619441A (en) * | 2017-10-19 | 2018-01-23 | 中国水产科学研究院黄海水产研究所 | A kind of preparation method and application of collagen peptide chelating calcium microballoon |
| CN113061669A (en) * | 2021-04-15 | 2021-07-02 | 四川大学 | Enzyme unhairing method for protecting skin grain surface by carrying out calcium salt mineralization coating on skin surface |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070087039A1 (en) * | 2005-10-13 | 2007-04-19 | Gu Jennifer L | Mineral collagen chelates and methods of making and using same |
| CN101773663A (en) * | 2009-01-12 | 2010-07-14 | 顾凌洁 | New application of collagen chelate |
-
2011
- 2011-04-18 CN CN2011100960765A patent/CN102178228A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070087039A1 (en) * | 2005-10-13 | 2007-04-19 | Gu Jennifer L | Mineral collagen chelates and methods of making and using same |
| CN101773663A (en) * | 2009-01-12 | 2010-07-14 | 顾凌洁 | New application of collagen chelate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232538A (en) * | 2013-04-27 | 2013-08-07 | 西北大学 | Sulfhydrylation modified collagen calcium compound |
| CN103232538B (en) * | 2013-04-27 | 2014-10-22 | 西北大学 | Sulfhydrylation modified collagen calcium compound |
| CN106579459A (en) * | 2016-12-09 | 2017-04-26 | 阿布加提·阿力甫斯巴依 | Preparation method of calcium caseinate |
| CN107619441A (en) * | 2017-10-19 | 2018-01-23 | 中国水产科学研究院黄海水产研究所 | A kind of preparation method and application of collagen peptide chelating calcium microballoon |
| CN107619441B (en) * | 2017-10-19 | 2021-05-11 | 中国水产科学研究院黄海水产研究所 | Preparation method and application of collagen peptide chelated calcium microspheres |
| CN113061669A (en) * | 2021-04-15 | 2021-07-02 | 四川大学 | Enzyme unhairing method for protecting skin grain surface by carrying out calcium salt mineralization coating on skin surface |
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Application publication date: 20110914 |