CN109294001A - It is a kind of uniformly in crossslinked sodium alginate film and preparation method thereof - Google Patents
It is a kind of uniformly in crossslinked sodium alginate film and preparation method thereof Download PDFInfo
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- CN109294001A CN109294001A CN201810895740.4A CN201810895740A CN109294001A CN 109294001 A CN109294001 A CN 109294001A CN 201810895740 A CN201810895740 A CN 201810895740A CN 109294001 A CN109294001 A CN 109294001A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0024—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid beta-D-Glucans; (beta-1,3)-D-Glucans, e.g. paramylon, coriolan, sclerotan, pachyman, callose, scleroglucan, schizophyllan, laminaran, lentinan or curdlan; (beta-1,6)-D-Glucans, e.g. pustulan; (beta-1,4)-D-Glucans; (beta-1,3)(beta-1,4)-D-Glucans, e.g. lichenan; Derivatives thereof
- C08B37/0027—2-Acetamido-2-deoxy-beta-glucans; Derivatives thereof
- C08B37/003—Chitin, i.e. 2-acetamido-2-deoxy-(beta-1,4)-D-glucan or N-acetyl-beta-1,4-D-glucosamine; Chitosan, i.e. deacetylated product of chitin or (beta-1,4)-D-glucosamine; Derivatives thereof
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2305/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2301/00 or C08J2303/00
- C08J2305/04—Alginic acid; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2405/00—Characterised by the use of polysaccharides or of their derivatives not provided for in groups C08J2401/00 or C08J2403/00
- C08J2405/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
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Abstract
It is a kind of uniformly in crossslinked sodium alginate film and preparation method thereof, each component comprising following parts by weight: 1-5 parts of sodium alginate, chitosan oligosaccharide -0.05-1 parts of calcium complex, 0.05-1 parts of the NaOH solution of 0.1M, 1-5 parts of organic acid, 2-10 parts of glycerol, 40-85 parts of deionized water.The present invention innovate using chitosan oligosaccharide-calcium complex as sodium alginate internal crosslinker, pass through the adjusting of system pH, in sodium alginate at uniformly releasing divalent calcium ions in film liquid, uniform calcium cross-linked sodium alginate film is prepared, external crosslinking technology is overcome since crosslinking is crossed in part, partial cross-linking spends low, caused film forming problem of non-uniform；The degree of cross linking of film can be regulated and controled by adjusting sodium alginate and chitosan oligosaccharide-calcium complex ratio simultaneously；In addition, the chitosan oligosaccharide that chitosan oligosaccharide-calcium complex releases can also assign film certain anti-microbial property, had a good application prospect in food industry and field of medicaments.
Description
Technical field
The present invention relates to sodium alginate based aquagel field more particularly to a kind of uniformly interior crossslinked sodium alginate film and its systems
Preparation Method.
Background technique
Sodium alginate is a kind of Natural linear polysaccharide extracted from brown alga, sargassum, is by β-Isosorbide-5-Nitrae-D mannuronic acid
A kind of random linear block copolymers that (M unit) and α-Isosorbide-5-Nitrae-D guluronic acid (G unit) are constituted, structure such as Fig. 1 institute
Show, be made of three kinds of residues: continuous G unit residue (GG), continuous M unit residue (MM) and GM mixing residue (GM).
As a kind of natural polysaccharide, sodium alginate because of its excellent performance, such as degradability, film forming, compatibility and by
It is widely used in the fields such as chemistry, biology, medicine, food；But its mechanical property is poor to be limited its application.Studies have shown that extra large
G unit in alginic acid sodium molecule can be crosslinked quickly under the action of bivalent cation, form gel, this ionomer
The formation of structure can effectively improve the mechanical property of sodium alginate, further expand sodium alginate in food industry and medicine
The application in field.Ca2+With the cross-linking reaction of sodium alginate have reaction speed it is fast/advantages such as reaction condition is mild, therefore, chlorination
Calcium solution is commonly used for the preparation of sodium alginate gel, currently, the preparation of sodium alginate gel is generally by Ca2+External crosslinking
Technology will contain Ca2+Solution and sodium alginate soln be mixed and obtain, but preparing alginic acid using solution casting method
When sodium gel film, it is still that sodium alginate soln addition calcium chloride is molten that sodium alginate soln either is added in chloride containing calcium solution
In liquid, due to Ca2+Ion complexation occurs for the G unit that can be in contact with it rapidly, forms cross-linked structure, and cross-linked structure once produces
It is raw, Ca2+It is difficult to be diffused into cross-linked structure, the G unit for including in cross-linked structure is caused to be difficult to and Ca2+It reacts, because
This, this external crosslinking technology, which frequently can lead to sodium alginate, locally to be crossed and is crosslinked, partial cross-linking spend it is low, to cause gel uneven
It is even, it is not able to satisfy the particular/special requirement of some applications.It researchs and proposes interior crosslinking technological and passes through control Ca2+It is uniform slowly
It discharges to control the uniformity of gel mould, but CaCO3 or CaSO is usually used in this interior crosslinking technological4As calcium source in acid
Ca is slowly released under the conditions of property2+, but CaCO3The CO of generation is dissolved in acid condition2Bubble will affect the film forming of gel
Property, and CaSO4Middle SO4 2-Introducing for gel mould in terms of application carry out potential uncertain risk.
Summary of the invention
The present invention overcomes the disadvantages of the prior art, provide it is a kind of uniformly in crossslinked sodium alginate film and its preparation side
Method.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions:
A kind of uniformly interior crossslinked sodium alginate film, each component comprising following parts by weight: 1-5 parts of sodium alginate, chitosan oligosaccharide-
0.05-1 parts of calcium complex, 0.05-1 parts of the NaOH solution of 0.1M, 1-5 parts of organic acid, 2-10 parts of glycerol, deionized water 40-85
Part.
A kind of preparation method of uniformly interior crossslinked sodium alginate film, comprising the following steps:
(1) sodium alginate powder is added in deionized water by formula, for heating systems to 60 DEG C, seaweed is prepared in stirring
Acid sodium aqueous solution is cooled to room temperature；
(2) glycerol is added into above-mentioned sodium alginate aqueous solution, after being dispersed with stirring uniformly, the NaOH solution tune of 0.1M is added
System pH is saved 10 or so；
(3) chitosan oligosaccharide-calcium complex is dissolved in suitable deionized water, 1-5% (w/v, g/100mL) is prepared
The chitosan oligosaccharide of concentration-calcium complex aqueous solution；
(4) under the mixing speed of 1000-2000rpm, the chitosan oligosaccharide in (3)-calcium complex aqueous solution is added drop-wise to (2)
In solution, mixing time 15-20min；
(5) under the mixing speed of 2000-3000rpm, organic acid is added dropwise into above-mentioned (4) system in 5-15min, adjusts
The pH value of system is between 5.5-6.5；
(6) sodium alginate obtained in (5) at film liquid vacuum filter and is deaerated, takes the film forming of 10-20mL handled well
Liquid is in the culture dish that diameter is 10cm, by culture dish as 20 DEG C, in the environment of humidity 30-40% after 72h, obtains in uniformly
The sodium alginate film wet film of crosslinking；
(7) sodium alginate film wet film obtained in (6) drying in 105 DEG C of baking oven is placed at least for 24 hours, to obtain in uniformly
The sodium alginate film dry film of crosslinking.
Further, the concentration of the sodium alginate aqueous solution is between 0.2-1% (w/v, g/100mL)；Chitosan oligosaccharide-calcium network
The concentration of object aqueous solution is closed between 1-5% (w/v, g/100mL).
Further, the sodium alginate and chitosan oligosaccharide-calcium complex mass ratio are between 1:0.1-0.2.
Further, the mass ratio of the sodium alginate and glycerol is between 1:0.5-2.
Further, the organic acid is citric acid or glucolactone, and the acid that organic acid is configured to 0.05-0.1M is molten
Liquid uses.
Wherein, the chitosan oligosaccharide-calcium complex preparation method the following steps are included:
(1) preparation of calcium salt concentrated solution
In deionized water by calcium salt dissolution, preparation obtains calcium salt concentrated solution, controls the concentration of calcium saline solution in 50-
85% (m/v, g/100mL)；
(2) chitosan oligosaccharide-calcium complex preparation
By formula by the calcium salt concentrated solution in chitosan oligosaccharide dissolution in step (1), pH adjusting agent, regulation system pH value is added
Between 9-10,30-45min is complexed at room temperature；
(3) chitosan oligosaccharide-calcium complex alcohol precipitation
Dehydrated alcohol is added in complex system in step (2), controls the volume ratio of dehydrated alcohol and complex system
Between 1.5-2:1, after being sufficiently mixed, make chitosan oligosaccharide-calcium complex precipitating 1-2h.
(4) chitosan oligosaccharide-calcium complex separation and purification
Step (3) are centrifugated (5000-10000rpm/15-20min), and wash precipitating 2-3 times with dehydrated alcohol,
Vacuum drying, obtains lily chitosan oligosaccharide-calcium complex.
Further, the chitosan oligosaccharide be low molecular weight water soluble chitosan, molecular weight between 1000-3000Da,
The calcium salt is water-soluble Ca salt, and the water-soluble Ca salt is calcium chloride, calcium bromide, calcium iodide or calcium nitrate, the water solubility
The mass ratio of chitosan oligosaccharide and water-soluble Ca salt is between 1:30-80.
Compared with prior art, the beneficial effects of the present invention are:
The present invention innovate using chitosan oligosaccharide-calcium complex as sodium alginate internal crosslinker, by the adjusting of system pH,
In sodium alginate at divalent calcium ions are uniformly released in film liquid, uniform calcium cross-linked sodium alginate film is prepared, gram
External crosslinking technology is taken since crosslinking is crossed in part, partial cross-linking spends low, caused film forming problem of non-uniform；Tune can be passed through simultaneously
Section sodium alginate and chitosan oligosaccharide-calcium complex ratio regulate and control the degree of cross linking of film；In addition, chitosan oligosaccharide-calcium complex is released
The chitosan oligosaccharide released can also assign film certain anti-microbial property, before food industry and field of medicaments have application well
Scape.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and is used to explain the present invention together with embodiments of the present invention,
It is not construed as limiting the invention, in the accompanying drawings:
Fig. 1 sodium alginate structural schematic diagram；
The thermal weight loss the performance test results of Fig. 2 dry film sample.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
1. the preparation of chitosan oligosaccharide-calcium complex:
(1) preparation of calcium salt concentrated solution
70g anhydrous calcium chloride is dissolved in 100mL deionized water, preparation obtains calcium salt concentrated solution, obtain 70% (m/v,
G/100mL concentration calcium chloride concentrated solution)；
(2) chitosan oligosaccharide-calcium complex preparation
It takes 0.3g chitosan oligosaccharide to be added in the above-mentioned calcium chloride solution of 20mL, pH adjusting agent is added, regulation system pH value is in 9-
Between 10,30-45min is complexed at room temperature；
(3) chitosan oligosaccharide-calcium complex alcohol precipitation
35mL dehydrated alcohol is added in complex system in (2), after shaking up mixing, makes chitosan oligosaccharide-calcium complex precipitating
1-2h；
(4) chitosan oligosaccharide-calcium complex separation and purification
(3) are centrifugated (8000rpm/20min), filter cake washs precipitating 2-3 times with dehydrated alcohol, and vacuum drying obtains
To lily chitosan oligosaccharide-calcium complex.
2. the preparation of crossslinked sodium alginate film in uniformly
(1) 2g sodium alginate powder is added in 100mL deionized water, for heating systems to 60 DEG C, stirring is prepared 2%
(m/v, g/100mL) sodium alginate aqueous solution, is cooled to room temperature；
(2) NaOH of 0.1M is added after being dispersed with stirring uniformly in the glycerol that 3mL is added into above-mentioned sodium alginate aqueous solution
Solution regulation system pH value is 10 or so；
(3) 0.1g chitosan oligosaccharide-calcium complex is dissolved in 10mL deionized water, 1% (w/v, g/100mL) is prepared
The chitosan oligosaccharide of concentration-calcium complex aqueous solution；
(4) under the mixing speed of 1000-2000rpm, the chitosan oligosaccharide in (3)-calcium complex aqueous solution is added drop-wise to (2)
In solution system, mixing time 15-20min；
(5) under the mixing speed of 2000-3000rpm, the citric acid of 1M is added dropwise in 5-15min into above-mentioned (4) system
Solution, the pH value of regulation system is between 5.5-6.5；
(6) sodium alginate obtained in (5) at film liquid vacuum filter and is deaerated, take 15mL handle well at film liquid in
Diameter is, by culture dish as 20 DEG C, in the environment of humidity 30-40% after 72h, to obtain crosslinking in uniformly in the culture dish of 10cm
Sodium alginate film wet film；
(7) sodium alginate film wet film obtained in (6) drying in 105 DEG C of baking oven is placed at least for 24 hours, to obtain in uniformly
The sodium alginate film dry film of crosslinking.
Embodiment 2
The present embodiment is substantially same as Example 1, and difference is in uniform the step of the preparation of crossslinked sodium alginate film
(3) in, 0.2g chitosan oligosaccharide-calcium complex is dissolved in 10mL deionized water, 2% (w/v, g/100mL) concentration is prepared
Chitosan oligosaccharide-calcium complex aqueous solution.
Embodiment 3
The present embodiment is substantially same as Example 1, and difference is: 1. in the preparation of uniform interior crossslinked sodium alginate film
The step of (1) in, by 5g sodium alginate powder be added 100mL deionized water in, to 60 DEG C, stirring is prepared heating systems
5% (m/v, g/100mL) sodium alginate aqueous solution, is cooled to room temperature；2. the step of the preparation in uniform interior crossslinked sodium alginate film
Suddenly in (3), 0.5g chitosan oligosaccharide-calcium complex is dissolved in 10mL deionized water, it is dense that 5% (w/v, g/100mL) is prepared
The chitosan oligosaccharide of degree-calcium complex aqueous solution.
Performance detection data: chitosan oligosaccharide-calcium complex blank sodium alginate is not added referring to the formula preparation of embodiment 1
Film sample carries out performance detection, the crosslinking of embodiment 1-3 to the uniform interior crossslinked sodium alginate film of embodiment 1-3 and blank sample
Density uniformity testing result is shown in Table 1.The thermal weight loss testing result of embodiment 1-3 and blank sample dry film is shown in Fig. 1.
The uniformity of sodium alginate film is measured using wet film/dry film weight ratio, and 3 pieces of areas are taken on each sample
Size is about 2*2cm21., 2., 3. film, number are followed successively by, successively weigh and record the weight of its wet/dry film, calculate theirs
Dry/wet weight ratio ((wet film weight-dry film weight)/wet film weight), the standard deviation size according to calculated result and average value
Judge the uniformity of film crosslinking.
1 sodium alginate film sample crosslink density uniformity testing result of table
From sodium alginate film sample in table 1 it is dry/the Mean Deviation value analysis of wet film weight ratio: embodiment 1-3 sample
In, appoint the wet/dry film for taking 3 pieces of areas about the same to carry out weighing calculating in any one sample, the results showed that, the same sample
In, dry/wet film weight ratio of any 3 block film is close, and average deviation shows the uniformity of sample within 0.01%
Good, i.e., chitosan oligosaccharide-calcium complex can effectively promote the uniform interior crosslinking of sodium alginate film.
From figure 2 above: compared with blank sample, the thermal decomposition temperature of embodiment 1-3 starting increases；In high temperature
Under, the thermal weight loss rate of embodiment 1-3 is slow compared with blank sample, and above-mentioned phenomenon shows that the sodium alginate dry film of embodiment 1-3 is formed
Effective cross-linked structure.
Finally, it should be noted that these are only the preferred embodiment of the present invention, it is not intended to restrict the invention, although
Referring to embodiment, invention is explained in detail, for those skilled in the art, still can be to aforementioned
Technical solution documented by each embodiment is modified or equivalent replacement of some of the technical features, but it is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in protection of the invention
Within the scope of.
Claims (8)
1. a kind of uniformly interior crossslinked sodium alginate film, which is characterized in that each component comprising following parts by weight: sodium alginate 1-5
Part, chitosan oligosaccharide -0.05-1 parts of calcium complex, 0.05-1 parts of the NaOH solution of 0.1M, 1-5 parts of organic acid, 2-10 parts of glycerol, go from
Sub- water 40-85 parts.
2. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 1, which is characterized in that including following
Step:
(1) sodium alginate powder is added in deionized water by formula, for heating systems to 60 DEG C, sodium alginate is prepared in stirring
Aqueous solution is cooled to room temperature；
(2) glycerol is added into above-mentioned sodium alginate aqueous solution, after being dispersed with stirring uniformly, the NaOH solution that 0.1M is added adjusts body
It is pH value 10 or so；
(3) chitosan oligosaccharide-calcium complex is dissolved in suitable deionized water, 1-5% (w/v, g/100mL) concentration is prepared
Chitosan oligosaccharide-calcium complex aqueous solution；
(4) under the mixing speed of 1000-2000rpm, the chitosan oligosaccharide in (3)-calcium complex aqueous solution is added drop-wise to (2) solution
In, mixing time 15-20min；
(5) under the mixing speed of 2000-3000rpm, organic acid, regulation system is added dropwise into above-mentioned (4) system in 5-15min
PH value between 5.5-6.5；
(6) sodium alginate obtained in (5) at film liquid vacuum filter and is deaerated, take 10-20mL handle well at film liquid in
Diameter is, by culture dish as 20 DEG C, in the environment of humidity 30-40% after 72h, to obtain crosslinking in uniformly in the culture dish of 10cm
Sodium alginate film wet film；
(7) sodium alginate film wet film obtained in (6) is placed in drying in 105 DEG C of baking oven and at least for 24 hours, obtains crosslinking in uniformly
Sodium alginate film dry film.
3. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 2, which is characterized in that the seaweed
The concentration of acid sodium aqueous solution is between 0.2-1% (w/v, g/100mL)；Chitosan oligosaccharide-calcium complex aqueous solution concentration is in 1-5%
Between (w/v, g/100mL).
4. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 2, which is characterized in that the seaweed
Sour sodium and chitosan oligosaccharide-calcium complex mass ratio are between 1:0.1-0.2.
5. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 2, which is characterized in that the seaweed
The mass ratio of sour sodium and glycerol is between 1:0.5-2.
6. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 2, which is characterized in that described organic
Acid is citric acid or glucolactone, and the acid solution that organic acid is configured to 0.05-0.1M is used.
7. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 2, which is characterized in that wherein, institute
State chitosan oligosaccharide-calcium complex preparation method the following steps are included:
(1) preparation of calcium salt concentrated solution
In deionized water by calcium salt dissolution, preparation obtains calcium salt concentrated solution, controls the concentration of calcium saline solution in 50-85%
(m/v, g/100mL)；
(2) chitosan oligosaccharide-calcium complex preparation
By formula by the calcium salt concentrated solution in chitosan oligosaccharide dissolution in step (1), pH adjusting agent is added, regulation system pH value is in 9-
Between 10,30-45min is complexed at room temperature；
(3) chitosan oligosaccharide-calcium complex alcohol precipitation
Dehydrated alcohol is added in complex system in step (2), the volume ratio for controlling dehydrated alcohol and complex system exists
Between 1.5-2:1, after being sufficiently mixed, make chitosan oligosaccharide-calcium complex precipitating 1-2h；
(4) chitosan oligosaccharide-calcium complex separation and purification
Step (3) are centrifugated (5000-10000rpm/15-20min), and wash precipitating 2-3 times with dehydrated alcohol, vacuum
It is dry, obtain lily chitosan oligosaccharide-calcium complex.
8. a kind of preparation method of uniformly interior crossslinked sodium alginate film according to claim 7, which is characterized in that the shell is few
Sugar is the water soluble chitosan of low molecular weight, and for molecular weight between 1000-3000Da, the calcium salt is water-soluble Ca salt, institute
Stating water-soluble Ca salt is calcium chloride, calcium bromide, calcium iodide or calcium nitrate, the quality of the water-soluble chitosan oligosaccharide and water-soluble Ca salt
Than between 1:30-80.
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| US11560487B2 (en) | 2020-09-22 | 2023-01-24 | Swimc Llc | Coating compositions containing low molecular weight chitosan composition |
| WO2023067161A1 (en) * | 2021-10-22 | 2023-04-27 | Mujō Lab Ohg | Method for producing an alginate-based film, and alginate-based film |
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| CN113174060A (en) * | 2021-03-22 | 2021-07-27 | 中国海洋大学 | Alginic acid-chitosan oligosaccharide-zinc oxide composite hydrogel and preparation method and application thereof |
| CN113174060B (en) * | 2021-03-22 | 2022-04-29 | 中国海洋大学 | Alginic acid-chitosan oligosaccharide-zinc oxide composite hydrogel and preparation method and application thereof |
| WO2023067161A1 (en) * | 2021-10-22 | 2023-04-27 | Mujō Lab Ohg | Method for producing an alginate-based film, and alginate-based film |
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