CN104194015B - A kind of preparation method of food packaging soybean protein and sodium alginate cross-linking film - Google Patents
A kind of preparation method of food packaging soybean protein and sodium alginate cross-linking film Download PDFInfo
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- CN104194015B CN104194015B CN201410449481.4A CN201410449481A CN104194015B CN 104194015 B CN104194015 B CN 104194015B CN 201410449481 A CN201410449481 A CN 201410449481A CN 104194015 B CN104194015 B CN 104194015B
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Abstract
The invention discloses the preparation method of a kind of food packaging soybean protein and sodium alginate cross-linking film, belong to biomaterial and packaging for foodstuff preparing technical field.Preparation technology is carried out according to the following steps：Soy bean proteinous soln and sodium alginate soln are prepared with distilled water respectively, according to mass volume ratio 4:6,5:5,6:4 ratio be stirred it is well mixed after add crosslinking agent and carry out cross-linking reaction and dialyse to remove crosslinking agent, then film forming solution is flat in glass plate, the cross linking membrane that different proportion can be prepared after 12 16h is dried under the conditions of 40 DEG C.Cross linking membrane is characterized after 48h is balanced under conditions of 25 DEG C of relative humidity 50% or so.The extension at break of cross linking membrane, which is selected, is far longer than soybean protein sodium alginate blend film and simple sodium alginate, and has preferable water preventing ability and oxygen resistance.The cross linking membrane has good biocompatibility and a biodegradability, and the advantages that nontoxic, tasteless and nonirritant, can be widely applied to food packaging applications.
Description
Technical field
The invention belongs to biomaterial and packaging for foodstuff preparing technical field, and in particular to a kind of soybean protein and alginic acid
The preparation method of sodium cross linking membrane.
Background technology
In recent years, with gradual enhancing of the people to environmental protection consciousness, and energy crisis and resource constraint are recognized
Gradual intensification, using from plant resources biological degradable material replace from petroleum resources non-biodegradable
Plastics, the research for preparing environment-friendly biological packing material greatly paid close attention to, and be increasingly becoming Materials must
Right trend.
Soybean protein is the higher polymer substance of the protein content extracted in the accessory substance after soybean slag oil expression, by a variety of
Amino acid forms, and its wide material sources is cheap, nutritious, renewable, and there is good biocompatibility and biology can drop
Xie Xing, and have good filming performance and oxygen resistance.But fragility is big during independent film forming, cold resistance is poor, and block-water performance is poor.
Sodium alginate (SA) is a kind of polyuronide for the line style extracted from natural brown alga, by α-L- guluronic acids (G units) and
The random copolymer that beta-D-mannuronic acid (M units) is connected into by 1,4 glycosidic bonds.G and M ratio determines sodium alginate
The characteristic such as different structures and biocompatibility.SA is safe in food, in the relevant standard regulation of US and European,
Ratify sodium alginate and be used as " safe, applicable, disposable composition ".Sodium alginate has good film forming, but single
One film poor plasticity, gloss is bad, and film-strength is low, and oxygen resistance is also poor.The main object of the present invention is integrated soybean protein
With the premium properties of sodium alginate, improve the resistance oxygen of soybean protein isolate and sodium alginate cross-linking film, block water and mechanical strength
Deng key index, be allowed to can extensively using with food in terms of performance be greatly improved, there is preferable application prospect.
The content of the invention
The invention aims to provide the preparation side of a kind of simple and practical soybean protein and sodium alginate cross-linking film
Method, it can apply to food packaging applications.
To achieve these goals, the technical solution adopted by the present invention is：
The preparation method of a kind of food packaging soybean protein and sodium alginate cross-linking film, comprises the following steps：
(1) film forming solution is prepared：Distilled water compound concentration is 1-25% soybean protein and sodium alginate soln, according to big
Legumin is 4 with sodium alginate mass ratio:6,5:5,6:4 ratio is stirred well mixed；
(2) cross-linking reaction：The mixed solution of step (1) is added to appropriate crosslinking agent, is stirred at room temperature and is reacted and dialyse；
(3) it is film-made：The solution of step (2) is poured into homemade glass plate, after dry 12-24h under the conditions of 40 DEG C
It can be prepared by the cross linking membrane of soybean protein and sodium alginate.
The soybean protein is water-soluble soybean protein, and molecular weight is 1-10 ten thousand, protein content 40-90%.
The crosslinking agent is that 1- ethyls-(3- dimethylaminopropyls) phosphinylidyne diimmonium salt hydrochlorate and N- hydroxysuccinimidyls acyl are sub-
The composition of amine.
The addition of the 1- ethyls-(3- dimethylaminopropyls) phosphinylidyne diimmonium salt hydrochlorate is sodium alginate mass ratio
1-15 times；The addition of the n-hydroxysuccinimide is 1-5 times of sodium alginate mass ratio.
Room temperature stirring reaction 4-24h after addition crosslinking agent in the step (2).
Beneficial effects of the present invention：
(1) present invention is using soybean protein as primary raw material, green non-poisonous, non-environmental-pollution；
(2) present invention provides a kind of preparation method of the crosslinked film of soybean protein and sodium alginate, simple to operate, is made
Film thickness it is uniform, surfacing is smooth, and elongation percentage is big, resistance oxygen block-water performance it is good, there is good biocompatibility and life
Biodegradable.
Brief description of the drawings
Fig. 1 is the FIRT of soybean protein and alginate films detections figure made from embodiment 1-4.
Fig. 2 is the biodegradability of soybean protein and alginate films measure figure made from embodiment 1-4；It will make
Cross linking membrane be put into potato agar medium, access aspergillus CGMCC 3.3928, cultivate 7 days in 26 DEG C of incubator, hair
The surface of existing cross linking membrane overgrows with clone, shows that obtained soybean protein has biodegradability with sodium alginate cross-linking film
Energy.
Fig. 3 is the cell survival rate result figure of soybean protein made from embodiment 1-4 and alginate films；Simple original
The cell survival rate of material and the composite membrane of soybean protein and sodium alginate shows obtained soybean protein and sea more than 90%
Mosanom crosslinked film has good biocompatibility.
Embodiment
Embodiment 1
The preparation method of a kind of food packaging soybean protein and sodium alginate cross-linking film, comprises the following steps：
(1) film forming solution is prepared：Add soybean protein 0.8g and 1.2g sodium alginate, 100ml distilled water, i.e. material quality
Than for 4:6, it is uniformly mixed；
(2) cross-linking reaction：The mixed solution of step (1) is added into 2.4g 1- ethyls-(3- dimethylaminopropyls) phosphinylidyne
Diimmonium salt hydrochlorate, 1.2g n-hydroxysuccinimides, reaction 16h is stirred at room temperature, reaction solution is dialysed afterwards；
(3) it is film-made：The solution of step (2) is poured into homemade glass plate, after dry 16h under the conditions of 40 DEG C
The crosslinked film abbreviation CS40A60 of soybean protein and sodium alginate is made.
Embodiment 2
The preparation method of a kind of food packaging soybean protein isolate and sodium alginate cross-linking film, comprises the following steps：
(1) film forming solution is prepared：Soybean protein 1.5g and 1.5g sodium alginate is added, 100ml distilled water, i.e. mass ratio are
5:5,100ml distilled water, i.e. material quality ratio are 5:5 are uniformly mixed；
(2) cross-linking reaction：The mixed solution of step (1) is added into mixed solution and adds 3.0g 1- ethyls-(3- dimethyl
Aminopropyl) phosphinylidyne diimmonium salt hydrochlorate, 1.5g n-hydroxysuccinimides, reaction 16h is stirred at room temperature, afterwards by reaction solution
Dialysis；
(3) it is film-made：The solution of step (2) is poured into homemade glass plate, after dry 16h under the conditions of 40 DEG C
The crosslinked film abbreviation CS50A50 of soybean protein and sodium alginate is made.
Embodiment 3
The preparation method of a kind of food packaging soybean protein and sodium alginate cross-linking film, comprises the following steps：
(1) film forming solution is prepared：Soybean protein 1.2g and 0.8g sodium alginate is added, 100ml distilled water, i.e. mass ratio are
5:5,100ml distilled water, i.e. material quality ratio are 6:4 are uniformly mixed；
(2) cross-linking reaction：The mixed solution of step (1) is added into mixed solution and adds 1.6g 1- ethyls-(3- dimethyl
Aminopropyl) phosphinylidyne diimmonium salt hydrochlorate, 0.80g n-hydroxysuccinimides, reaction 16h is stirred at room temperature, afterwards by reaction solution
Dialysis；
(3) it is film-made：The solution of step (2) is poured into homemade glass plate, after dry 16h under the conditions of 40 DEG C
The crosslinked film abbreviation CS60A40 of soybean protein and sodium alginate is made.
Embodiment 4
The preparation method of a kind of food packaging soybean protein isolate and sodium alginate blend film, comprises the following steps：
(1) film forming solution is prepared：Soybean protein 1.5g and 1.5g sodium alginate is added, 100ml distilled water, i.e. mass ratio are
5:5,100ml distilled water, i.e. material quality ratio are 5:5 are uniformly mixed；
(2) it is film-made：The solution of step (1) is poured into homemade glass plate, after dry 16h under the conditions of 40 DEG C
The blend film abbreviation BS50A50 of soybean protein and sodium alginate is made.
Soybean protein made from embodiment 1-4 and alginate films are done film thickness, tensile strength, elongation at break,
The performance test of moisture-vapor transmission, OTR oxygen transmission rate, its method difference are as follows：
(1) detection is characterized：It is 50% ± 5 that obtained film is put into relative humidity, and temperature balances under conditions of being 25 ± 5 DEG C
48h。
(2) film thickness：10 different sites are chosen, the digital display thousand produced using Taizhou plain Ai Ce Instrument Ltd. is divided
Calibrator determines the thickness of film, obtains average value.
(3) tensile strength and elongation at break：Controlled according to ASTM Standard D-882-02 standard laws using microcomputer
Universal testing machine determines the tensile strength and elongation at break of film.
(4) OTR oxygen transmission rate：Method according to the measure dissolved oxygen amounts proposed of Winkler in 1888 is O2―→2Mn
(OH)2―→MnMnO3―→2I2―→4Na2S2O3Using the method for titration, soybean protein is determined respectively and is answered with sodium alginate
Close the OTR oxygen transmission rate of film.
(5) moisture-vapor transmission：Appropriately sized film is cut to be sealed on the identical vial mouth of volume size,
Vial is filling with water at bottleneck 1cm, is put into relative humidity as 50% or so, under conditions of temperature is 25 DEG C, timing survey
Determine the change of weight；Moisture-vapor transmission calculation formula is：WAP=Δ w/ Δ t*A*L/ Δ p, Δ w/ Δs t are weight with the time
Rate of change, A is the size of bottleneck film, and L is the thickness of film, and Δ p is that the external and internal pressure of film is poor.
(6) biocompatibility detects：Carried out according to ISO10993-5 standard test methods：Weigh 15mg film distilled water
Soak and dry after 12h, ultraviolet irradiates simultaneously to be cleaned 3 times with culture medium, adds the incubator at 37 DEG C after 10ml culture medium
Interior standing 24h is the preparation for completing leaching liquor；Mouse embryo fibroblast NIH3T3 digests after cultivating to logarithmic phase to be diluted to
Every milliliter contains 5-6 × 104Individual cell, after 37 DEG C of bed board cultivates 24h, leaching liquor is replaced, cultivate 24h, distinguish after 48h, 72h
Determine its OD570nm light absorption value, using add mass percent as 0.64% phenol as a control group, according to formula
Cellviability (%)=OD570 (sample)/OD570 (blank) * 100 calculates cell survival rate.
(7) biodegradability：The flat board containing potato culture medium is layered on after the film ultraviolet irradiation of clip 2cm*2cm sizes
On, cultivated 7 days or so under conditions of 26 DEG C, observe colony growth form.
(8) infrared detection：Fourier transform infrared detection is carried out to composite membrane, and draws out infrared spectrogram.To implementing
Soybean protein and alginate films made from example 1-4 do film thickness, tensile strength, elongation at break,
The performance test of moisture-vapor transmission, OTR oxygen transmission rate and cell survival rate, as a result see the table below：
Claims (4)
1. the preparation method of a kind of food packaging soybean protein and sodium alginate cross-linking film, it is characterised in that including following step
Suddenly：
（1）Prepare film forming solution：Distilled water compound concentration is 1-25% soybean protein and sodium alginate soln, according to soybean egg
It is in vain 4 with sodium alginate mass ratio:6,5:5,6:4 ratio is stirred well mixed；
（2）Cross-linking reaction：By step（1）Mixed solution add appropriate crosslinking agent, be stirred at room temperature and react and dialyse；
（3）Film：By step（2）Solution pour into homemade glass plate, after drying 12-24 h under the conditions of 40 DEG C
The cross linking membrane of soybean protein and sodium alginate is made；
The step（2）Room temperature stirring reaction 4-24h after middle addition crosslinking agent.
2. the preparation method of a kind of food packaging soybean protein according to claim 1 and sodium alginate cross-linking film, its
It is characterised by：The soybean protein is water-soluble soybean protein, and molecular weight is 1-10 ten thousand, protein content 40-90%.
3. the preparation method of a kind of food packaging soybean protein according to claim 1 and sodium alginate cross-linking film, its
It is characterised by：The crosslinking agent is 1- ethyls-(3- dimethylaminopropyls) phosphinylidyne diimmonium salt hydrochlorate and N- hydroxysuccinimidyl acyls
The composition of imines.
4. the preparation method of a kind of food packaging soybean protein according to claim 1 and sodium alginate cross-linking film, its
It is characterised by：The addition of the 1- ethyls-(3- dimethylaminopropyls) phosphinylidyne diimmonium salt hydrochlorate is sodium alginate quality
1-15 times of ratio；The addition of the n-hydroxysuccinimide is 1-5 times of sodium alginate mass ratio.
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| CN105254908B (en) * | 2015-10-09 | 2018-05-15 | 青岛大学 | A kind of preparation method and application of anisotropy alginate film |
| CN108467708A (en) * | 2018-05-07 | 2018-08-31 | 长乐智高生物科技有限公司 | A kind of preparation method of modified soy protein adhesive |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134400A (en) * | 2010-01-27 | 2011-07-27 | 吉林农业大学 | Method for preparing edible film taking soybean proteins as matrixes through hydrolase modification |
| CN102731810A (en) * | 2012-07-16 | 2012-10-17 | 渤海大学 | Method for preparing degradable dry beancurd preservation packaging film |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102134400A (en) * | 2010-01-27 | 2011-07-27 | 吉林农业大学 | Method for preparing edible film taking soybean proteins as matrixes through hydrolase modification |
| CN102731810A (en) * | 2012-07-16 | 2012-10-17 | 渤海大学 | Method for preparing degradable dry beancurd preservation packaging film |
Non-Patent Citations (1)
| Title |
|---|
| EDC和NHS对玉米醇溶蛋白成膜性质的影响;张敏等;《食品科学》;20150115;第35卷(第1期);摘要及背景技术部分 * |
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