CN103951854A - Chitosan/burdock extract/glycerinum composite membrane and preparation method thereof - Google Patents
Chitosan/burdock extract/glycerinum composite membrane and preparation method thereof Download PDFInfo
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- CN103951854A CN103951854A CN201410221826.0A CN201410221826A CN103951854A CN 103951854 A CN103951854 A CN 103951854A CN 201410221826 A CN201410221826 A CN 201410221826A CN 103951854 A CN103951854 A CN 103951854A
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Abstract
The invention discloses a chitosan/burdock extract/glycerinum composite membrane and a preparation method thereof. By taking chitosan as a base material, a burdock extract as a modifying material and glycerinum as a plasticizer, the composite membrane is prepared by the following steps: I, preparing the burdock extract; II, preparing a chitosan solution and adding the burdock extract and glycerinum to obtain a blending solution; III, uniformly stirring the blending solution obtained in the step II and carrying out vacuum debubbling; IV, putting the solution in a culture dish for tape casting, drying and solidifying by sodium hydroxide, immediately washing away sodium hydroxide by water and uncovering the membrane and airing to obtain the chitosan/burdock extract/glycerinum composite membrane. The burdock extract has strong resistance to oxidation and antibacterial activity and is blended with chitosan and glycerinum to enhance the resistance to oxidation and antibacterial activity of chitosan. The mechanical property, the air permeability and the permeability are enhanced, so that the membrane is a novel edible composite packaging membrane.
Description
Technical field
The present invention relates to a kind of taking chitosan as base material, the composite membrane of burdock extract as material modified, glycerine as softening agent and preparation method thereof.
Background technology
Chitosan (CS) is the product that polysaccharide chitin obtains after deacetylated, cheap, be easy to processing.The film of preparing taking chitosan as base material has nontoxic pollution-free, feature that gas permeability is good, has good application in preserving fruit and vegetable utilizing.Chitosan monofilm water vapour permeability is high, mechanical property is poor, when fresh-keeping to fruit and vegetable coating, easily chap, can not meet needs of production, to chitin modified the best way be and other material blend film forming at present, conventional material modified have inorganic oxide, starch, vegetable-protein etc.
Burdock (BK) can be used as medicine, and also edible is a kind of nutritious healthcare product, and it is rich in synanthrin, Mierocrystalline cellulose, protein, calcium, phosphorus, iron, the mineral substance, the amino acid that wait needed by human body to want.Burdock price is low, extraction process is simple, and synanthrin and polyphenols a large amount of in burdock extract (E-BK) make it have good oxidation-resistance and germ resistance, is obviously better than common material modified.
Summary of the invention
The object of the invention is to research and develop a kind of chitosan/burdock extract/glycerine composite membrane and its preparation method is provided, taking chitosan as base material, burdock extract is that material modified, glycerine is that softening agent is made chitosan/burdock extract/glycerine composite membrane and composite membrane is characterized and performance test, for its application in Fresh-keeping Packaging for Fruits and Vegetables is provided fundamental basis.
The object of the invention is to be achieved through the following technical solutions:
A kind of chitosan/burdock extract/glycerine composite membrane, is prepared from by 2.0 ± 0.5% (w/v) chitosan, 0.1 ± 0.05g/mL burdock extracting solution, 0.5 ± 0.3% (v/v) glycerine.
Above-mentioned chitosan/burdock extract/glycerine composite membrane, taking chitosan as base material, burdock extract is as material modified, glycerine are softening agent, is prepared from according to following steps:
One, the citric acid solution that Root of Great Burdock stripping and slicing is placed in to 2% (w/v) soaks drying and crushing after 7～13min, the powder obtaining is put into the ethanol of 70% (v/v), filter 23～4 time after extraction time 0.8～1.2h in 45～55 DEG C of waters bath with thermostatic control, filtrate rotary evaporation to concentration is 1g/mL, with brown reagent bottle splendid attire, 3.5～5 DEG C save backup.
Two, take a certain amount of chitosan, be dissolved in the acetic acid solution of 1% (v/v), add solution and glycerine in step 1, obtaining chitosan concentration is that 2.0 ± 0.5% (w/v), burdock extract concentration are that 0.1 ± 0.05g/mL, glycerol concentration are the blended liquid of 0.5 ± 0.3% (v/v).
Three, step 2 gained blended liquid is stirred evenly to final vacuum deaeration.
One, solution is placed in to culture dish curtain coating, after drying, solidify 60～65s with the sodium hydroxide of 10% (v/v) in 36～45 DEG C of baking ovens, water is rinsed sodium hydroxide well immediately, takes off film and dries, and obtains chitosan/burdock extract/glycerine composite membrane.
Tool of the present invention has the following advantages: burdock extract has strong anti-oxidation and biocidal property, by itself and chitosan, glycerine blend, oxidation-resistance and the biocidal property of having strengthened chitosan, mechanical property, ventilation property and perviousness are promoted, and are a kind of novel edible composite package films.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of chitosan monofilm and composite membrane;
Fig. 2 is pure chistosan film surface SEM photo;
Fig. 3 is pure chistosan film surface of fracture SEM photo;
Fig. 4 is chitosan/burdock extract/glycerine composite membrane surface SEM photo;
Fig. 5 is chitosan/burdock extract/glycerine composite membrane surface of fracture SEM photo;
Fig. 6 is chitosan/burdock extract tensile strength and elongation at break test result;
Fig. 7 is chitosan/burdock extract ventilation property test result;
Fig. 8 is chitosan/burdock extract water vapour permeability test result.
Embodiment
Below in conjunction with accompanying drawing, technical scheme of the present invention is further described; but be not limited to this; every technical solution of the present invention is modified or is equal to replacement, and not departing from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
1 material and equipment
1.1 material
Chitosan: deacetylation reaches >=and 95%, Shandong Hua De biological products company limited.Burdock: purchased from Harbin Carrefour.Sodium hydroxide, Glacial acetic acid, glycerine and various detection are analytical pure with reagent.
1.2 equipment
The omnipotent test machine of WDW-20J microcomputer controlled electronic, Jinan Nai Er trier company limited; Germany's Brooker Fourier infrared spectrograph, Tianjin Brighton Science and Technology Ltd.; JEM-2000FX type high resolving power transmission electron microscope, Guangzhou business quarters of Jeol Ltd.; The water vapour permeability tester of TSY-T1H model, Labthink Instruments Co., Ltd.; Magnetic stirring apparatus, thermostatical water bath, vacuumfilter etc.
2 experimental techniques
2.1 composite membrane preparations
Root of Great Burdock stripping and slicing is placed in to 2% citric acid solution and soaks drying and crushing after 10min, the powder obtaining is put into 70% ethanol, filtered three time after extracting 1h in 50 DEG C of waters bath with thermostatic control, filtrate rotary evaporation to concentration is 1g/mL, with brown reagent bottle splendid attire, 4 DEG C save backup.Take a certain amount of chitosan, be dissolved in the acetic acid solution of 1% (v/v) for subsequent use.Chitosan, burdock extracting solution, glycerine are mixed in proportion, stir evenly rear standing and defoaming.Blend solution is placed in respectively to culture dish curtain coating, after drying, solidifies 65s with 10% sodium hydroxide in 40 DEG C of baking ovens, water is rinsed sodium hydroxide well immediately, takes off film and dries.
2.2 performance test
Mechanics Performance Testing.The tensile property of composite membrane is measured the method specifying according to GB13022-91 and is carried out.
The mensuration of ventilation property.Composite membrane CO
2transmission coefficient adopts highly basic absorption process to measure, composite membrane O
2transmission coefficient is tested with OTR oxygen transmission rate determinator.
Water vapour permeability is measured.The water vapour permeability of composite membrane is measured the method specifying according to GB/T21529-2008 and is carried out.
Structural characterization.The German Brooker Fourier infrared spectrograph of high resolving power transmission electron microscope and Tianjin Brighton Science and Technology Ltd. characterizes composite membrane.
3 results and discussion
3.1 structural characterization
3.1.1 the Infrared spectroscopy of chitosan monofilm and composite membrane
The infrared spectrogram of chitosan monofilm and composite membrane is as Fig. 1.In the infrared spectra of chitosan monofilm, 1637cm
-1absorption peak belong to the flexible vibrations of v (N-H), 1401cm
-1the absorption peak at place belongs to the in-plane bending vibration of δ (O-H).Relatively the spectrogram of chitosan and chitosan complex film is found: 1637cm
-1v (N-H) absorption peak at place broadens and moves to 1628cm to lower wave number
-1place, 894cm
-1β-glycosidic link absorption peak at place moves to 886cm to lower wave number
-1place, this shows that chitosan molecule forms stronger hydrogen bond with the acidic substance reaction in burdock extract; At 1401cm
-1narrow its content of δ (O-H) absorption peak at place increases, and shows that the polyphenols that contains δ (O-H) in burdock in extract does not react, and the anti-microbial property of composite membrane does not weaken; At 663cm
-1the absorption peak at place is CO
2disturb; 584cm
-1the absorption peak that place occurs belongs to the stretching vibration of the v (C-C-O) of polysaccharide in burdock extract.
3.1.2SEM photo analysis
From Fig. 2 and 3, can find out, pure chistosan film surface and surface of fracture smoother, compact; Chitosan film surface and the surface of fracture that from Fig. 4 and Fig. 5, can find out interpolation burdock extract are more smooth, and chitosan mixes with the burdock extract of few additive, does not occur phase-splitting, illustrates that the consistency between chitosan and burdock extract is better.
3.2 burdock extract concentration are to composite membrane performance impact
3.2.1 mechanical property
Composite membrane tensile strength and elongation at break test result are as shown in Figure 6.As shown in Figure 6: add that the tensile strength of composite membrane after burdock extract obviously improves, elongation at break reduces; Along with the tensile strength of the increase composite membrane of burdock extract concentration first increases afterwards and reduces, elongation at break is on a declining curve, but slightly rise in 0.1～0.15g/mL, reason is that organic acid abundant in burdock extract reduces the pH of complex liquid, in solution-NH3
+quantity increases, and intermolecular interaction force increase is risen composite membrane intensity.But in the time that complex liquid pH value is too low, between the protonated group of molecule in chitosan and burdock extract, produce very strong electrostatic repulsion forces, combination between molecule is impacted to composite membrane strength degradation.And setting rate also causes elongation at break to decline soon in the time of alkaline purification, but burdock extract concentration loose elongation at break of composite membrane reticulated structure in the time of 0.1～0.15g/mL rises slightly; From Fig. 6, it can also be seen that tensile strength and elongation at break increase along with the increase composite membrane of chitosan concentration.Consider in composite complex liquid composite membrane machinery best performance when chitosan concentration is 2.0% (w/v), burdock extract 0.1g/ml.
3.2.2 ventilation property
The ventilation property test result of composite membrane is as Fig. 7, as shown in Figure 7: the O of composite membrane
2and CO
2transmission coefficient is along with the increase of burdock extract concentration is all first to reduce rear increase, and reason is that the densification of burdock extract concentration increase chitosan reticulated structure reduces composite membrane ventilation property, and in the time of excessive concentration, the poor ventilation property of composite membrane film-forming properties increases; Air transmission coefficient strengthens and reduces because of the increase of chitosan concentration, film-forming properties; O thoroughly
2coefficient/CO thoroughly
2coefficient <<1, this is that (D is spread coefficient because of the gas permeability P=DS of gas to macromolecular compound; S is solubility coefficient), CO
2and O
2spread coefficient to air is basically identical, but the former solubleness in chitosan film is larger, so CO
2air transmission coefficient compare O
2air transmission coefficient large.In preserving fruit and vegetable utilizing, the saturating O of composite membrane
2coefficient/CO thoroughly
2coefficient <<1 can either ensure that fruits and vegetables breathe, and maintains the continuity of its life, can control and slow down again its respiratory intensity, extends the postharvest fruit and vegetable life-span.
3.2.3 water vapour permeability (WVTR)
The water vapour permeability test result of composite membrane is as Fig. 8.As shown in Figure 8: after interpolation burdock extract, the water vapour permeability of composite membrane reduces; Along with the increase of burdock extract concentration, WVTR first reduces rear increase, because impelling chitosan molecule formation hydrogen bond that composite membrane is combined closely, burdock extract cause WVTR to reduce, in the time that burdock extract is too high, wetting ability polyphenol in the loose and extract of chitosan reticulated structure, can impel film water absorption and swelling to cause that the loose WVTR of structure of composite membrane becomes large; From Fig. 8, it can also be seen that the larger composite membrane WVTR of chitosan concentration is larger, because chitosan molecule has stronger wetting ability hydroxyl (OH) and the amino (NH of obtaining
2) can impel film water absorption and swelling, the loose WVTR of structure of composite membrane becomes large.
3.3 orthogonal test analysis
Taking chitosan concentration as 1.0%, 1.5%, 2.0% (w/v), burdock extract concentration is 0.05g/mL, 0.1g/mL, 0.15g/mL, glycerol concentration is 0.2%, 0.5%, 0.8% (v/v) design Three factors-levels orthogonal test, test index is tensile strength, elongation at break, CO2 coefficient thoroughly, water vapor transmission rate (WVTR), bacteriostasis rate, hydroxyl radical free radical clearance rate, after each index being optimized with matrix-analysis method, obtaining composite membrane optimum preparating condition is that in complex liquid, chitosan concentration is 1.5% (w/v), burdock extract 0.1g/ml, glycerol concentration is 0.5% (volume ratio).
4 conclusions
(1) draw by infrared spectra and the analysis of SEM photo, the intermolecular formation hydrogen bond of composite membrane, reticulated structure densification,, there is not phase-splitting in composite membrane smooth surface, the two consistency is better.
(2) tested and drawn by the chitosan/burdock extract composite membrane to different proportionings, the tensile strength of composite membrane, ventilation property, water vapour permeability obviously improve, but elongation at break reduces.
(3) composite membrane oxygen permeability coefficient/CO thoroughly
2coefficient <<1 can ensure fruits and vegetables breathing in preserving fruit and vegetable utilizing, can control again its respiratory intensity, extends the postharvest fruit and vegetable life-span, and chitosan-burdock extract composite membrane has good freshening effect in theory.
(4) orthogonal experiments analysis show that the best preparation scheme of chitosan/burdock/glycerine composite membrane is that in complex liquid, chitosan concentration is that 2.0% (w/v), burdock extract concentration are that 0.1g/ml, glycerol concentration are 0.5% (v/v).
Claims (8)
1. chitosan/burdock extract/glycerine composite membrane, is characterized in that described composite membrane is prepared from by 2.0 ± 0.5% (w/v) chitosan, 0.1 ± 0.05g/mL burdock extracting solution, 0.5 ± 0.3% (v/v) glycerine.
2. chitosan/burdock extract according to claim 1/glycerine composite membrane, is characterized in that described chitosan concentration is that 2.0% (w/v), burdock extract concentration are that 0.1g/mL, glycerol concentration are 0.5% (v/v).
3. a preparation method for chitosan/burdock extract/glycerine composite membrane, it is characterized in that described method taking chitosan as base material, burdock extract is as material modified, glycerine are softening agent, be prepared from according to following steps:
One, Root of Great Burdock stripping and slicing is placed in to citric acid solution and soaks drying and crushing after 7～13min, the powder obtaining is put into ethanol, in 45～55 DEG C of waters bath with thermostatic control, after extraction time 0.8～1.2h, filter three times, filtrate rotary evaporation to concentration is 1g/mL, with brown reagent bottle splendid attire, 3.5～5 DEG C save backup;
Two, take a certain amount of chitosan, be dissolved in acetic acid solution, add solution and glycerine in step 1, obtaining chitosan concentration is that 2.0 ± 0.5% (w/v), burdock extract concentration are that 0.1g ± 0.05/mL, glycerol concentration are the blended liquid of 0.5 ± 0.3% (v/v);
Three, step 2 gained blended liquid is stirred evenly to final vacuum deaeration;
Four, solution is placed in to culture dish curtain coating, after drying, solidifies 60～65s with sodium hydroxide in 36～45 DEG C of baking ovens, water is rinsed sodium hydroxide well immediately, takes off film and dries, and obtains chitosan/burdock extract/glycerine composite membrane.
4. the preparation method of chitosan/burdock extract according to claim 3/glycerine composite membrane, the concentration that it is characterized in that described citric acid solution is 2% (w/v).
5. the preparation method of chitosan/burdock extract according to claim 3/glycerine composite membrane, the concentration that it is characterized in that described ethanolic soln is 70% (v/v).
6. the preparation method of chitosan/burdock extract according to claim 3/glycerine composite membrane, the concentration that it is characterized in that described acetic acid solution is 1% (v/v).
7. the preparation method of chitosan/burdock extract according to claim 3/glycerine composite membrane, the concentration that it is characterized in that described sodium hydroxide solution is 10% (v/v).
8. the preparation method of chitosan/burdock extract according to claim 3/glycerine composite membrane, is characterized in that described chitosan concentration is that 2.0% (w/v), burdock extract concentration are that 0.1g/mL, glycerol concentration are 0.5% (v/v).
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Cited By (2)
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| CN111269467A (en) * | 2020-04-09 | 2020-06-12 | 浙江李子园食品股份有限公司 | Aralia continentalis root extract chitosan composite membrane and preparation method thereof |
| CN115678061A (en) * | 2022-09-07 | 2023-02-03 | 长江师范学院 | Method for preparing antibacterial preservative film by utilizing litchi seed/shell extract and application |
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| CN101627780A (en) * | 2008-07-14 | 2010-01-20 | 青岛农业大学 | Purely natural edible multifunctional preservative film |
| CN103275358A (en) * | 2013-05-20 | 2013-09-04 | 吉林大学 | Method for preparing chitosan-based composite preservative film or coating |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111269467A (en) * | 2020-04-09 | 2020-06-12 | 浙江李子园食品股份有限公司 | Aralia continentalis root extract chitosan composite membrane and preparation method thereof |
| CN115678061A (en) * | 2022-09-07 | 2023-02-03 | 长江师范学院 | Method for preparing antibacterial preservative film by utilizing litchi seed/shell extract and application |
| CN115678061B (en) * | 2022-09-07 | 2024-04-09 | 长江师范学院 | Method for preparing antibacterial preservative film by using lychee seed/shell extract and application of antibacterial preservative film |
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