CN115715588A - Preparation method and application of hordein-chitosan high internal phase Pickering emulsion - Google Patents
Preparation method and application of hordein-chitosan high internal phase Pickering emulsion Download PDFInfo
- Publication number
- CN115715588A CN115715588A CN202210896299.8A CN202210896299A CN115715588A CN 115715588 A CN115715588 A CN 115715588A CN 202210896299 A CN202210896299 A CN 202210896299A CN 115715588 A CN115715588 A CN 115715588A
- Authority
- CN
- China
- Prior art keywords
- hordein
- chitosan
- solution
- preparation
- emulsion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000839 emulsion Substances 0.000 title claims abstract description 109
- 229920001661 Chitosan Polymers 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 108010068370 Glutens Proteins 0.000 claims abstract description 34
- 239000007788 liquid Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000003921 oil Substances 0.000 claims description 52
- 235000019198 oils Nutrition 0.000 claims description 51
- 239000000243 solution Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000002105 nanoparticle Substances 0.000 claims description 19
- 239000011550 stock solution Substances 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 17
- 239000003381 stabilizer Substances 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 11
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 239000003549 soybean oil Substances 0.000 claims description 8
- 235000012424 soybean oil Nutrition 0.000 claims description 8
- 235000007340 Hordeum vulgare Nutrition 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 239000011780 sodium chloride Substances 0.000 claims description 5
- 238000002390 rotary evaporation Methods 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 230000000295 complement effect Effects 0.000 claims description 2
- 238000004108 freeze drying Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 238000009210 therapy by ultrasound Methods 0.000 claims description 2
- 240000005979 Hordeum vulgare Species 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003002 pH adjusting agent Substances 0.000 claims 1
- 238000003860 storage Methods 0.000 abstract description 8
- 108090000623 proteins and genes Proteins 0.000 abstract description 5
- 102000004169 proteins and genes Human genes 0.000 abstract description 5
- 239000007787 solid Substances 0.000 abstract description 5
- 235000013305 food Nutrition 0.000 abstract description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 3
- 239000012296 anti-solvent Substances 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 77
- 235000013310 margarine Nutrition 0.000 description 21
- 239000003264 margarine Substances 0.000 description 19
- 239000002245 particle Substances 0.000 description 13
- 241000209140 Triticum Species 0.000 description 8
- 235000021307 Triticum Nutrition 0.000 description 8
- 239000006071 cream Substances 0.000 description 7
- 241000209219 Hordeum Species 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000011246 composite particle Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- 108010061711 Gliadin Proteins 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 239000003995 emulsifying agent Substances 0.000 description 3
- 239000000194 fatty acid Substances 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 150000002632 lipids Chemical class 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 235000008429 bread Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001055 chewing effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 108060006613 prolamin Proteins 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- ONIBWKKTOPOVIA-BYPYZUCNSA-N L-Proline Chemical compound OC(=O)[C@@H]1CCCN1 ONIBWKKTOPOVIA-BYPYZUCNSA-N 0.000 description 1
- KZSNJWFQEVHDMF-BYPYZUCNSA-N L-valine Chemical compound CC(C)[C@H](N)C(O)=O KZSNJWFQEVHDMF-BYPYZUCNSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- ONIBWKKTOPOVIA-UHFFFAOYSA-N Proline Natural products OC(=O)C1CCCN1 ONIBWKKTOPOVIA-UHFFFAOYSA-N 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- KZSNJWFQEVHDMF-UHFFFAOYSA-N Valine Natural products CC(C)C(N)C(O)=O KZSNJWFQEVHDMF-UHFFFAOYSA-N 0.000 description 1
- 229930003779 Vitamin B12 Natural products 0.000 description 1
- 229920002494 Zein Polymers 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000015895 biscuits Nutrition 0.000 description 1
- 235000014121 butter Nutrition 0.000 description 1
- 235000012970 cakes Nutrition 0.000 description 1
- -1 cationic polysaccharide Chemical class 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- FDJOLVPMNUYSCM-WZHZPDAFSA-L cobalt(3+);[(2r,3s,4r,5s)-5-(5,6-dimethylbenzimidazol-1-yl)-4-hydroxy-2-(hydroxymethyl)oxolan-3-yl] [(2r)-1-[3-[(1r,2r,3r,4z,7s,9z,12s,13s,14z,17s,18s,19r)-2,13,18-tris(2-amino-2-oxoethyl)-7,12,17-tris(3-amino-3-oxopropyl)-3,5,8,8,13,15,18,19-octamethyl-2 Chemical compound [Co+3].N#[C-].N([C@@H]([C@]1(C)[N-]\C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C(\C)/C1=N/C([C@H]([C@@]1(CC(N)=O)C)CCC(N)=O)=C\C1=N\C([C@H](C1(C)C)CCC(N)=O)=C/1C)[C@@H]2CC(N)=O)=C\1[C@]2(C)CCC(=O)NC[C@@H](C)OP([O-])(=O)O[C@H]1[C@@H](O)[C@@H](N2C3=CC(C)=C(C)C=C3N=C2)O[C@@H]1CO FDJOLVPMNUYSCM-WZHZPDAFSA-L 0.000 description 1
- 239000003240 coconut oil Substances 0.000 description 1
- 235000019864 coconut oil Nutrition 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000009881 electrostatic interaction Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 235000019866 hydrogenated palm kernel oil Nutrition 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 238000005528 milk analysis Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000031787 nutrient reservoir activity Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000518 rheometry Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000010692 trans-unsaturated fatty acids Nutrition 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
- 239000004474 valine Substances 0.000 description 1
- 235000019163 vitamin B12 Nutrition 0.000 description 1
- 239000011715 vitamin B12 Substances 0.000 description 1
- 239000005019 zein Substances 0.000 description 1
- 229940093612 zein Drugs 0.000 description 1
Images
Landscapes
- Colloid Chemistry (AREA)
Abstract
The invention discloses a preparation method of a hordein-chitosan high internal phase Pickering emulsion. Extracting hordein by adopting an Osborne method, mixing the hordein with acetic acid-dissolved chitosan by using an anti-solvent method, adjusting the pH value, adding oil phases with different mass ratios, and preparing hordein-chitosan stable high internal phase Pickering emulsion. The Pickering emulsion can load oil phase as high as 85% under the condition of 2% of water-phase protein concentration, has high stability, and does not generate the phenomena of elutriation and demulsification in the storage period of 28 days. The high internal phase Pickering emulsion shows a gel state when the oil phase is 75%, realizes the conversion from liquid oil to solid oil, and has wide application prospect in food.
Description
Technical Field
The invention belongs to the technical field of food, and particularly relates to preparation of a hordein-chitosan stable high internal phase Pickering emulsion and application thereof in margarine replacement
Background
The development of margarine has been long-standing and has been widely used in the food industry as a substitute for natural cream, such as cake, biscuit, bread and the like, due to its excellent price and large yield. The common oil used in margarine existing in the market is partially hydrogenated palm kernel oil or partially hydrogenated coconut oil, and the partial hydrogenation of the oil can generate a large amount of trans-fatty acid. Excessive intake of trans fatty acids can increase the incidence of cardiovascular diseases and induce asthma, tumor, type II diabetes and other diseases. In recent years, people gradually know the health problems of margarine along with the increase of health consciousness, so that the development of a zero-trans fatty acid cream product has potential market value.
The Pickering emulsion is stable emulsion taking solid particles as an emulsifier, has the advantages of economy, high stability, environmental friendliness, higher resistance to coalescence and the like compared with the traditional emulsion, and is rapidly researched and developed in nearly two decades. The high internal phase Pickering emulsion refers to a type of Pickering emulsion with an internal phase coefficient of more than 74 percent, can endow liquid lipid with plasticity, has a texture and plasticity similar to margarine, realizes the conversion of the liquid lipid to solid lipid, and is a potential margarine substitute.
Emulsions are thermally unstable systems and have several disadvantages in use. In order to enhance the stability of emulsions, studies have been made to improve the hydrophobicity of colloidal particles by complexing polysaccharides with proteins through hydrophobic or electrostatic interactions, which enhance interfacial properties of the colloidal particles such as electrostatic repulsion, steric hindrance, and the like.
Hordein is an important storage protein in barley, is generally enriched in beer lees and wastes after barley starch processing, contains high proportion of hydrophobic amino acids such as proline, valine and the like, and therefore, the hordein is insoluble in water and has strong hydrophobic activity. The related scholars have developed studies on Pickering emulsions based on hordein nanoparticles, and Sareh bookani prepared W1/O/W2 multiple Pickering emulsions with physically modified hordein nanoparticles, which had good stability and good encapsulation efficiency for vitamin B12, demonstrating that hordein nanoparticles have potential as green emulsifiers.
Chitosan is a cationic polysaccharide, and chitosan particles can be used as a green emulsifier due to hydrophobicity/hydrophilicity, biocompatibility and degradability, and researches show that chitosan is used for forming composite particles with some prolamines, such as zein and wheat prolamin, and the results show that the composite particles have good Pickering emulsion stabilizer performance. To date, there has been no report on the preparation of high internal phase Pickering emulsions using hordein/chitosan composite particles.
Therefore, in order to effectively utilize hordein, a resource, it is important to prepare a stable high internal phase Pickering emulsion.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides a preparation method of a hordein-chitosan stable high internal phase Pickering emulsion, which is simple to operate, good in stability and good in application prospect.
Specifically, the invention provides the following technical scheme:
a method of preparing a hordein-chitosan stabilized high internal phase Pickering emulsion comprising the steps of:
(1) Preparation of hordeins: grinding barley kernels into powder, adding n-hexane, continuously stirring, centrifuging to obtain a precipitate, sequentially adding deionized water and a NaCl solution into the precipitate, centrifuging and collecting the precipitate. Finally, adding an ethanol water solution into the precipitate, stirring, centrifuging, collecting supernatant, performing rotary evaporation to remove ethanol, and freeze-drying the sample to obtain a powder sample;
(2) Preparing a hordein stock solution: dissolving the hordein obtained in the step (1) in an ethanol water solution, and heating and stirring to obtain a hordein stock solution;
(3) Preparing a chitosan stock solution: dissolving chitosan in acetic acid solution, heating and stirring to obtain chitosan stock solution;
(4) And (3) adding the hordein solution obtained in the step (2) into the chitosan solution obtained in the step (3) for mixing, performing rotary evaporation to remove ethanol, adding distilled water to complement the volume, adjusting the pH of a system to 4.0 by using an acid-base regulator, and performing ultrasonic treatment to obtain the hordein-chitosan nanoparticle stabilizer.
(5) Preparation of hordein-chitosan high internal phase Pickering emulsion: mixing the hordein-chitosan nanoparticle stabilizer with the oil phase and shearing to obtain the hordein-chitosan high internal phase Pickering emulsion.
To further achieve the object of the present invention, preferably, in step (1), hordeins are prepared by the following method:
grinding barley into powder, adding n-hexane at a material-to-liquid ratio of 1:5 (m: v), continuously stirring at 25 deg.C for 2h, centrifuging at 4000 Xg at 25 deg.C for 5min with high speed refrigerated centrifuge, and removing supernatant; adding deionized water into the precipitate according to the ratio of 1:6 (m: v), continuously stirring for 30min, centrifuging at 4000 Xg for 5min, and removing the supernatant; 0.1M NaCl solution was added to the above precipitate in a ratio of 1:6 (M: v), continuously stirred for 30min, centrifuged at 4000 Xg for 5min, and the supernatant was discarded. And finally, adding 75% (v/v) ethanol aqueous solution into the precipitate according to the ratio of the material to the liquid of 1.
Further, in the step (2), the volume concentration of the ethanol aqueous solution is 75%, the heating temperature is 45 ℃, the stirring speed is 600rpm, and the mass percentage concentration of the obtained hordein stock solution is 4%.
Further, in the step (3), the mass percentage concentration of the acetic acid solution is 0.1%, the heating temperature is 45 ℃, the stirring speed is 600rpm, and the mass percentage concentration of the obtained chitosan stock solution is 0.16%.
Further, in the step (4), the volume ratio of the hordein solution to the chitosan solution is 1:1, the mixing conditions were magnetic stirring, and the stirring rate was 600rpm.
Further, in the step (4), the pH regulator is 0.1M sodium hydroxide solution or hydrochloric acid solution.
Further, the ultrasonic power in the step (4) is 150W, and the time is 5min.
Further, in the step (5), the oil phase is soybean oil, and the volume ratio of the hordein-chitosan nanoparticle stabilizer to the oil phase is 1:3 to 1:5.7.
preferably, the mixing shear is at 9000rpm for 1min.
Compared with the prior art, the invention has the beneficial effects that:
(1) The hordein-chitosan stable high internal phase Pickering emulsion can load up to 85% of oil phase under the concentration of 2% of water phase protein, has high emulsion stability, and does not generate an emulsion separation phenomenon and an emulsion breaking phenomenon in a 28-day storage period.
(2) The hordein-chitosan stable high internal phase Pickering emulsion shows a gel state when the oil phase is 75%, realizes the conversion from liquid oil to solid oil, and has wide application prospect in food.
(3) The hordein-chitosan stable high internal phase Pickering emulsion has no peculiar smell, does not contain trans fatty acid, is similar to the state of artificial butter sold in the market, has better plasticity, and can meet the requirements of consumers on cream products.
(4) The preparation method has the advantages of low cost, simple preparation process, common equipment and suitability for industrial production.
Drawings
FIG. 1 is a comparison of the appearance of the emulsion made according to the invention with a commercial margarine;
FIG. 2 shows the dispersion of the emulsion prepared by the present invention in different systems, the left is water phase and the right is oil phase;
FIG. 3 is a microscopic picture of the emulsion produced by the present invention and a commercial margarine;
FIG. 4 shows the rheological behaviour of the emulsion prepared according to the invention with a commercial margarine: apparent viscosity as a function of shear rate;
FIG. 5 shows the rheological behaviour of the emulsion prepared according to the invention with a commercial margarine: the storage modulus and loss modulus vary with angular frequency;
FIG. 6 shows the spreading characteristics of the emulsion prepared according to the invention with a commercial margarine.
Fig. 7 is an appearance diagram of a wheat gliadin-chitosan emulsion, the left is a freshly prepared emulsion, and the right is after standing for 1 h.
Detailed Description
The conception and the resulting technical effects of the present invention will be further described with reference to specific embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention. The method is a conventional method unless otherwise specified. The materials are commercially available from the open literature unless otherwise specified.
Example 1 preparation of hordeins
Preparation of hordeins: grinding barley into powder, adding n-hexane at a material-to-liquid ratio of 1:5 (m: v), continuously stirring at 25 deg.C for 2h, centrifuging at 25 deg.C at 4000 Xg for 5min with high speed refrigerated centrifuge, and removing supernatant; adding deionized water into the precipitate according to the ratio of material to liquid of 1:6 (m: v), continuously stirring for 30min, centrifuging at 4000 Xg for 5min, and removing supernatant; 0.1M NaCl solution was added to the above precipitate in a ratio of 1:6 (M: v), continuously stirred for 30min, centrifuged at 4000 Xg for 5min, and the supernatant was discarded. And finally, adding 75% (v/v) ethanol aqueous solution into the precipitate according to the ratio of the material to the liquid of 1.
Example 2 preparation of hordein-chitosan nanoparticle stabilizer
Preparation method of hordein-chitosan nanoparticle stabilizer
The preparation method comprises the following steps:
s1, preparing a hordein stock solution: dissolving the hordein freeze-dried powder in 75% ethanol water solution, and magnetically stirring at 45 ℃ to obtain 4% hordein stock solution.
S2, preparing a chitosan stock solution: dissolving chitosan in 0.1% acetic acid solution, and magnetically stirring at 45 deg.C to obtain 0.16% chitosan stock solution.
S3, mixing the hordein stock solution obtained in the step S1 at a stirring speed of 600rpm in a proportion of 1: adding the chitosan stock solution obtained in the step S2 at the ratio of 1 (v/v), rotationally evaporating at 45 ℃ to remove ethanol, adding distilled water to make up the volume, and adjusting the pH of the system to 4.0 by using 0.1M sodium hydroxide solution or hydrochloric acid solution. Then, the dispersion was treated with an ultrasonic disruptor at 150W for 5min to obtain a hordein-chitosan nanoparticle dispersion.
Example 3 preparation of high internal phase Pickering emulsion
1. The preparation method of the Pickering emulsion with phi =75% comprises the following steps:
the hordein-chitosan nanoparticle stabilizer obtained in example 2 and soybean oil (the volume ratio of the hordein-chitosan nanoparticle stabilizer to the soybean oil is 1:3) were mixed and sheared, the shearing speed was 9000rpm, and the shearing time was 1min, to obtain a uniform milky semisolid, i.e., a hordein-chitosan nanoparticle-stabilized high internal phase Pickering emulsion, in which the volume fraction of the oil phase in the emulsion was 75%.
This example gives an emulsion with an oil phase ratio of 75%, the appearance picture is shown in fig. 1, the surface is smooth and flat, the texture is uniform and free of impurities, and the color is softer and milky compared with commercial cream, and has a certain plasticity.
2. The preparation method of the Pickering emulsion with phi =80% comprises the following steps: similarly, when the hordein-chitosan nanoparticle stabilizer is mixed with soybean oil and sheared, the volume ratio of the hordein-chitosan nanoparticle stabilizer to the soybean oil is ensured to be 1:4.
this example gives an emulsion with an oil phase ratio of 80%, the appearance picture is shown in fig. 1, the surface is smooth and flat, the texture is uniform and free of impurities, and compared with commercial cream), the color is softer and milky white with certain plasticity.
3. The preparation method of the Pickering emulsion with phi =85% comprises the following steps: similarly, when the hordein-chitosan nanoparticle stabilizer is mixed with soybean oil and sheared, the volume ratio of the hordein-chitosan nanoparticle stabilizer to the soybean oil is ensured to be 3:17.
this example gives an emulsion with an oil phase ratio of 85%, the appearance picture is shown in fig. 1, the surface is smooth and flat, the texture is uniform and free of impurities, and compared with commercial cream, the color is softer and milky white with a certain plasticity.
Example 4 high internal phase Pickering emulsion Performance testing
(1) Type of high internal phase Pickering emulsion
The high internal phase Pickering emulsion prepared in example 3 was dropped into the oil phase or the water phase, respectively, and the dispersion was observed. If dispersed homogeneously in the oil phase, the emulsion is of the water-in-oil (W/O) type, whereas if dispersed homogeneously in the aqueous phase, the emulsion is of the oil-in-water (O/W) type. Fig. 2 shows the dispersion of the Pickering emulsion prepared by the present invention in different systems, and it can be observed that the emulsion is uniformly distributed in water and remains the original state in oil, thus it can be known that the Pickering emulsion stabilized by hordein-chitosan nanoparticles belongs to oil-in-water (O/W) type emulsion.
(2) Particle size determination of high internal phase Pickering emulsions
The average droplet size and the particle size distribution of the high internal phase Pickering emulsion prepared in example 3 were measured using a laser particle size analyzer (LS 230, beckmann coulter co., usa), and the particle size of the oil droplets of the emulsion was expressed by a volume-weighted average diameter (D4, 3).
TABLE 1 particle size of high internal phase Pickering emulsion
Note: phi =75% indicates that the volume ratio of the aqueous phase to the oil phase is 1:3; phi =80% indicates that the volume ratio of the aqueous phase to the oil phase is 1:4; phi =85% indicates that the volume ratio of the water phase to the oil phase is 3:17.
with the increase of the volume fraction of the oil phase from 75% to 85%, the particle size of the Pickering emulsion is significantly increased from 23.99 μm to 28.15 μm, and under the condition of a certain total volume of the emulsion, the increase of the volume fraction of the oil phase leads to the increase of the interface area, and the number of protein particles adsorbed on the oil-water interface is relatively reduced, so that the oil/water interface tension cannot be effectively reduced, and oil drops with larger particle size are formed.
(3) Microstructure observation of high internal phase Pickering emulsion
The high internal phase Pickering emulsion prepared in example 3 was diluted 10 times with deionized water, and the microstructure of the emulsion was observed by taking an image of the emulsion droplets with an optical microscope equipped with a camera. The microscopic image is shown in fig. 3, and oil drops in the emulsion are mutually closely contacted, do not aggregate, are uniformly distributed, have approximate sizes, and have regular structures and are spherical.
(4) Stability study of high internal phase Pickering emulsions
The high internal phase Pickering prepared in example 3 was left at 4 ℃ for 28 days and the milk analysis index CI% was recorded. The milk separation index formula is as follows:
in the formula: hs is the height of the subnatant, ht is the total height of the emulsion.
TABLE 2 creaming index before and after storage of high internal phase Pickering emulsion
The results show that no creaming occurs during storage of the high internal phase Pickering prepared by the invention, which indicates that the emulsion with high oil phase ratio can keep good stability during long-term storage, because the gel network structure of the Pickering emulsion is enhanced with the increase of the oil phase ratio, the creaming does not easily occur, and the emulsion has stronger emulsification stability.
(5) Rheology study of high internal phase Pickering emulsions
The rheological properties of the emulsions were determined using a rheometer. The frequency sweep oscillation frequency range is 0.1-100 rad/s, and the change of the storage modulus and the loss modulus along with the frequency is recorded. The flow sweep shear rate was set at 0.1 to 100s-1, giving a change in the apparent viscosity of the emulsion.
Results as shown in fig. 4 and 5, the storage modulus G' of all Pickering emulsions was consistently higher than the loss modulus G "throughout the sweep frequency range, indicating that the emulsions have an elastic gel structure, which may be formed due to a dense particle layer at the oil/water interface, and a 3D network structure formed in the continuous phase. Furthermore, G' and G "of all Pickering emulsions increased with increasing frequency, suggesting that non-covalent interactions may be the primary reason for the formation of an elastic-like gel structure by the emulsions. At the same time, the higher the G' and G "values of the Pickering emulsions with higher oil contents, which is probably due to the fact that the oil droplets in the emulsions with higher oil contents are closely linked to each other, thereby increasing their resistance to stress. Pickering emulsions of different oil phase fractions all have the typical characteristics of non-Newtonian fluids, i.e., apparent viscosity decreases with increasing shear rate, as indicated by shear thinning. Furthermore, the viscosity increases with increasing volume fraction of the oil phase, probably due to the close connection between oil droplets embedded in the 3D network structure at higher volume fraction of the oil phase, resulting in the formation of a solid-like emulsion, forming a stronger 3D network structure. Exhibit similar rheological behavior compared to commercial margarines.
(6) Exploration on texture characteristics of high internal phase Pickering emulsion
The texture properties of the high internal phase Pickering emulsion (phi =75%, 80%, 85%) and the commercial margarine and wheat pure soluble protein built emulsions were measured at 25 ℃ using a physical property analyzer using a compression mode with a measurement rate of 1mm/s, compression to 50% of the original height, relaxation time of 5s, and trigger force of 0.5N.
Meanwhile, in order to detect the quality and structure characteristics of the hordein-chitosan high internal phase Pickering emulsion as a margarine substitute, a sample was prepared by the same preparation method by using the hordein-chitosan high internal phase Pickering emulsion as a comparative example, and further comparison was performed. 75% hordein, 80% hordein, 85% hordein, respectively, are 75%, 80%, 85% by volume of the oil phase in example 3; 75% of wheat gliadin and 80% of wheat gliadin are Pickering emulsion with 75% and 80% of oil phase volume fraction respectively.
Comparative example preparation method: dissolving 0.5g of wheat gliadin in 20ml of ethanol solution with volume concentration of 70%; dissolving 0.025g chitosan in 50ml acetic acid solution with volume concentration of 1%, pouring the alcohol solution into the acetic acid solution while homogenizing, homogenizing at 6000rpm for 4min, rotary evaporating at 40 deg.C and 0.1Mpa vacuum degree for 20min, adjusting pH to 5.0, mixing 2ml and 2.5ml solutions with 8ml and 7.5ml corn oil, shearing, and emulsifying to obtain wheat prolamin emulsion with shearing emulsifying speed of 5000rpm for 1min. The procedure for the addition of the oil phase to the emulsion was the same as in example 3, except that the volume fraction of the oil phase added was different.
TABLE 3 texture characteristics of high internal phase Pickering emulsions and margarines
The volume fraction of the oil phase has a significant influence on both the hardness and the viscous force. Hardness, which may reflect the force required to compress the sample between the tongue and jaw, increases with increasing oil phase volume due to the higher internal phase fraction of the emulsion gel network, which is more dense. Hardness is one of the most important factors affecting the mouthfeel of cream, and emulsion hardness values close to margarine, indicating that it has a creamy mouthfeel. The viscosity also increased with increasing oil phase volume, probably due to increasing oil phase fraction leading to an increase in the viscosity of the emulsion, consistent with the results of the rheological properties. The cohesiveness is the characteristic that the sample resists damage and is firmly adhered to maintain the integrity of the product in the chewing process, and reflects the internal binding force of the sample, and the data in the table 3 show that the cohesiveness of the emulsion is smaller in absolute numerical value, so that the chewing is facilitated.
The high internal phase Pickering emulsion has good stability and plasticity, and the solid property of the high internal phase Pickering emulsion can enable the high internal phase Pickering emulsion to be applied to a substitute of margarine. As shown in figure 6, the high internal phase Pickering emulsion has an appearance similar to margarine, has uniform, fine and smooth texture without impurities, presents softer milky color, and can be uniformly spread on the surface of bread like margarine.
As can be seen from the data in Table 3, the various indices of the emulsion more closely approached margarine as the volume fraction of the oil phase increased. The wheat gliadin-chitosan composite particles can stabilize emulsion with 80% of oil phase volume fraction at the highest, when the oil phase volume fraction is 85%, the emulsion is demulsified, high flocculation is shown after the emulsion is placed for 1h, and phase separation is observed (figure 7). The hordein-chitosan emulsion with the oil phase volume fraction of 85 percent basically has no significant difference in the texture characteristics of margarine, and is obviously superior to the hordein-chitosan emulsion.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Although the present invention has been described in detail hereinabove by way of general description, specific embodiments and experiments, it is not limited to the above-described embodiments, but may be modified or improved on the basis of the present invention, as will be apparent to those skilled in the art. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A preparation method of hordein-chitosan high internal phase Pickering emulsion is characterized by comprising the following steps:
(1) Preparation of hordeins: grinding barley kernels into powder, adding n-hexane, continuously stirring, centrifuging to obtain a precipitate, sequentially adding deionized water and a NaCl solution into the precipitate, centrifuging to collect the precipitate, finally adding an ethanol water solution into the precipitate, stirring, centrifuging to collect a supernatant, performing rotary evaporation to remove ethanol, and freeze-drying a sample to obtain a powder sample;
(2) Preparing a hordein stock solution: dissolving the hordein obtained in the step (1) in an ethanol water solution, and heating and stirring to obtain a hordein stock solution;
(3) Preparing a chitosan stock solution: dissolving chitosan in acetic acid solution, heating and stirring to obtain chitosan stock solution;
(4) Adding the hordein solution obtained in the step (2) into the chitosan solution obtained in the step (3) for mixing, performing rotary evaporation to remove ethanol, adding distilled water to complement the volume, adjusting the pH of a system to 4.0 by using an acid-base regulator, and performing ultrasonic treatment to obtain a hordein-chitosan nanoparticle stabilizer;
(5) Preparation of hordein-chitosan high internal phase Pickering emulsion: mixing the hordein-chitosan nanoparticle stabilizer with the oil phase and shearing to obtain the hordein-chitosan high internal phase Pickering emulsion.
2. The method according to claim 1, wherein the preparation of hordeins in step (1) comprises:
grinding barley into powder, adding n-hexane at a material-to-liquid ratio of 1:5 (m: v), continuously stirring at 25 deg.C for 2h, centrifuging at 25 deg.C at 4000 Xg for 5min with high speed refrigerated centrifuge, and removing supernatant; adding deionized water into the precipitate according to the ratio of material to liquid of 1:6 (m: v), continuously stirring for 30min, centrifuging at 4000 Xg for 5min, and removing supernatant; adding 0.1M NaCl solution into the precipitate according to the ratio of 1:6 (M: v), continuously stirring for 30min, centrifuging for 5min at 4000 Xg, removing the supernatant, finally adding 75% (v/v) ethanol aqueous solution into the precipitate according to the ratio of 1.
3. The preparation method according to claim 1, wherein in the step (2), the ethanol aqueous solution has a volume concentration of 75%, a heating temperature of 45 ℃, a stirring speed of 600rpm, and a mass percentage concentration of the obtained hordein stock solution of 4%.
4. The preparation method according to claim 1, wherein in the step (3), the mass percentage concentration of the acetic acid solution is 0.1%, the heating temperature is 45 ℃, the stirring speed is 600rpm, and the mass percentage concentration of the obtained chitosan stock solution is 0.16%.
5. The preparation method according to claim 1, wherein in the step (4), the volume ratio of the hordein solution to the chitosan solution is 1:1, the mixing conditions were magnetic stirring, and the stirring rate was 600rpm.
6. The preparation method according to claim 1, wherein, in the step (4), the pH adjusting agent is a 0.1M sodium hydroxide solution or a hydrochloric acid solution.
7. The preparation method according to claim 1, wherein the ultrasonic power in the step (4) is 150W and the time is 5min.
8. The preparation method according to claim 1, wherein, in the step (5), the oil phase is soybean oil, and the volume ratio of the hordein-chitosan nanoparticle stabilizer to the oil phase is 1:3 to 1:5.7.
9. the production method according to claim 1, wherein in the step (5), the mixing shear rate is 9000rpm for 1min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210896299.8A CN115715588A (en) | 2022-07-27 | 2022-07-27 | Preparation method and application of hordein-chitosan high internal phase Pickering emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210896299.8A CN115715588A (en) | 2022-07-27 | 2022-07-27 | Preparation method and application of hordein-chitosan high internal phase Pickering emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115715588A true CN115715588A (en) | 2023-02-28 |
Family
ID=85253888
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210896299.8A Pending CN115715588A (en) | 2022-07-27 | 2022-07-27 | Preparation method and application of hordein-chitosan high internal phase Pickering emulsion |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115715588A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105853358A (en) * | 2016-05-30 | 2016-08-17 | 华南理工大学 | Preparation method of edible protein stable Pickering emulsion |
| CN105968825A (en) * | 2016-05-30 | 2016-09-28 | 华南理工大学 | Method for preparing cellular material from biological cross-linking agent crosslinked protein |
| CN106046803A (en) * | 2016-05-30 | 2016-10-26 | 华南理工大学 | Preparation method of edible protein porous material |
| CN106578335A (en) * | 2016-11-16 | 2017-04-26 | 华南理工大学 | High internal phase gelatinous wheat gliadin Pickering emulsion and preparation method thereof |
| CN108464428A (en) * | 2018-03-21 | 2018-08-31 | 华南理工大学 | A kind of method that ultrasound prepares stable gel shape wheat gliadin Pickering lotions |
| CN110122876A (en) * | 2019-05-31 | 2019-08-16 | 广州大学 | A kind of preparation method of gliadin-chitosan condensation product |
| CN114015094A (en) * | 2022-01-07 | 2022-02-08 | 中国农业大学 | High-strength hordein chitosan composite membrane and preparation method thereof |
-
2022
- 2022-07-27 CN CN202210896299.8A patent/CN115715588A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105853358A (en) * | 2016-05-30 | 2016-08-17 | 华南理工大学 | Preparation method of edible protein stable Pickering emulsion |
| CN105968825A (en) * | 2016-05-30 | 2016-09-28 | 华南理工大学 | Method for preparing cellular material from biological cross-linking agent crosslinked protein |
| CN106046803A (en) * | 2016-05-30 | 2016-10-26 | 华南理工大学 | Preparation method of edible protein porous material |
| CN106578335A (en) * | 2016-11-16 | 2017-04-26 | 华南理工大学 | High internal phase gelatinous wheat gliadin Pickering emulsion and preparation method thereof |
| CN108464428A (en) * | 2018-03-21 | 2018-08-31 | 华南理工大学 | A kind of method that ultrasound prepares stable gel shape wheat gliadin Pickering lotions |
| CN110122876A (en) * | 2019-05-31 | 2019-08-16 | 广州大学 | A kind of preparation method of gliadin-chitosan condensation product |
| CN114015094A (en) * | 2022-01-07 | 2022-02-08 | 中国农业大学 | High-strength hordein chitosan composite membrane and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| FEIFAN LI，等: "Preparation and characterization of pickering emulsion stabilized by hordein-chitosan complex particles" * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tang et al. | Stability and rheology of canola protein isolate-stabilized concentrated oil-in-water emulsions | |
| Patel | Alternative routes to oil structuring | |
| Hayati et al. | Droplet characterization and stability of soybean oil/palm kernel olein O/W emulsions with the presence of selected polysaccharides | |
| Zhao et al. | Effect of regenerated cellulose fiber on the properties and microstructure of emulsion model system from meat batters | |
| Patel et al. | Biopolymer-based structuring of liquid oil into soft solids and oleogels using water-continuous emulsions as templates | |
| Alizadeh et al. | Characterization of sodium caseinate/Hydroxypropyl methylcellulose concentrated emulsions: Effect of mixing ratio, concentration and wax addition | |
| Kim et al. | Preparation of multiple emulsions based on thermodynamic incompatibility of heat-denatured whey protein and pectin solutions | |
| CN111163859B (en) | Process for producing water-soluble or water-dispersible fine particles, use of the particles, and method of use of the particles | |
| US20080044543A1 (en) | Stabilized emulsions, methods of preparation, and related reduced fat foods | |
| Kim et al. | Nature of protein-protein interactions during the gelation of canola protein isolate networks | |
| Alavi et al. | Complexation of nanofibrillated egg white protein and low methoxy pectin improves microstructure, stability, and rheology of oil-in-water emulsions | |
| EP1998627B1 (en) | A solid product comprising oil-droplets | |
| Sirvente et al. | Structuring and functionalization of dispersions containing egg yolk, plasma and granules induced by mechanical treatments | |
| Li et al. | Studies of phase separation in soluble rice protein/different polysaccharides mixed systems | |
| CN114190443A (en) | Method for preparing oleogel from protein gel | |
| CN116138346A (en) | Novel fat substitute 3D printing vegetable protein-based emulsion gel, and preparation method and application thereof | |
| Kavya et al. | Pectin emulsions and emulgels: Bridging the correlation between rheology and microstructure | |
| Fasinu et al. | Influence of selected physicochemical factors on the stability of emulsions stabilized by Bambara groundnut flour and starch | |
| CN113875978B (en) | A high internal phase Pickering emulsion prepared from camellia oil and tea cake extract | |
| Li et al. | Effects of sinapine on structure, rheology, stability, and antioxidant properties of protein-based capillary bridging oleogels | |
| Kasprzak et al. | Effects of fibre addition and processing on the stability, rheology and in vitro gastric digestion of whey protein-xanthan gum stabilised emulsions with high oil phase | |
| CN115715588A (en) | Preparation method and application of hordein-chitosan high internal phase Pickering emulsion | |
| Cai et al. | Emulsifying and whipping properties of mixing polysaccharide dispersions: effect of ratio between insoluble soybean fiber and hydroxypropyl methylcellulose | |
| CN111685220A (en) | Method for producing chicken liver protein powder with good emulsifying property | |
| Wei et al. | Roles of NaCl in Enhancing the Stability of Water-in-Oil High Internal Phase Emulsions |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20230228 |