CN109864931B - Pickering emulsion stabilized by theabrownin and preparation method and application thereof - Google Patents
Pickering emulsion stabilized by theabrownin and preparation method and application thereof Download PDFInfo
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- CN109864931B CN109864931B CN201910101202.8A CN201910101202A CN109864931B CN 109864931 B CN109864931 B CN 109864931B CN 201910101202 A CN201910101202 A CN 201910101202A CN 109864931 B CN109864931 B CN 109864931B
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Abstract
The invention belongs to the technical field of materials, and discloses a Pickering emulsion stabilized by theabrownin, and a preparation method and application thereof. The method comprises the following steps: (1) extracting theabrownin; (2) and adjusting the pH of the theabrownin dispersion phase, mixing the theabrownin dispersion phase with the oil phase, and performing shearing homogenization and high-pressure homogenization to obtain the stable Pickering emulsion. The invention takes theabrownin as the Pickering stabilizer, has clean, green and healthy materials, and can be widely applied to the fields of food and medicine as a conveying carrier.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a Pickering emulsion stabilized by theabrownin, and a preparation method and application thereof.
Background
The Pickering emulsion is a novel emulsion with solid particles replacing the traditional surfactant to stabilize an emulsion system. Compared with the traditional emulsion, the Pickering emulsion does not need to use a surfactant, and has lower cost and small toxicity. At present, most of researches on stabilization of Pickering by solid particles are focused on inorganic or synthetic particles such as silicon dioxide, Janus particles, laponite clay and the like. Although these particles have a good ability to stabilize Pickering emulsion, the use of Pickering emulsion prepared using them in the fields of biomedicine, food, cosmetics, etc. is limited due to problems of safety, biocompatibility, etc. The Pickering emulsion stabilized by the particles of biological origin does not have the problem, and can be used for loading low-stability or fat-soluble nutrient and functional components, improving the texture of food and the like. It has therefore become a hotspot of current research to seek suitable particles of biological origin as stabilizers for Pickering emulsions.
According to the existing research, the Pickering emulsion stabilizer from biological sources mainly comprises polysaccharide, protein, lipid, flavonoid compounds, polysaccharide-protein compound and the like. Theabrownin is a complex of proteins, polysaccharides, polyphenol oxides, and the like. The emulsion has a large molecular weight, contains a large amount of hydroxyl, carboxyl, carbonyl, amino and other groups, has certain hydrophilicity and hydrophobicity, and has the capability of constructing Pickering emulsion. In addition, the compound is one of important active ingredients of black tea and black tea, has the functions of reducing blood fat, resisting oxidation, resisting fatigue, inhibiting bacteria and the like, can strengthen the health efficacy of the Pickering emulsion by using the compound as a stabilizer, and widens the application range of the Pickering emulsion.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention mainly aims to provide a preparation method of stable Pickering emulsion by using theabrownin; the method takes theabrownin as a Pickering stabilizer to prepare food-grade Pickering emulsion with strong stability.
The invention also aims to provide the Pickering emulsion prepared by the method.
The invention further aims to provide application of the Pickering emulsion.
The purpose of the invention is realized by the following technical scheme:
a preparation method of Pickering emulsion stabilized by theabrownin comprises the following steps:
(1) extracting theabrownin;
(2) preparing Pickering emulsion by taking theabrownin as a stabilizer;
the theabrownin extraction in the step (1) specifically comprises the following steps: soaking dry tea leaves in ethanol for 4-48 h to remove impurities, and adding water with the temperature of 25-100 ℃ into tea leaves, wherein the mass ratio of the dry tea leaves to the water is 1: 10-1: 250; then leaching for 2-120 min under the condition of water bath at 25-100 ℃ to obtain a tea extract, sequentially extracting for 1-5 times by using dichloromethane, extracting for 1-5 times by using ethyl acetate, extracting for 1-5 times by using n-butyl alcohol, concentrating a finally obtained water layer, adding ethanol to ensure that the volume percentage concentration of the ethanol is 50% -95%, and carrying out alcohol precipitation for 4-48 h; freeze drying, and storing at-20 deg.C to obtain theabrownin lyophilized powder.
The dry tea is black tea or black tea.
The mass ratio of the dry tea leaves to the water is 1: 25; the temperature of the water bath is 100 ℃; the leaching time is 60 min; the extraction times of the dichloromethane are 2 times; the extraction times of the ethyl acetate are 3 times; the number of n-butanol extractions is 4; the volume ratio of the dichloromethane, the ethyl acetate and the n-butanol to the water phase is 1: 1.
The preparation method for stabilizing Pickering emulsion by using theabrownin comprises the following steps: dissolving theabrownin freeze-dried powder by using water according to the mass percent of 0.5-6.0%, adding sodium azide with the mass fraction of 0.02%, adjusting the pH of a theabrownin dispersion phase to 2-11, adding an oil phase according to the oil-water volume ratio of 1: 9-6: 4, carrying out high-speed shearing homogenization at the speed of 10000-20000 r/min for 1-2 min, and carrying out high-pressure homogenization at the pressure of 40MPa for 1-3 times to obtain Pickering emulsion.
The oil phase is immiscible with water.
The addition amount of the theabrownin freeze-dried powder is 2% by mass; the pH value of the theabrownin dispersion phase is 8; the volume ratio of the oil to the water is 4: 6; the rotation speed of the high-speed shearing homogenization is 20000r/min, and the time is 2 min; the pressure of the high-pressure homogenization is 40MPa, and the homogenization times are 3 times.
A Pickering emulsion prepared according to the above preparation method.
The Pickering emulsion is applied to the fields of food, cosmetics and biomedicine.
The prepared Pickering emulsion is stored at room temperature (25-32 ℃), and is characterized every 7 days within 35 days. Measuring the particle size of the Pickering emulsion liquid drop by a laser light scattering technology, and evaluating the size of the Pickering emulsion liquid drop obtained by the invention; the Zeta potential of a Pickering emulsion system is measured by a laser Doppler velocity measurement technology, and the electrostatic stability of the Pickering emulsion obtained by the invention is evaluated; evaluating the standing stability of the Pickering emulsion obtained by the invention through photographing and recording the appearance; the microstructure of the Pickering emulsion was observed by an optical microscope to evaluate the stabilizing effect of the Pickering emulsion obtained in the present invention.
Compared with the prior art, the invention has the following advantages and beneficial effects:
according to the invention, a food-grade Pickering stabilizer is adopted, and theabrownin is used as Pickering particles to construct a green and healthy Pickering emulsion, so that the Pickering emulsion is endowed with the efficacy of theabrownin bioactive components, the application field of the Pickering emulsion is widened, and the application value of the Pickering emulsion is improved.
Drawings
FIG. 1 shows the effect of storage time on the particle size (A) and particle size distribution (B) of a theabrownin-Pickering emulsion droplet.
FIG. 2 shows the effect of storage time on Zeta potential of a theabrownin-Pickering emulsion system.
FIG. 3 is a graph of the effect of storage time on the appearance of a theabrownin-Pickering emulsion.
FIG. 4 is a graph of the effect of storage time on the microstructure of a theabrownin-Pickering emulsion.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the present invention is not limited thereto.
In order to make the purpose and technical scheme of the invention more clear, the invention is further explained in detail by taking Pu' er tea theabrownin of Yunnan large-leaf as a stabilizer for example. The equipment and the reagent used in the invention are all commonly used in the field. It should be understood that the examples described herein are for illustrative purposes only and are not intended to limit the present invention.
Example 1: a preparation method for stabilizing Pickering emulsion by using theabrownin and the prepared Pickering emulsion.
(1) Accurately weighing 40g of ground Pu 'er tea raw material, soaking Pu' er tea in absolute ethyl alcohol for 12h for impurity removal, adding 100 ℃ water into Pu 'er tea residues according to the material-liquid ratio (the dry tea mass (g) before soaking): the water mass (g)) of 1:25, then leaching for 60min under the condition of 100 ℃ water bath to obtain Pu' er tea extract, respectively extracting for 2, 3 and 4 times by using dichloromethane, ethyl acetate and n-butanol, concentrating the finally obtained water layer, adding ethanol to ensure that the volume percentage concentration of the ethanol is 85%, and carrying out 12h alcohol precipitation; freeze drying to obtain theabrownin freeze-dried powder for later use.
(2) Dissolving theabrownin with the mass fraction of 2.0% by using ultrapure water with a certain volume, adding sodium azide with the mass fraction of 0.02%, uniformly mixing, standing a tin foil paper overnight (12-14 h) in the dark, adding soybean oil according to the oil-water volume ratio of 4:6(20mL:30mL), shearing and homogenizing for 2min at 20000r/min, and homogenizing for 3 times at high pressure of 40MPa to obtain the theabrownin-Pickering emulsion (namely the Pickering emulsion stabilized by theabrownin). The emulsion is placed at room temperature (25-32 ℃), and the influence of the storage time within 35d on the particle size and the particle size distribution of the droplets of the theabrownin-Pickering emulsion is examined. As a result, as shown in FIG. 1, the particle size of the emulsion droplets was kept small within 35d, and the change of the particle size and the particle size distribution was small with the lapse of time, thus confirming that the emulsion had good stability.
Example 2: a Pickering emulsion is prepared from theabrownin as stabilizer.
The effect of the storage time of the theabrownin-Pickering emulsion obtained in example 1 within 35d on the electrostatic stability of the theabrownin-Pickering emulsion was examined. As shown in FIG. 2, the Zeta potential values of the emulsion are all higher than 45mV within 35d, and the Zeta potential changes slightly with the increase of time. It is generally considered that the strong electrostatic repulsion force exists when the Zeta potential value of the system reaches 30 mV. Thus, it was demonstrated that the emulsion system can maintain high electrostatic stability for 35 days.
Example 3: a Pickering emulsion is prepared from theabrownin as stabilizer.
The effect of the storage time of the theabrownin-Pickering emulsion obtained in example 1 within 35d on the appearance of the theabrownin-Pickering emulsion was examined. As a result, as shown in FIG. 3, the emulsion remained homogeneous after 14 days, but a small amount of water was precipitated from the lower part of the emulsion from 21 days, and the precipitated volume increased with time, but the precipitated volume was small in 35 days and the precipitated portion was not completely separated. The emulsion can keep good stability at room temperature within 7 days, and the stabilizing effect gradually decreases with the increase of time, but the stability within 35 days is still better.
Example 4: a Pickering emulsion is prepared from theabrownin as stabilizer.
The storage time of the theabrownin-Pickering emulsion obtained in example 1 within 35d was examined for the effect on the microstructure of the theabrownin-Pickering emulsion. As shown in FIG. 4, the emulsion droplets remained uniformly dispersed within 35d, and the droplet size did not change significantly, demonstrating good stability and dispersibility of the emulsion.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. A preparation method of Pickering emulsion stabilized by theabrownin is characterized by comprising the following steps:
(1) the method for extracting theabrownin specifically comprises the following steps: soaking dry tea leaves in ethanol for 4-48 h to remove impurities, and adding water with the temperature of 25-100 ℃ into tea leaves, wherein the mass ratio of the dry tea leaves to the water is 1: 10-1: 250; then leaching for 2-120 min under the condition of water bath at 25-100 ℃ to obtain a tea extract, sequentially extracting for 1-5 times by using dichloromethane, extracting for 1-5 times by using ethyl acetate, extracting for 1-5 times by using n-butyl alcohol, concentrating a finally obtained water layer, adding ethanol to ensure that the volume percentage concentration of the ethanol is 50% -95%, and carrying out alcohol precipitation for 4-48 h; freeze drying, and storing at-20 deg.C to obtain theabrownin lyophilized powder;
(2) the Pickering emulsion is prepared by taking theabrownin as a stabilizer, and specifically comprises the following steps: dissolving theabrownin freeze-dried powder by using water according to the mass percent of 0.5-6.0%, adding sodium azide with the mass fraction of 0.02%, adjusting the pH of a theabrownin dispersion phase to 2-11, adding an oil phase according to the oil-water volume ratio of 1: 9-6: 4, carrying out high-speed shearing homogenization at the speed of 10000-20000 r/min for 1-2 min, and carrying out high-pressure homogenization at the pressure of 40MPa for 1-3 times to obtain Pickering emulsion.
2. The method of claim 1, wherein the Pickering emulsion stabilized with theabrownin is prepared by: the dry tea leaves in the step (1) are black tea or black tea.
3. The method of claim 1, wherein the Pickering emulsion stabilized with theabrownin is prepared by: the mass ratio of the dry tea leaves to the water in the step (1) is 1: 25; the temperature of the water bath is 100 ℃; the leaching time is 60 min; the extraction times of the dichloromethane are 2 times; the extraction times of the ethyl acetate are 3 times; the number of n-butanol extractions is 4; the volume ratio of the dichloromethane, the ethyl acetate and the n-butanol to the water phase is 1: 1.
4. The method of claim 1, wherein the Pickering emulsion stabilized with theabrownin is prepared by: and (3) the oil phase is not soluble in water in the step (2).
5. The method of claim 1, wherein the Pickering emulsion stabilized with theabrownin is prepared by: the addition amount of the theabrownin freeze-dried powder in the step (2) is 2% by mass; the pH value of the theabrownin dispersion phase is 8; the volume ratio of the oil to the water is 4: 6; the rotation speed of the high-speed shearing homogenization is 20000r/min, and the time is 2 min; the pressure of the high-pressure homogenization is 40MPa, and the homogenization times are 3 times.
6. A Pickering emulsion prepared according to the preparation method of any one of claims 1 to 5.
7. Use of Pickering emulsion according to claim 6 in the food, cosmetic and biomedical fields.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001437A (en) * | 2014-05-09 | 2014-08-27 | 中国科学院过程工程研究所 | Pickering emulsion with uniform particle size, and preparation method and application thereof |
| CN104082452A (en) * | 2014-07-04 | 2014-10-08 | 杭州艺福堂茶业有限公司 | Rough extraction method and fine extraction method of theabrownine |
| CN107792837A (en) * | 2017-08-31 | 2018-03-13 | 华南农业大学 | The nanometer selenium for preparing the method for nanometer selenium using camellia plant nanometer aggregation and being prepared |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104001437A (en) * | 2014-05-09 | 2014-08-27 | 中国科学院过程工程研究所 | Pickering emulsion with uniform particle size, and preparation method and application thereof |
| CN104082452A (en) * | 2014-07-04 | 2014-10-08 | 杭州艺福堂茶业有限公司 | Rough extraction method and fine extraction method of theabrownine |
| CN107792837A (en) * | 2017-08-31 | 2018-03-13 | 华南农业大学 | The nanometer selenium for preparing the method for nanometer selenium using camellia plant nanometer aggregation and being prepared |
Non-Patent Citations (3)
| Title |
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| "Pickering乳状液及其在油田中的应用";陈馥等;《精细化工》;20140115;第31卷(第1期);第1-6页 * |
| "Spontaneously Assembled Nano-aggregates in Clear Green Tea";xiaorong lin et al;《journal of agricultural and food chemistry》;20170415;第3757-3766页 * |
| "茶褐素的提取纯化与生理功效研究进展";王伟伟等;《食品安全质量检测学报》;20150430;第6卷(第4期);第1187-1192页 * |
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