CN114015108A - Crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material, preparation method and application - Google Patents
Crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material, preparation method and application Download PDFInfo
- Publication number
- CN114015108A CN114015108A CN202111457881.6A CN202111457881A CN114015108A CN 114015108 A CN114015108 A CN 114015108A CN 202111457881 A CN202111457881 A CN 202111457881A CN 114015108 A CN114015108 A CN 114015108A
- Authority
- CN
- China
- Prior art keywords
- effervescent
- crude tea
- tea extract
- chitosan oligosaccharide
- nanoparticle
- 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.)
- Granted
Links
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Abstract
The invention relates to the technical field of active substance processing and delivery, in particular to a crude tea extract/chitosan oligosaccharide nanoparticle effervescent paste material, a preparation method and application. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material is prepared from an effervescent agent, a plastic agent, a non-ionic surfactant, a wall material and a core material by adopting a specific preparation method. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream and the preparation method are provided aiming at the defects of high energy consumption, long time, equipment requirement and organic solvent use in the field of nano material preparation, the technical requirements of simple and quick operation and low energy input are realized, the popularization and the use of nano materials in production practice and daily life are promoted, and a new scheme is provided for nano delivery of hydrophobic substances.
Description
Technical Field
The invention relates to the technical field of active substance processing and delivery, in particular to a crude tea extract/chitosan oligosaccharide nanoparticle effervescent paste material, a preparation method and application.
Background
Compared to the general size, the nanoscale materials have various advantages, such as larger specific surface area, higher loading capacity, better bioassability, and the like. In the fields of food, medicine, biology and the like, the nano-composite has been widely researched and applied in the aspects of food preservation, activity and drug delivery, supported enzyme catalysis and the like.
The current preparation methods of nanomaterials (including nanoparticles, nanoliposomes, nanofilaments, etc.) are mainly based on two types of methods: firstly, the formation of the nano-composite is promoted by means of the shearing effect brought by high-speed stirring or homogenization depending on the input of external mechanical energy, and the method is mainly used for preparing polysaccharide-based (such as chitosan oligosaccharide) or inorganic (such as gold and silver) nano-composite; secondly, the anti-solvent method is used to produce nanoparticles according to the solubility difference of raw materials in different solvents, and the method is commonly used to produce protein-based nanoparticles, especially Zein (Zein) and wheat Gliadin (Gliadin) based nanoparticles.
The technical means are flexible and have wide applicability, and are widely adopted. However, the high-speed shearing method has high requirements on equipment and takes a long time, and generally requires a homogenizing and stirring device to process a sample for tens of minutes or even hours, and the use of the high-speed homogenizing device also brings a certain potential safety hazard. The antisolvent method requires a rotary evaporation treatment of the nanodispersion system using an organic solvent, which causes environmental burden. The existence of the above disadvantages limits the further application and popularization of the nano technology, and therefore, the development of a simple, rapid, safe and low-cost nano material preparation technology is urgently needed.
Effervescence has been used as a drug delivery and dispersion means for hundreds of years, and representative effervescent products such as vitamin C effervescent tablets, fruity effervescent beverages, drug effervescent tablets (such as aspirin effervescent tablets) and the like are still available in the market at present. Specifically, the effervescent agent is prepared by mixing an acidic substance and a basic substance represented by a carbonic acid or bicarbonate salt, and enters an aqueous solution environment to increase the reaction rate and promote the release of chemical energy, while CO is released2The movement of the bubbles in the solution provides a homogeneous-like mixing effect for the components in the system. Therefore, the effervescence has great potential in the field of colloid dispersion as a mild, rapid and safe means.
Although the effervescent technology is well applied to the dispersion of drinks and medicines, effervescent products are generally sold by taking solid powder as a carrier, and some products are sold by tabletting effervescent powder into tablets, and effervescent products taking liquid or paste as a carrier are not marketed.
Likewise, there has been no report to date on the application of the effervescent technique to nanomaterial preparation. The reason is that the nano material has high requirement on the uniformity of the system in the preparation process, and each component in the multi-component nano particles taking biological macromolecules as the material needs to form a uniform and stable dispersion system (an anti-solvent method) under the intervention of the outside or make the molecules fully contact (homogenizing and stirring) so as to fully exert the interaction (such as electrostatic force and hydrogen bonds) between the molecules and in the molecules, thereby forming particles with relatively balanced particle size distribution rather than aggregates of a single component or insoluble aggregates formed by growing a plurality of particles. The solubility of biological macromolecules represented by polysaccharide and protein is different, and a uniform dispersion system is difficult to form under the drive of effervescence only by replacing a dispersion means so as to create an environment for intermolecular self-assembly; and the effervescence reaction rate is fast, and the mixed state of tens of minutes can not be maintained, which is the main obstacle of the direct application of the effervescence technology to the preparation of nanometer materials.
Disclosure of Invention
The invention relates to a preparation method of hydrophobic substance-loaded effervescent cream, and particularly provides a crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material, a preparation method and application; aiming at the defects of high energy consumption, long time, equipment requirements and use of organic solvents in the field of nano material preparation, the invention provides a method for quickly preparing a crude tea extract/chitosan oligosaccharide nano particle effervescent paste material based on an effervescent means, so as to realize the technical requirements of simple and quick operation and low energy input, promote the popularization and use of nano materials in production practice and daily life, provide a new scheme for nano delivery of hydrophobic substances, and solve the problems in the prior art.
One of the technical schemes adopted by the invention is as follows:
a crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material is prepared from the following components in parts by weight:
530 parts of effervescent agent 310, 450 parts of plastic agent 150, 0-100 parts of nonionic surfactant, 30-180 parts of wall material and 0-25 parts of core material;
the effervescent agent comprises an acidic component and an alkaline substance component, wherein the acidic component accounts for 250 parts by weight, and the alkaline substance component accounts for 280 parts by weight;
the wall material is prepared from 0-80 parts of chitosan oligosaccharide and 30-100 parts of crude tea extract.
Further, the weight ratio of the crude tea extract to the chitosan is not less than 7:3, or the weight ratio of the crude tea extract to the chitosan is 1: 1.
Further, the deacetylation degree of the chitosan oligosaccharide is more than or equal to 80 percent; the crude tea extract is prepared by purifying crude tea through a water extraction and alcohol precipitation method.
Further, the raw tea includes raw tea stem and tea leaves.
Further, the alkaline material component is a carbonate or bicarbonate based alkaline material component.
Further, the water purification and precipitation method comprises the following operation steps:
(1) cleaning crude tea, grinding, placing in ethanol solution, stirring and soaking at 25-40 deg.C for 20-40min for pre-decolorizing treatment, wherein the weight volume ratio of crude tea and ethanol is 15-25% (w/v);
(2) repeatedly filtering, drying, extracting with deionized water at 75-85 deg.C for 60-90min, and repeating twice;
(3) centrifuging to remove insoluble contaminants, concentrating the supernatant to appropriate concentration, adding ethanol to precipitate polysaccharide, and adding ethanol to 80% (v/v); then, separating the precipitate, dissolving the precipitate in water, and repeating the alcohol precipitation step at least twice;
(4) washing the obtained precipitate with anhydrous ethanol, acetone and diethyl ether in sequence to remove small molecules, and repeating the washing twice; re-dissolving the precipitate in water, removing polyphenol with crosslinked polyvinylpyrrolidone, and lyophilizing to obtain crude tea extract powder.
Further, the mass concentration of the ethanol solution in the step (1) of the water purification and precipitation method is 60-80%.
Further, the mass concentration of the ethanol solution in the step (3) of the water purification and precipitation method is 60-80%.
Further, in the step (4) of the water purification and precipitation method, the concentration of the precipitate re-dissolved in water is 25-35 mg/mL; the concentration of the cross-linked polyvinylpyrrolidone is 6-10 mg/mL.
Further, the step (2) of the water purification and precipitation method is repeatedly filtered for 10-12 times; and (4) centrifuging for 10min under the centrifugal condition of 5000rpm in the step (3).
Further, the acid component is one or more of malic acid, tartaric acid and citric acid; the alkaline substance component is sodium carbonate and/or sodium bicarbonate.
Further, the plasticizer is one or more of polyethylene glycol, glycerol and sorbitol ester; the non-ionic surfactant is monoglyceride, tween or span; the core material is allyl isothiocyanate, eugenol or other hydrophobic active substances.
The second technical scheme adopted by the invention is as follows:
a method for preparing the crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream comprises the following operation steps:
s1: pulverizing effervescent and wall material, grinding, sieving, drying and storing;
s2: rapidly drying the crude tea extract, chitosan oligosaccharide and effervescent agent for use;
s3: preparing paste carrier raw materials in parts by weight: mixing a plasticizer and a nonionic surfactant, and homogenizing at 3000-8000rpm for 3-5min at high speed to prepare an unloaded paste carrier, wherein the paste is easy to extrude and can be molded from the application viewpoint;
s4: adding the effervescent agent and the wall material powder into the no-load paste carrier of S3, adding the core material, and manually stirring for 3-5min until the paste and the powder are primarily mixed uniformly; and continuing homogenizing for 10-30min by the homogenizer to obtain the nanoparticle effervescent cream.
Further, the mesh sieved in the step S1 is not less than 40 meshes; the core material of the step S4 is allyl isothiocyanate, eugenol or other hydrophobic active substances.
The third technical scheme adopted by the invention is as follows:
the preparation method and the application of the prepared crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream in preparing foods or medicines loaded with different types of core materials.
The invention has the beneficial effects that:
compared with a high-speed shearing method for inputting mechanical energy from the outside, the crude tea extract/chitosan oligosaccharide nano particle effervescent cream and the preparation method thereof greatly reduce energy consumption in technical aspect. In the assembling process of the nano particles, chemical energy is quickly released by the reaction of acid and alkali in an aqueous solution, and the chemical energy is used as a fundamental energy source in the process; the acid reacts with carbonate or bicarbonate quickly and releases to move in the solution systemCO of2The bubbles are assembled in the process to play a role in mixing and homogenizing, a high-rotation-speed shearing method is replaced to a certain extent, and the nano particles are prepared in a shorter time. In addition, when the nano particle effervescent cream is used for preparing nano particles, the prepared effervescent cream is only required to be added into water, other equipment or auxiliary reagents are not required, the preparation process is greatly simplified, and the further development and popularization of the nano technology are facilitated.
In terms of raw materials, the invention uses the crude old tea leaves as a source of crude tea extract rich in tea polysaccharide and also contains substances such as tea polyphenol, and the physiological activities of the tea polysaccharide and the tea polyphenol are widely studied internationally and proved to have the functions of assisting blood sugar reduction and antioxidation respectively. Further, no nano material using tea polysaccharide as a wall material raw material is published at present. China is the first tea planting country and the first producing country in the world, and a large amount of crude old tea and tea residue waste are generated in agricultural picking and industrial production of tea beverages.
In the aspect of action, the preparation method has wide application prospect and can be suitable for preparing various products such as nano particle effervescent paste food, medicines and the like wrapping different core materials. Moreover, no effervescent cream product is reported at present, and the invention provides a new idea.
Drawings
FIG. 1 is a distribution diagram of the particle size of nanoparticles obtained by effervescence of the effervescent cream prepared in the comparative examples 1 and 2 in water according to the examples 1 and 2 of the present invention;
FIG. 2 is a morphology chart of nanoparticles under a transmission electron microscope under no-load and example 1 loading AITC conditions;
FIG. 3 is a photograph of the Tyndall effect exhibited by unloaded and AITC-loaded nanoparticles of example 1;
FIG. 4 is a diagram showing the appearance of the effervescent cream prepared in example 1 of the present invention filled into a small tube;
wherein, fig. 2(a) is a morphology of unloaded nanoparticles under a transmission electron microscope, fig. 2(b) is a morphology of nanoparticles under a transmission electron microscope under a loading condition of example 1, and fig. 2(c) is a morphology of nanoparticles with a scale for adjusting a wall material ratio of comparative example 2; FIG. 3(a) is a photograph of a Tyndall effect of comparative example 1 of unloaded particles, and FIG. 3(b) is a photograph of the Tyndall effect exhibited by nanoparticles of example 1 loaded with AITC;
FIG. 1 results were measured using Malvern Zetasizer NanoZS 90; FIG. 2 the results are shown in the data of magnification and acceleration voltage using a JEM-1200EX transmission electron microscope.
Detailed Description
In order to clearly explain the technical features of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings.
All materials used in the specific examples are conventional materials used in the art and are commercially available and consistent with the general understanding of those skilled in the art.
Example 1
A preparation method of crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream loaded with Allyl Isothiocyanate (AITC) comprises the following steps:
s1: respectively taking 70 parts of crude tea extract rich in tea polysaccharide as wall material, 30 parts of chitosan oligosaccharide, 180 parts of citric acid as acid and alkali in the effervescent agent and 280 parts of sodium bicarbonate solid, crushing, grinding until no obvious large particles exist, sieving until the mesh size is more than or equal to 40 meshes, and drying and storing for later use;
s2: drying the crude tea extract in the S1, the chitosan oligosaccharide, the citric acid and the sodium bicarbonate in a freeze dryer for 24 hours, wherein the samples are dried as much as possible to ensure the stability of the paste during storage;
s3: mixing PEG-600 which is liquid at normal temperature and PEG-800 which is waxy solid at normal temperature to prepare proper carrier viscosity and the addition amount of the co-emulsifier, wherein the addition amount of the PEG-600 is 382 parts, and the addition amount of the PEG-800 is 38 parts; homogenizing the PEG mixture at 4000rpm for 5min to obtain an unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in S2 into the empty-load paste carrier obtained in S3, finally adding 10 parts of core material AITC, and manually stirring for 3min until the paste and the powder are initially mixed uniformly; and homogenizing the whole paste for 15min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
In step S1, the crude tea extract is prepared in advance, and the preparation steps are:
(1) cleaning and grinding the crude tea, putting the crude tea into an ethanol solution with the mass fraction of 80%, stirring and soaking the crude tea at the temperature of 30 ℃ for 30min, and decolorizing the crude tea before stirring and soaking; wherein the mass of the crude tea accounts for 16.7% (w/v) of the volume of the ethanol solution;
(2) repeatedly filtering for 10 times; drying, extracting with deionized water at 84 deg.C for 70min, and repeating twice;
(3) centrifugation at 5000rpm for 10min was used to remove insoluble contaminants; concentrating the supernatant to a suitable concentration by rotary evaporation, adding ethanol to the concentrated solution to precipitate polysaccharide until the concentration of the added ethanol is 80% (v/v); then separating the precipitate, dissolving the precipitate in water, and repeating the alcohol precipitation step at least twice;
(4) washing the obtained precipitate with anhydrous ethanol, acetone and diethyl ether in sequence to remove small molecules, and repeating the washing twice; redissolving the precipitate in water again at a concentration of 25mg/mL, removing polyphenols with crosslinked polyvinylpyrrolidone at a concentration of 8mg/mL, and lyophilizing to obtain crude tea extract powder.
Example 2
A preparation method of Vitamin E (VE) -loaded crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream comprises the following steps:
s1: respectively taking 80 parts of crude tea extract rich in tea polysaccharide as wall material, 20 parts of chitosan oligosaccharide, 180 parts of citric acid as acid and alkali in the effervescent agent and 280 parts of sodium bicarbonate solid, crushing, grinding until no obvious large particles exist, sieving until the mesh size is more than or equal to 40 meshes, and drying and storing for later use;
s2: drying the crude tea extract in the S1, chitosan oligosaccharide, citric acid and sodium bicarbonate in a freeze dryer for 48h, wherein the samples should be dried as much as possible to ensure the stability of the paste during storage;
s3: mixing PEG-600 which is liquid at normal temperature and PEG-800 which is waxy solid at normal temperature to prepare proper carrier viscosity and the addition amount of the co-emulsifier, wherein the addition amount of the PEG-600 is 382 parts, and the addition amount of the PEG-800 is 38 parts; homogenizing the PEG mixture at 5000rpm for 3min to obtain unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in the step S2 into the no-load paste carrier obtained in the step S3, finally adding 10 parts of core material VE, and manually stirring for 5min until the paste and the powder are initially mixed uniformly; and homogenizing the whole paste for 15min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
The extraction procedure of the crude tea extract used was the same as in example 1.
Example 3
A preparation method of crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream loaded with Allyl Isothiocyanate (AITC) comprises the following steps:
s1: respectively taking 50 parts of crude tea extract rich in tea polysaccharide as wall material, 10 parts of chitosan oligosaccharide, 150 parts of tartaric acid as acid and alkali in the effervescent agent and 160 parts of sodium carbonate solid, crushing, grinding until no obvious large particles exist, sieving, and drying and storing for later use, wherein the mesh size is not less than 40 meshes;
s2: drying the crude tea extract, chitosan oligosaccharide, tartaric acid and sodium carbonate in the S1 in a freeze dryer for 24h, wherein the samples should be dried as much as possible to ensure the stability of the paste during storage;
s3: mixing and blending 150 parts of glycerol and 100 parts of tween; homogenizing the mixture at 6000rpm for 4min to obtain unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in S2 into the empty-load paste carrier obtained in S3, finally adding 10 parts of core material AITC, and manually stirring for 4min until the paste and the powder are primarily mixed uniformly; and homogenizing the whole paste for 20min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
In step S1, the crude tea extract is prepared in advance, and the preparation steps are:
(1) cleaning and grinding the crude tea, putting the crude tea into an ethanol solution with the mass fraction of 70%, stirring and soaking the crude tea at 25 ℃ for 40min, and decolorizing; wherein the weight of the crude tea accounts for 20% (w/v) of the volume of the ethanol solution;
(2) repeatedly filtering for 12 times; drying, extracting with deionized water at 75 deg.C for 90min, and repeating twice;
(3) centrifugation at 5000rpm for 10min was used to remove insoluble contaminants; concentrating the supernatant to a suitable concentration by rotary evaporation, adding ethanol to the concentrated solution to precipitate polysaccharide until the concentration of the added ethanol is 80% (v/v); then separating the precipitate, dissolving the precipitate in water, and repeating the alcohol precipitation step at least twice;
(4) washing the obtained precipitate with anhydrous ethanol, acetone and diethyl ether in sequence to remove small molecules, and repeating the washing twice; redissolving the precipitate in water again at a concentration of 30mg/mL, removing polyphenols with crosslinked polyvinylpyrrolidone at a concentration of 6mg/mL, and lyophilizing to obtain crude tea extract powder.
Example 4
A crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream loaded with Eugenol (Eugenol) is prepared by the following steps:
s1: respectively taking 90 parts of crude tea extract rich in tea polysaccharide as wall material, 50 parts of chitosan oligosaccharide, 230 parts of malic acid as acid and alkali in the effervescent agent and 280 parts of sodium bicarbonate solid, crushing, grinding until no obvious large particles exist, sieving until the mesh size is more than or equal to 40 meshes, and drying and storing for later use;
s2: drying the crude tea extract, chitosan oligosaccharide, malic acid and sodium bicarbonate in S1 in a freeze dryer for 24h, wherein the sample should be dried as much as possible to ensure the stability of the paste during storage;
s3: mixing 350 parts of sorbitol ester and 70 parts of span, and blending; homogenizing the mixture at 3000rpm for 5min to obtain unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in S2 into the empty-load paste carrier obtained in S3, finally adding 10 parts of core material Eugenol (Eugenol), and manually stirring for 5min until the paste and the powder are primarily mixed uniformly; and homogenizing the whole paste for 25min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
In step S1, the crude tea extract is prepared in advance, and the preparation steps are:
(1) cleaning and grinding the crude tea, putting the crude tea into an ethanol solution with the mass fraction of 60%, stirring and soaking the crude tea at 40 ℃ for 20min, and decolorizing the crude tea before stirring; wherein the weight of the crude tea accounts for 25% (w/v) of the volume of the ethanol solution;
(2) repeatedly filtering for 10 times; drying, extracting with deionized water at 85 deg.C for 60min, and repeating twice;
(3) centrifugation at 5000rpm for 10min was used to remove insoluble contaminants; concentrating the supernatant to a suitable concentration by rotary evaporation, adding ethanol to the concentrated solution to precipitate polysaccharide until the concentration of the added ethanol is 80% (v/v); then separating the precipitate, dissolving the precipitate in water, and repeating the alcohol precipitation step at least twice;
(4) washing the obtained precipitate with anhydrous ethanol, acetone and diethyl ether in sequence to remove small molecules, and repeating the washing twice; redissolving the precipitate in water again at a concentration of 35mg/mL, removing polyphenols with crosslinked polyvinylpyrrolidone at a concentration of 10mg/mL, and lyophilizing to obtain crude tea extract powder. The extraction procedure of the crude tea extract used was the same as in example 3.
Comparative example 1
The preparation method of the idle-load nano particle effervescent cream comprises the following steps:
s1: respectively taking 90 parts of crude tea extract rich in tea polysaccharide as wall material, 10 parts of chitosan oligosaccharide, 180 parts of citric acid as acid and alkali in the effervescent agent and 280 parts of sodium bicarbonate solid, crushing, grinding until no obvious large particles exist, sieving until the mesh size is more than or equal to 40 meshes, and drying and storing for later use;
s2: drying the crude tea extract in the S1, the chitosan oligosaccharide, the citric acid and the sodium bicarbonate in a freeze dryer for 24 hours, wherein the samples are dried as much as possible to ensure the stability of the paste during storage;
s3: mixing PEG-600 which is liquid at normal temperature and PEG-800 which is waxy solid at normal temperature to prepare proper carrier viscosity and the addition amount of the co-emulsifier, wherein the addition amount of the PEG-600 is 382 parts, and the addition amount of the PEG-800 is 38 parts; homogenizing the PEG mixture at 4000rpm for 5min to obtain an unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in S2 into the empty-load paste carrier obtained in S3, adding no load, and manually stirring for 3min until the paste and the powder are primarily mixed; and homogenizing the whole paste for 15min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
The crude tea extract and extraction procedure used were the same as in example 1.
Comparative example 2
The preparation method of the nanoparticle effervescent cream loaded with Allyl Isothiocyanate (AITC) for adjusting the proportion of wall material components comprises the following steps:
s1: respectively taking 50 parts of crude tea extract rich in tea polysaccharide as wall material, 50 parts of chitosan oligosaccharide, 180 parts of citric acid as acid and alkali in the effervescent agent and 280 parts of sodium bicarbonate solid, crushing, grinding until no obvious large particles exist, sieving until the mesh size is more than or equal to 40 meshes, and drying and storing for later use;
s2: drying the crude tea extract in the S1, the chitosan oligosaccharide, the citric acid and the sodium bicarbonate in a freeze dryer for 24 hours, wherein the samples are dried as much as possible to ensure the stability of the paste during storage;
s3: mixing PEG-600 which is liquid at normal temperature and PEG-800 which is waxy solid at normal temperature to prepare proper carrier viscosity and the addition amount of the co-emulsifier, wherein the addition amount of the PEG-600 is 382 parts, and the addition amount of the PEG-800 is 38 parts; homogenizing the PEG mixture at 4000rpm for 5min to obtain an unloaded paste carrier;
s4: adding the effervescent agent and wall material powder obtained in S2 into the empty-load paste carrier obtained in S3, finally adding 10 parts of core material AITC, and manually stirring for 3min until the paste and the powder are initially mixed uniformly; and homogenizing the whole paste for 15min by using a homogenizer to obtain uniform and stable effervescent paste which can be used for preparing nano particles.
The crude tea extract and extraction procedure used were the same as in example 1.
Characterization and determination procedure for examples and comparative examples:
1. measurement of particle diameter of nanoparticles
The effervescent pastes prepared in the examples and comparative examples of the present invention were added to 100mL of water for effervescence, and the nanoparticle encapsulation efficiency was immediately measured using high performance liquid chromatography. At the time of measurement, 10-fold dilution was performed using double distilled water, and then measurement was performed using a dynamic light scattering method using a zetasizer nanozs90 laser particle sizer, and the particle size and PDI thereof were recorded, and the results are shown in fig. 1.
As can be seen from FIG. 1, the AITC-loaded nanoparticles in example 1 and the VE-loaded nanoparticles in example 2 had Z-Average of 436.9nm and 456.3nm, respectively, and their PDI of 0.293 and 0.259. It can be seen that the nanoparticles carrying AITC can reach the nano-grade particle size, and the lower PDI value indicates that the particle size distribution of the nanoparticles obtained by the two methods of effervescence is more uniform. However, the particle size of the nanoparticles is greatly changed with further increase of the addition amount of the chitosan oligosaccharide, and the particle distribution tends to be scattered. In contrast, the no-load nanoparticles of comparative example 1 have a reduced particle size due to the absence of the active substance, and have a Z-Average of 364.9nm and a PDI of 0.292. The nanoparticles from the effervescent paste described in comparative example 2 were studied and the Z-Average was 563.3nm, the PDI value was 0.576, and the difference in PDI values indicates that the particle size of the nanoparticles in comparative example 2 was increased by the increased proportion of chitooligosaccharide, and the same change was also found in the particle size distribution diagram (FIG. 1), in which there are two distinct peaks in the particle size distribution diagram of comparative example 2, while the other nanoparticles tend to be more uniform.
2. Determination of the nanoparticle effervescence time
3g of the effervescent cream loaded with AITC of example 1 was added to 100mL of water, and the effervescent time was measured, and the end point of effervescence was defined as the point at which no new foam was formed on the water surface. The test was repeated 5 times. The results are shown in table 1, and it can be seen that the effervescence process is completed within about 2min, compared with the traditional technology of which the treatment process is tens of minutes to hours, the preparation method provided by the invention has the obvious advantage of shorter time consumption.
Table 1 cream effervescence time data
3. Determination of nanoparticle morphology
The basic morphology of the resulting nanoparticles, loaded with AITC and unloaded with nanoparticles, was photographed using a scanning electron microscope (JEM-1200EX) at an accelerating voltage of 100 kV. As shown in fig. 2(a), the basic morphology of the unloaded nanoparticles described in comparative example 1 is uniform round globule shape, while in fig. 2(b) the basic morphology of the nanoparticles in example 1 is shown, the loaded nanoparticles are loaded with white spots on the basis of the round basic morphology, which indicates that the loaded nanoparticles formed are polynuclear nanoparticles and the essential oil components are embedded inside the nanoparticles. Fig. 2(c) shows that the nanoparticles obtained in comparative example 2 by changing the composition of the wall material and increasing the ratio of the chitosan oligosaccharide component in the wall material have a larger average particle size than those shown in fig. 2(a) and (b), and the particle size and morphology tend to be irregular, indicating that the degree of uniformity of the particles is relatively reduced, which is consistent with the broader peak width of the particle size distribution of the comparative example in fig. 1. However, white spots also appeared in the particles at the upper right corner in fig. 2(c), indicating that the essential oil was successfully embedded inside the particles. Therefore, when the technology is applied to the preparation of the nano particles composed of no-load, load and different wall material proportions, the obtained particles can form nano-scale particles although the distribution and the particle size are different, and the particles with load can be successfully embedded.
4. The resulting nanoparticle dispersions and appearance
Figure 3(a) shows the appearance of a dispersion of unloaded nanoparticles as described in comparative example 1 and figure 3(b) shows the appearance of loaded AITC nanoparticles as described in example 1, both pictures showing the typical tyndall effect. The fundamental characteristic of the tyndall effect is that a significant light path occurs when light passes through the dispersion, which can be used as a preliminary judgment for colloidal dispersions. As can be seen from the two pictures, the solution is clear and transparent, and a distinct red light path passes through the solution, which is the general characteristic of the Tyndall effect, and the system can be preliminarily judged to be a colloidal dispersion system. Due to the presence of tea polyphenol residues in the crude tea extract, the colloidal system exhibits a similar brown colour due to tea polyphenols after exposure to air.
Figure 4 shows the appearance of the effervescent paste prepared in example 1 of the present invention filled into plastic tubes.
The above-described embodiments should not be construed as limiting the scope of the invention, and any alternative modifications or alterations to the embodiments of the present invention will be apparent to those skilled in the art.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (9)
1. A crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material is characterized by being prepared from the following components in parts by weight:
530 parts of effervescent agent 310, 450 parts of plastic agent 150, 0-100 parts of nonionic surfactant, 30-180 parts of wall material and 0-25 parts of core material;
the effervescent agent comprises an acidic component and an alkaline substance component, wherein the acidic component accounts for 250 parts by weight, and the alkaline substance component accounts for 280 parts by weight;
the wall material is prepared from 0-80 parts of chitosan oligosaccharide and 30-100 parts of crude tea extract.
2. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material as claimed in claim 1, wherein the deacetylation degree of chitosan oligosaccharide is greater than or equal to 80%; the crude tea extract is prepared by purifying crude tea through a water extraction and alcohol precipitation method.
3. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material of claim 2, wherein the water purification precipitation method comprises the following steps:
(1) cleaning crude tea, grinding, placing in ethanol solution, stirring and soaking at 25-40 deg.C for 20-40min for pre-decolorizing treatment, wherein the weight volume ratio of crude tea and ethanol is 15-25% (w/v);
(2) repeatedly filtering, drying, extracting with deionized water at 75-85 deg.C for 60-90min, and repeating twice;
(3) centrifuging to remove insoluble contaminants, concentrating the supernatant to appropriate concentration, adding ethanol to precipitate polysaccharide, and adding ethanol to 80% (v/v); then, separating the precipitate, dissolving the precipitate in water, and repeating the alcohol precipitation step at least twice;
(4) washing the obtained precipitate with anhydrous ethanol, acetone and diethyl ether in sequence to remove small molecules, and repeating the washing twice; re-dissolving the precipitate in water, removing polyphenol with crosslinked polyvinylpyrrolidone, and lyophilizing to obtain crude tea extract powder.
4. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material of claim 1, wherein the acidic component is a combination of one or more of malic acid, tartaric acid, citric acid; the alkaline substance component is sodium carbonate and/or sodium bicarbonate.
5. The crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material of claim 1, wherein the plasticizer is a combination of one or more of polyethylene glycol, glycerin, sorbitol ester; the non-ionic surfactant is monoglyceride, tween or span; the core material is allyl isothiocyanate, eugenol or other hydrophobic active substances.
6. A process for preparing a crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material as claimed in any one of claims 1 to 5, comprising the following operative steps:
s1: pulverizing effervescent and wall material, grinding, sieving, drying and storing;
s2: rapidly drying the crude tea extract, chitosan oligosaccharide and effervescent agent for use;
s3: preparing paste carrier raw materials in parts by weight: mixing a plasticizer and a nonionic surfactant, and homogenizing at 3000-8000rpm for 3-5min to prepare an unloaded paste carrier;
s4: adding the effervescent agent and the wall material powder into the no-load paste carrier of S3, adding the core material, and manually stirring for 3-5min until the paste and the powder are primarily mixed uniformly; and continuing homogenizing for 10-30min by the homogenizer to obtain the nanoparticle effervescent cream.
7. The method for preparing the crude tea extract/chitosan oligosaccharide nanoparticle effervescent cream material according to claim 6, wherein the mesh sieved in step S1 is not less than 40 meshes; the core material of the step S4 is allyl isothiocyanate, eugenol or other hydrophobic active substances.
8. The preparation method of claim 6 or 7 and the use of the prepared crude tea extract/chitosan oligosaccharide nanoparticle effervescent paste material in the preparation of foods or medicines loaded with different types of core materials.
9. Use according to claim 8, wherein the core material is allyl isothiocyanate, eugenol or another hydrophobic active substance.
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