CN114106582A - Bio-based microcapsule emulsion wrapping natural pigment and preparation method thereof - Google Patents
Bio-based microcapsule emulsion wrapping natural pigment and preparation method thereof Download PDFInfo
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- CN114106582A CN114106582A CN202111435194.4A CN202111435194A CN114106582A CN 114106582 A CN114106582 A CN 114106582A CN 202111435194 A CN202111435194 A CN 202111435194A CN 114106582 A CN114106582 A CN 114106582A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0001—Post-treatment of organic pigments or dyes
- C09B67/0004—Coated particulate pigments or dyes
Abstract
The invention relates to the field of package printing, and discloses a bio-based microcapsule emulsion wrapping natural pigments and a preparation method thereof. The invention adopts a protein and polysaccharide system, self-assembles the protein and polysaccharide system to form bio-based composite nanoparticles by adjusting the pH value, and combines the Pickering emulsion technology to prepare the microcapsule wrapping natural pigment. The introduction of calcium chloride in the system is helpful to adjust the concentration of water phase ions to enable more nano particles to be adsorbed on an oil-water interface to form a stable emulsion, and on the other hand, the introduction of calcium ions can form an ionic cross-linking structure on the surface of the microcapsule, so that the stability of the microcapsule is further improved, the damage of external factors such as light, oxygen and the like to natural pigments is effectively inhibited, and the color protection effect is achieved. The product is safe and has no toxic or side effect, can be used for preparing edible ink, and has great application prospect in the fields of packaging and printing of foods, medicines and the like.
Description
Technical Field
The invention relates to the field of package printing, in particular to a bio-based microcapsule emulsion wrapping natural pigments and a preparation method thereof.
Background
At present, pigments used for packaging printing are mainly synthetic pigments, and the pigments are attached to the surface of a packaging material by dyeing the packaging material or mixing the pigments into ink and printing color pictures and texts. The synthetic pigment has toxic and side effects of carcinogenesis, teratogenesis and the like, so the synthetic pigment is not suitable for the field of food packaging. In contrast, natural pigments are various in types, natural in color, safe and non-toxic, even have nutritive value and a pharmacotherapeutic effect, and are very suitable for the field of food packaging. However, the natural pigment is extracted from organisms, the original physiological environment is removed, and the natural pigment is easily affected by external factors such as light, oxygen and the like to fade and discolor in the use process, so that the coloring effect of a packaged product is affected, and the use of the natural pigment is severely restricted.
Microencapsulation of natural pigments is one of the effective means for color protection. By adopting the wall material to wrap the natural pigment, the possibility of the natural pigment acting with external factors such as light, oxygen and the like can be effectively reduced, thereby reducing the probability of structural damage and playing a role in color protection. The raw materials of the wall material are natural, safe and nontoxic as natural pigments, so that the application requirement in the field of food packaging can be met. Therefore, how to select wall material raw materials meeting the requirements and prepare the microcapsule with good stability to realize good wrapping protection of the natural pigment is a key problem in the application process of the natural pigment.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a safe and nontoxic natural pigment-coated bio-based microcapsule emulsion and a preparation method thereof.
(II) technical scheme
In order to realize the purpose of the invention, the following technical scheme is adopted:
the bio-based microcapsule emulsion for wrapping natural pigments is characterized by comprising the following raw materials in parts by weight: 10-40 parts of bio-based composite nanoparticle aqueous solution, 10-40 parts of natural pigment and 0.02-0.08 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.02-0.1 part of polysaccharide, 0.1-0.4 part of protein, 0.1-2 parts of pH regulator and 12-50 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.02-0.1 part by weight of polysaccharide into 2-10 parts by weight of deionized water, adding 0.1-0.4 part by weight of protein into 10-40 parts by weight of deionized water, stirring and dissolving to respectively obtain a polysaccharide aqueous solution and a protein aqueous solution, mixing the two aqueous solutions, adding 0.1-2 parts by weight of pH regulator, and performing ultrasonic dispersion at an ultrasonic power of 300-600W and a temperature of-5 ℃ for 15-30 min to obtain a bio-based composite nanoparticle aqueous solution.
The natural pigment is one of monascus pigment, curcumin, beta-carotene and lycopene.
The polysaccharide is one or more of sodium alginate, chitosan, pectin and sodium carboxymethylcellulose.
The protein is one or two of lysozyme and gelatin.
The pH regulator is 1mol/L hydrochloric acid aqueous solution or sodium hydroxide aqueous solution
The preparation method of the bio-based microcapsule emulsion wrapping the natural pigment is prepared by the following steps:
adding 0.02-0.08 weight part of calcium chloride into 10-40 weight parts of bio-based composite nanoparticle aqueous solution for complete dissolution, dropwise adding 10-40 weight parts of natural pigment while performing ultrasonic treatment at-5 ℃ under the ultrasonic power of 300-600W, and performing ultrasonic treatment for 15-30 min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the natural pigment.
(III) advantageous effects
Compared with the prior art, the invention provides a bio-based microcapsule emulsion wrapping natural pigments and a preparation method thereof, and the bio-based microcapsule emulsion has the following beneficial effects: the invention adopts a protein and polysaccharide system, self-assembles the protein and polysaccharide system to form bio-based composite nanoparticles by adjusting the pH value, and combines the Pickering emulsion technology to prepare the microcapsule wrapping natural pigment. The introduction of calcium chloride in the system is helpful to adjust the concentration of water phase ions to enable more nanoparticles to be adsorbed on an oil-water interface to form a stable emulsion, and on the other hand, the introduction of calcium ions can form an ionic cross-linking structure on the surface of the microcapsule, so that the stability of the microcapsule can be further improved, the damage of external factors such as light, oxygen and the like to natural pigments can be effectively inhibited, and the color protection effect is achieved. The product is safe and has no toxic or side effect, can be used for preparing edible ink, and has great application prospect in the fields of packaging and printing of foods, medicines and the like.
Drawings
FIG. 1 is a graph showing the particle size and particle size distribution of bio-based composite nanoparticles in example 1 of the present invention;
FIG. 2 is a graph showing the particle size and particle size distribution of bio-based composite nanoparticles in example 2 of the present invention;
FIG. 3 is a graph showing the particle size and particle size distribution of bio-based composite nanoparticles in example 3 of the present invention;
FIG. 4 is a graph showing the particle size and particle size distribution of bio-based composite nanoparticles in example 4 of the present invention;
FIG. 5 is a graph showing the particle size and particle size distribution of bio-based composite nanoparticles in example 5 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention are described in further detail below.
The particle size and the particle size distribution of the bio-based composite nanoparticles are measured by a Malvern ZETASIZER 3000HAS nanometer laser particle sizer.
The ZETA potential of the bio-based microcapsule emulsion coated with natural pigments was measured using a Malvern ZETASIZER 3000HAS nano laser particle sizer.
Stability testing of natural pigment-encapsulated bio-based microcapsules:
and centrifuging, washing and drying the bio-based microcapsule emulsion wrapping the natural pigment to obtain bio-based microcapsule powder wrapping the natural pigment. Dissolving natural pigment and natural pigment-coated bio-based microcapsule powder in ethanol to obtain natural pigment ethanol solution and natural pigment-coated bio-based microcapsule ethanol solution
And respectively scanning ethanol, a natural pigment ethanol solution and a bio-based microcapsule ethanol solution wrapping the natural pigment by using a UV-Probe2550 double-beam ultraviolet spectrometer, wherein the scanning range is 200-800 nm, the maximum absorption wavelength of the natural pigment is used as a measurement wavelength, the absorbance of the indoor natural light for 10 days is measured, and the residual rate of the absorbance is respectively calculated according to the following formula and is used as a stability index.
Wherein A% is the residual rate of absorbance, AoAbsorbance of the sample before light irradiation, AxIs the absorbance of the sample after illumination.
Example 1:
a bio-based microcapsule emulsion wrapping monascus pigment comprises the following raw materials in parts by weight: 10 parts of bio-based composite nanoparticle aqueous solution, 10 parts of monascus pigment and 0.02 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.1 part of sodium alginate, 0.1 part of lysozyme, 0.1 part of 1mol/L hydrochloric acid aqueous solution and 20 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.1 part by weight of sodium alginate into 10 parts by weight of deionized water and adding 0.1 part by weight of lysozyme into 10 parts by weight of deionized water, stirring and dissolving to respectively obtain a sodium alginate aqueous solution and a lysozyme aqueous solution, mixing the two aqueous solutions, adding 0.1 part by weight of 1mol/L hydrochloric acid aqueous solution, and performing ultrasonic dispersion for 30min at the ultrasonic power of 300W and the temperature of 5 ℃ to obtain the bio-based composite nanoparticle aqueous solution.
The preparation method of the bio-based microcapsule emulsion wrapping the monascus pigment is prepared by the following steps:
adding 0.02 weight part of calcium chloride into 10 weight parts of bio-based composite nanoparticle aqueous solution, completely dissolving, dropwise adding 10 weight parts of monascus pigment while performing ultrasonic treatment at the temperature of 5 ℃ and the ultrasonic power of 300W, and performing ultrasonic treatment for 30min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the monascus pigment.
Example 2:
the bio-based microcapsule emulsion wrapping curcumin comprises the following raw materials in parts by weight: 40 parts of bio-based composite nanoparticle aqueous solution, 40 parts of curcumin and 0.08 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.1 part of chitosan, 0.1 part of gelatin, 0.3 part of 1mol/L hydrochloric acid aqueous solution and 20 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.1 part by weight of chitosan into 10 parts by weight of deionized water and adding 0.1 part by weight of gelatin into 10 parts by weight of deionized water, stirring and dissolving to respectively obtain a chitosan aqueous solution and a gelatin aqueous solution, mixing the two aqueous solutions, adding 0.3 part by weight of 1mol/L hydrochloric acid aqueous solution, and performing ultrasonic dispersion at the ultrasonic power of 600W and the temperature of-5 ℃ for 15min to obtain the bio-based composite nanoparticle aqueous solution.
The preparation method of the bio-based microcapsule emulsion wrapping curcumin comprises the following steps:
adding 0.08 weight part of calcium chloride into 40 weight parts of bio-based composite nanoparticle aqueous solution, completely dissolving, dropwise adding 40 weight parts of curcumin while carrying out ultrasonic treatment at the temperature of-5 ℃ and the ultrasonic power of 600W, and carrying out ultrasonic treatment for 15min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the curcumin.
Example 3:
the beta-carotene-wrapped bio-based microcapsule emulsion comprises the following raw materials in parts by weight: 20 parts of bio-based composite nanoparticle aqueous solution, 20 parts of beta-carotene and 0.04 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.1 part of sodium alginate, 0.1 part of gelatin, 0.2 part of 1mol/L hydrochloric acid aqueous solution and 20 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.1 part by weight of sodium alginate into 10 parts by weight of deionized water and adding 0.1 part by weight of gelatin into 10 parts by weight of deionized water, stirring and dissolving to respectively obtain a sodium alginate aqueous solution and a gelatin aqueous solution, mixing the two aqueous solutions, adding 0.2 part by weight of 1mol/L hydrochloric acid aqueous solution, and performing ultrasonic dispersion at the ultrasonic power of 300W and the temperature of 5 ℃ for 30min to obtain the bio-based composite nanoparticle aqueous solution.
The preparation method of the beta-carotene-wrapped bio-based microcapsule emulsion is prepared by the following steps:
adding 0.04 part by weight of calcium chloride into 20 parts by weight of bio-based composite nanoparticle aqueous solution, completely dissolving, dropwise adding 20 parts by weight of beta-carotene while carrying out ultrasonic treatment at the temperature of-5 ℃ under the ultrasonic power of 600W, and carrying out ultrasonic treatment for 15min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the beta-carotene.
Example 4:
the bio-based microcapsule emulsion for coating lycopene comprises the following raw materials in parts by weight: 20 parts of bio-based composite nanoparticle aqueous solution, 40 parts of lycopene and 0.08 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.1 part of pectin, 0.4 part of lysozyme, 2 parts of 1mol/L sodium hydroxide aqueous solution and 50 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.1 part by weight of pectin into 10 parts by weight of deionized water and adding 0.4 part by weight of lysozyme into 40 parts by weight of deionized water, stirring and dissolving to respectively obtain a pectin aqueous solution and a lysozyme aqueous solution, mixing the two aqueous solutions, adding 2 parts by weight of 1mol/L sodium hydroxide aqueous solution, and performing ultrasonic dispersion at the ultrasonic power of 600W and the temperature of-5 ℃ for 30min to obtain the bio-based composite nanoparticle aqueous solution.
The preparation method of the lycopene-coated bio-based microcapsule emulsion is prepared by the following steps:
adding 0.08 weight part of calcium chloride into 20 weight parts of bio-based composite nanoparticle aqueous solution, completely dissolving, dropwise adding 40 weight parts of lycopene while performing ultrasonic treatment at the temperature of-5 ℃ and the ultrasonic power of 600W, and performing ultrasonic treatment for 30min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping lycopene.
Example 5:
the bio-based microcapsule emulsion wrapping the monascus pigment is characterized by comprising the following raw materials in parts by weight: 40 parts of bio-based composite nanoparticle aqueous solution, 20 parts of monascus pigment and 0.06 part of calcium chloride.
The bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.02 part of sodium carboxymethylcellulose, 0.1 part of gelatin, 0.1 part of 1mol/L sodium hydroxide aqueous solution and 12 parts of deionized water.
The preparation method of the bio-based composite nanoparticle aqueous solution comprises the following steps:
adding 0.02 weight part of sodium carboxymethylcellulose into 2 weight parts of deionized water and adding 0.1 weight part of gelatin into 10 weight parts of deionized water, stirring and dissolving to respectively obtain a sodium carboxymethylcellulose aqueous solution and a gelatin aqueous solution, mixing the two aqueous solutions, adding 0.1 weight part of 1mol/L sodium hydroxide aqueous solution, and performing ultrasonic dispersion at the ultrasonic power of 300W and the temperature of 5 ℃ for 15min to obtain the bio-based composite nanoparticle aqueous solution.
The preparation method of the bio-based microcapsule emulsion wrapping the monascus pigment is prepared by the following steps:
adding 0.06 weight part of calcium chloride into 40 weight parts of bio-based composite nanoparticle aqueous solution, completely dissolving, dropwise adding 20 weight parts of monascus pigment while performing ultrasonic treatment at the temperature of 5 ℃ and the ultrasonic power of 300W, and performing ultrasonic treatment for 15min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the monascus pigment.
The potential and stability test results of the natural pigment-coated bio-based microcapsule emulsion ZETA described in examples 1-5 are shown in Table 1.
TABLE 1
| Test items | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| ZETA potential (mV) | -35.5 | -31.6 | -29.8 | -40.5 | -32.3 |
| Residual ratio of absorbance (%) | 28.7 | 22.2 | 18.2 | 25.3 | 28.7 |
| Residual rate of absorbance (%) | 88.7 | 90.2 | 85.5 | 83.9 | 87.5 |
As can be seen from Table 1, the ZETA potential absolute values of the bio-based microcapsule emulsion coated with the natural pigment prepared by the method are basically greater than 30mV, which indicates that the emulsion has excellent stability. By comparing the test results of the absorbance residual rate before and after natural pigment coating in examples 1-5, the absorbance residual rate after the coating with the bio-based microcapsule is significantly improved, which shows that the system stability is high, and the damage of external factors to the natural pigment can be effectively inhibited, so that the bio-based microcapsule emulsion coating the natural pigment prepared by the method has a wide application prospect.
The above examples are merely illustrative for clearly illustrating the present invention and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. The bio-based microcapsule emulsion for wrapping natural pigments is characterized by comprising the following raw materials in parts by weight: 10-40 parts of bio-based composite nanoparticle aqueous solution, 10-40 parts of natural pigment and 0.02-0.08 part of calcium chloride.
The bio-based microcapsule emulsion coated with the natural pigment is characterized in that the bio-based composite nanoparticle solution comprises the following raw materials in parts by weight: 0.02-0.1 part of polysaccharide, 0.1-0.4 part of protein, 0.1-2 parts of pH regulator and 12-50 parts of deionized water.
2. The bio-based microcapsule emulsion encapsulating natural pigment according to claim 1, wherein the preparation method of the bio-based composite nanoparticle aqueous solution is as follows:
adding 0.02-0.1 part by weight of polysaccharide into 2-10 parts by weight of deionized water, adding 0.1-0.4 part by weight of protein into 10-40 parts by weight of deionized water, stirring and dissolving to respectively obtain a polysaccharide aqueous solution and a protein aqueous solution, mixing the two aqueous solutions, adding 0.1-2 parts by weight of pH regulator, and performing ultrasonic dispersion at an ultrasonic power of 300-600W and a temperature of-5 ℃ for 15-30 min to obtain a bio-based composite nanoparticle aqueous solution.
3. The bio-based microcapsule emulsion encapsulating natural pigment according to claim 1, wherein said natural pigment is one of monascus pigment, curcumin, β -carotene, lycopene.
4. The bio-based microcapsule emulsion wrapping natural pigments according to claim 1, wherein the polysaccharide is one or more of sodium alginate, chitosan, pectin, and sodium carboxymethylcellulose.
5. The bio-based microcapsule emulsion encapsulating natural pigments according to claim 1, wherein said protein is one or both of lysozyme and gelatin.
6. The bio-based microcapsule emulsion encapsulating natural pigments according to claim 1, wherein said pH regulator is 1mol/L aqueous hydrochloric acid or aqueous sodium hydroxide.
7. The preparation method of the bio-based microcapsule emulsion coated with natural pigments according to claims 1 to 6, characterized by comprising the following steps:
adding 0.02-0.08 weight part of calcium chloride into 10-40 weight parts of bio-based composite nanoparticle aqueous solution for complete dissolution, dropwise adding 10-40 weight parts of natural pigment while performing ultrasonic treatment at-5 ℃ under the ultrasonic power of 300-600W, and performing ultrasonic treatment for 15-30 min after dropwise adding to obtain the bio-based microcapsule emulsion wrapping the natural pigment.
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| CN103157415A (en) * | 2011-12-14 | 2013-06-19 | 金红叶纸业集团有限公司 | Colored microcapsule and its preparation method |
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| WO2020209908A1 (en) * | 2019-04-12 | 2020-10-15 | International Flavors & Fragrances Inc. | Consumer product with controlled release, biodegradable core-shell microcapsule compositions |
| CN113521027A (en) * | 2021-06-07 | 2021-10-22 | 华中农业大学 | Microcapsule preparation rich in astaxanthin, preparation method and application thereof |
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- 2021-11-29 CN CN202111435194.4A patent/CN114106582A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103157415A (en) * | 2011-12-14 | 2013-06-19 | 金红叶纸业集团有限公司 | Colored microcapsule and its preparation method |
| CN105010934A (en) * | 2015-05-27 | 2015-11-04 | 青岛农业大学 | Protein-chitosan complex coacervation food microcapsule system and preparation method thereof |
| CN107029639A (en) * | 2017-04-28 | 2017-08-11 | 陕西科技大学 | Casein sodium alginate is used for slow odor type polyelectrolyte multiplayer microcapsule of compound wall materialses and preparation method thereof |
| WO2020209908A1 (en) * | 2019-04-12 | 2020-10-15 | International Flavors & Fragrances Inc. | Consumer product with controlled release, biodegradable core-shell microcapsule compositions |
| CN110547452A (en) * | 2019-09-18 | 2019-12-10 | 大连工业大学 | preparation method of gelatin-sodium alginate complex coacervate procyanidine microcapsule |
| CN113521027A (en) * | 2021-06-07 | 2021-10-22 | 华中农业大学 | Microcapsule preparation rich in astaxanthin, preparation method and application thereof |
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