CN107674451B - A kind of Blueberry pigment microcapsules and preparation method thereof - Google Patents
A kind of Blueberry pigment microcapsules and preparation method thereof Download PDFInfo
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- CN107674451B CN107674451B CN201710907995.3A CN201710907995A CN107674451B CN 107674451 B CN107674451 B CN 107674451B CN 201710907995 A CN201710907995 A CN 201710907995A CN 107674451 B CN107674451 B CN 107674451B
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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
- C09B67/0096—Purification; Precipitation; Filtration
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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
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
Abstract
The present invention relates to a kind of Blueberry pigment microcapsules and preparation method thereof, belong to food processing technology field, and the wall material of the microcapsules is made of chitosan, sodium tripolyphosphate and sodium alginate, and core material is water-soluble Blueberry pigment；The microcapsules emulsify core material using high-pressure homogeneous, then form microcapsules by complex coacervation, then are made through vacuum freeze drying.Preparation process of the present invention is simple, preparation condition is mild, easy to spread, and microcapsules good dispersion obtained, stability are high, suitable for industries such as food, health care product, cosmetics.
Description
Technical field
The present invention relates to a kind of Blueberry pigment microcapsules and preparation method thereof, belong to food processing technology field.
Background technique
Pigment in Blueberry belongs to is muttered (C with flavylium ion6-C3-C6) be parent nucleus flavone compound,
As natural and free radical scavenger, there is anti-oxidant, promotion erythrolabe to synthesize again, improve immunity, anti-painstaking effort
A variety of physiological active functions such as pipe disease, anti-aging have broad application prospects in fields such as food, cosmetics, drugs.But
Blueberry pigment is water colo(u)r, and for yellow melt salt cation, alkaline and oxidisability is strong, and the phenolic hydroxyl group on parent nucleus is in acid and goes back
Originality, conjugated double bond is easy to happen the displacement of B- ring electronics on pyranoid ring, so the environmental factors such as acid, alkali, oxidant, light radiation
It can be acted on blueberry anthocyanin, the change of the chemical structures such as quinoid alkali, pseudobase, chalcone, addition, open loop, aquation occurs.
The unstability of this chemical structure of Blueberry pigment seriously affects the performance of its physiological activity, or even makes active disappearance, answers it
With being greatly limited, and microcapsules technology is then to solve the problems, such as this effective way.
Microcapsules technology be the core material with functional activity is embedded in it is small and in the wall material that seals, prevent core material and light
With the direct contact of the external environments such as heat, the stability of core material is improved, is obtained extensively in fields such as food, cosmetics, drugs
Using.Currently, core material belongs to the microcapsules technology of the molten substance of oil comparative maturity, such as application No. is
The Chinese patent of CN200810015871.5 discloses " a kind of Xanthophyll micro-capsule and preparation method thereof ", and lutein is dissolved in
Organic solvent is added to emulsifying in the gumwater containing emulsifier and antioxidant, is then added to chitosan or gelatin
Encystation is agglomerated in solution, heated-air drying obtains microcapsules.And the microcapsules that core material belongs to water-soluble substances are then studied less, it is external
The microcapsule product for the water-soluble core material being commercialized mainly has ferrous sulfate, citric acid etc., the domestic research to this aspect
Mainly there are sodium bicarbonate, vitamin C, L-carnitine etc..Application No. is the Chinese patents of CN200720154938.4 to disclose " one
Kind oligomeric proanhocyanidins microcapsule ", microcapsules wrap up in capsule by the capsule suitcase that one layer of maltodextrin and Arabic gum are wall material
Content is constituted, and wherein content is glucosidase procyanidins pulverulent solids.Different core materials and different Microencapsulation Methods
There is different requirements for microencapsulation wall, using Blueberry pigment as core material, chitosan, sodium tripolyphosphate and sodium alginate are wall
Material yet there are no report using research of the multiple cohesion-Vacuum Freezing & Drying Technology in terms of Blueberry pigment embedding.
Summary of the invention
It is soluble easily in water for Blueberry pigment and be easy under the action of illumination, high temperature and oxygen to occur oxidative degradation, it is difficult
The problem of to be widely used in current food, the invention discloses a kind of Blueberry pigment microcapsules and preparation method thereof, propose
A kind of microencapsulation technology for keeping water colo(u)r stability and expanding use scope, to increase its dispersibility and to heat, light
With the tolerance of oxygen etc..
To solve the above problems, the present invention adopts the following technical scheme:
The invention discloses a kind of Blueberry pigment microcapsules, it is characterized in that: the wall material of the microcapsules is by chitosan, three
Polyphosphate sodium and sodium alginate composition, core material are water-soluble Blueberry pigment.
Blueberry pigment microcapsules of the present invention the preparation method comprises the following steps: emulsifying core material using high-pressure homogeneous, then by coagulating again
Poly- method forms microcapsules, then through vacuum freeze drying, i.e. acquisition target product Blueberry pigment microcapsules.Specifically, including wall
The preparation of material solution, the emulsification of core material, microcapsules are formed and dry four steps of microcapsules, the specific steps are as follows:
(1) preparation of wall material solution:
It under 30 DEG C~40 DEG C water bath conditions, adds chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 0.5~2%；
Sodium tripolyphosphate and sodium alginate are add to deionized water, with magnetic stirrer to solution at transparence
State obtains sodium tripolyphosphate-mixed solution of sodium alginate, and wherein the mass concentration of sodium tripolyphosphate is 1~3%, sodium alginate
Mass concentration be 0.4~0.6%；
(2) emulsification of core material:
It is 10:1:1 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratio, in 30 DEG C~40 DEG C water-bath items
Under part, Tween-80 and sucrose fatty ester SE-5 are added into the chitosan solution of step (1) configuration, after mixing evenly, to institute
It obtains in mixed liquor and Blueberry pigment is added, be stirred well to Blueberry pigment dissolution, further pressed using high-pressure homogeneous mulser
Power 40Mpa condition emulsified 2 times, obtain Blueberry pigment/chitosan emulsion；Wherein, the body of Blueberry pigment and the mixed liquor
Product is than 1:5~15；
(3) microcapsules are formed:
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with the speed of 10mL/min be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, centrifugation settles microcapsules；
The Blueberry pigment/chitosan emulsion and the volume ratio of the sodium tripolyphosphate-mixed solution of sodium alginate are
11:20~40；
(4) microcapsules are dry:
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, i.e. acquisition target produces
Reddish blue certain kind of berries pigment microcapsule.
Preferably, the extracting method of the Blueberry pigment are as follows: blueberry is freezed 5~10 days under the conditions of -18 DEG C, is then taken
Out and thaw at RT 1h, it is added in the edible alcohol of pH=3 according still further to solid-liquid ratio 1g:10mL, is placed in 40 DEG C of water bath with thermostatic control
120min is extracted in pot, is filtered, filtrate is collected, remaining filter residue is primary by the same terms repetitive operation, merges filtrate twice simultaneously
Centrifugation, then rotary evaporation is concentrated, i.e. acquisition Blueberry pigment medicinal extract.
Preferably, centrifugation described in step (3) is to be centrifuged 10min under the conditions of 10000r/min.
Preferably, the mass concentration of chitosan solution described in step (1) is 1%, the sodium tripolyphosphate-sodium alginate
The mass concentration of sodium tripolyphosphate is 2% in mixed solution, the mass concentration of sodium alginate is 0.5%；Blueberry color in step (2)
The plain volume ratio 1:10 with the mixed liquor；Blueberry pigment described in step (3)/chitosan emulsion and the tripolyphosphate
Sodium-mixed solution of sodium alginate volume ratio is 11:30.
The beneficial effects of the present invention are embodied in:
1, preparation process of the present invention is simple, preparation condition is mild, easy to spread, microcapsules good dispersion obtained,
Stability is high, suitable for industries such as food, health care product, cosmetics.
2, Blueberry pigment extract is passed through multiple cohesion-Vacuum Freezing & Drying Technology system using microencapsulation technology by the present invention
The flavor and nutrition at microcapsules, not retaining functional components therein only effectively, and keeping blueberry intrinsic, can be used as into
The raw material of one step deep processing, develops various food products, such as functional food；And the chance for survival of microorganism can be reduced,
Long-term transport, preservation at room temperature balance production and marketing peak to extend the supply season of product, have very big market
Potentiality.
3, Blueberry pigment microcapsule preparation method of the invention has the advantage that
(1) blueberry is freezed but not broken use is acidified edible alcohol extraction, Blueberry pigment yield and purity is high；
(2) it uses chitosan, sodium tripolyphosphate and sodium alginate for wall material, meets the needs of water-soluble core material class product；
(3) Vacuum Freezing & Drying Technology is used, the bioactivity of Blueberry pigment is utmostly kept.
Detailed description of the invention
Fig. 1 is the finished product photo of present invention gained Blueberry pigment microcapsules, and wherein A is capsule appearance structure, and B is capsule electricity
Mirror structure chart.
Fig. 2 is the particle size and particle size distribution figure of 2 gained Blueberry pigment microcapsules of embodiment.
Specific embodiment
Technical solution of the present invention is described in detail by the following examples.
Blueberry pigment medicinal extract used in following embodiments extracts as follows: blueberry is freezed 5~10 under the conditions of -18 DEG C
It, then takes out simultaneously thaw at RT 1h, is added to according still further to solid-liquid ratio (ratio of blueberry quality and edible alcohol volume) 1g:10mL
It in the edible alcohol of pH=3, is placed in 40 DEG C of thermostat water bath and extracts 120min, filter, collect filtrate, remaining filter residue presses phase
It is primary with condition repetitive operation, merge filtrate twice and centrifugation, then rotary evaporation be concentrated into condenser pipe no longer go out alcohol, i.e.,
Obtain Blueberry pigment medicinal extract.
Embodiment 1
The present embodiment prepares Blueberry pigment microcapsules as follows:
(1) preparation of wall material solution:
It under 30 DEG C~40 DEG C water bath conditions, adds chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 0.5%；
Sodium tripolyphosphate and sodium alginate are add to deionized water, with magnetic stirrer to solution at transparence
State obtains sodium tripolyphosphate-mixed solution of sodium alginate, and wherein the mass concentration of sodium tripolyphosphate is the matter of 1%, sodium alginate
Measuring concentration is 0.4%；
(2) emulsification of core material:
It is 10:1:1 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratio, in 30 DEG C~40 DEG C water-bath items
Tween-80 and sucrose fatty ester SE-5 are added in the chitosan solution configured under part to step (1), 10min is stirred, to gained
Blueberry pigment medicinal extract is added in mixed liquor, is stirred well to Blueberry pigment dissolution, is further existed using high-pressure homogeneous mulser
Pressure 40Mpa condition emulsified 2 times, obtain Blueberry pigment/chitosan emulsion；Wherein, the volume of Blueberry pigment and mixed liquor
Than for 1:15；
(3) microcapsules are formed:
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with the speed of 10mL/min be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, are centrifuged (10000r/min, 10min),
Settle microcapsules；
The volume ratio of Blueberry pigment/chitosan emulsion and the sodium tripolyphosphate-mixed solution of sodium alginate is 11:
40；
(4) microcapsules are dry:
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, i.e. acquisition target produces
Reddish blue certain kind of berries pigment microcapsule.
Embodiment 2
The present embodiment prepares Blueberry pigment microcapsules as follows:
(1) preparation of wall material solution:
It under 30 DEG C~40 DEG C water bath conditions, adds chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 1%；
Sodium tripolyphosphate and sodium alginate are add to deionized water, with magnetic stirrer to solution at transparence
State obtains sodium tripolyphosphate-mixed solution of sodium alginate, and wherein the mass concentration of sodium tripolyphosphate is the matter of 2%, sodium alginate
Measuring concentration is 0.5%；
(2) emulsification of core material:
It is 10:1:1 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratio, in 30 DEG C~40 DEG C water-bath items
Tween-80 and sucrose fatty ester SE-5 are added in the chitosan solution configured under part to step (1), 10min is stirred, to gained
Blueberry pigment medicinal extract is added in mixed liquor, is stirred well to Blueberry pigment dissolution, is further existed using high-pressure homogeneous mulser
Pressure 40Mpa condition emulsified 2 times, obtain Blueberry pigment/chitosan emulsion；Wherein, the volume of Blueberry pigment and mixed liquor
Than for 1:10；
(3) microcapsules are formed:
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with the speed of 10mL/min be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, are centrifuged (10000r/min, 10min),
Settle microcapsules；
Blueberry pigment/chitosan emulsion and sodium tripolyphosphate-mixed solution of sodium alginate volume ratio are 11:30；
(4) microcapsules are dry:
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, i.e. acquisition target produces
Reddish blue certain kind of berries pigment microcapsule.
Embodiment 3
The present embodiment prepares Blueberry pigment microcapsules as follows:
(1) preparation of wall material solution:
It under 30 DEG C~40 DEG C water bath conditions, adds chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 2%；
Sodium tripolyphosphate and sodium alginate are add to deionized water, with magnetic stirrer to solution at transparence
State obtains sodium tripolyphosphate-mixed solution of sodium alginate, and wherein the mass concentration of sodium tripolyphosphate is the matter of 3%, sodium alginate
Measuring concentration is 0.6%；
(2) emulsification of core material:
It is 10:1:1 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratio, in 30 DEG C~40 DEG C water-bath items
Tween-80 and sucrose fatty ester SE-5 are added in the chitosan solution configured under part to step (1), 10min is stirred, to gained
Blueberry pigment medicinal extract is added in mixed liquor, is stirred well to Blueberry pigment dissolution, is further existed using high-pressure homogeneous mulser
Pressure 40Mpa condition emulsified 2 times, obtain Blueberry pigment/chitosan emulsion；Wherein, the volume of Blueberry pigment and mixed liquor
Than for 1:5；
(3) microcapsules are formed:
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with the speed of 10mL/min be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, are centrifuged (10000r/min, 10min),
Settle microcapsules；
The volume ratio of Blueberry pigment/chitosan emulsion and the sodium tripolyphosphate-mixed solution of sodium alginate is 11:
20；
(4) microcapsules are dry:
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, i.e. acquisition target produces
Reddish blue certain kind of berries pigment microcapsule.
Physical features observation is carried out to the various embodiments described above to compare, and the results are shown in Table 1, it can be seen that 2 gained sample of embodiment
It is uniform particle sizes, scattered.Particle size and the particle size distribution figure of 2 gained microcapsules of embodiment are as shown in Fig. 2, after tested, wrap
Rate is buried up to 76.36%.
Sample obtained by each embodiment is divided in valve bag, and is placed 1 year under room temperature environment, appearance is without change
Change, shows storage stability of the sample under light heat environment.
The different embodiment anthocyanidin microcapsules physical features of table 1 compare
Above content is only citing made for the present invention and explanation, affiliated those skilled in the art are to being retouched
The specific embodiment stated does various modifications or additions or is substituted in a similar manner, as long as it does not deviate from the concept of invention
Or beyond the scope defined by this claim, it is within the scope of protection of the invention.
Claims (3)
1. a kind of preparation method of Blueberry pigment microcapsules, it is characterised in that: the wall material of the Blueberry pigment microcapsules is gathered by shell
Sugar, sodium tripolyphosphate and sodium alginate composition, core material are water-soluble Blueberry pigment；
The Blueberry pigment microcapsules the preparation method comprises the following steps: emulsify core material using high-pressure homogeneous, then made by complex coacervation
Microcapsules are formed, then through vacuum freeze drying, i.e. acquisition target product Blueberry pigment microcapsules；Specifically include the system of wall material solution
Standby, core material emulsification, microcapsules are formed and dry four steps of microcapsules:
(1) preparation of wall material solution:
It under 30 DEG C~40 DEG C water bath conditions, adds chitosan into deionized water, stirring obtains mass concentration to being completely dissolved
0.5~2% chitosan solution；
Sodium tripolyphosphate and sodium alginate are add to deionized water, with magnetic stirrer to solution at pellucidity,
Sodium tripolyphosphate-mixed solution of sodium alginate is obtained, wherein the mass concentration of sodium tripolyphosphate is the matter of 1~3%, sodium alginate
Measuring concentration is 0.4~0.6%；
(2) emulsification of core material:
It is 10:1:1 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratio, under 30 DEG C~40 DEG C water bath conditions,
Tween-80 and sucrose fatty ester SE-5 is added in the chitosan solution configured to step (1), it is after mixing evenly, mixed to gained
It closes in liquid and Blueberry pigment is added, Blueberry pigment dissolution is stirred well to, further using high-pressure homogeneous mulser in pressure
40Mpa condition emulsified 2 times, obtain Blueberry pigment/chitosan emulsion；Wherein, the volume of Blueberry pigment and the mixed liquor
Than 1:5~15；
The extracting method of the Blueberry pigment are as follows: blueberry is freezed 5~10 days under the conditions of -18 DEG C, then takes out simultaneously room temperature solution
Freeze 1h, is added in the edible alcohol of pH=3 according still further to solid-liquid ratio 1g:10mL, is placed in 40 DEG C of thermostat water bath and extracts
120min is filtered, and collects filtrate, and remaining filter residue is primary by the same terms repetitive operation, merges filtrate twice and centrifugation, then
Rotary evaporation concentration, i.e. acquisition Blueberry pigment medicinal extract；
(3) microcapsules are formed:
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, it is rapid that progress is added dropwise with the speed of 10mL/min
(1) in the sodium tripolyphosphate-mixed solution of sodium alginate configured, microcapsules are formed, centrifugation settles microcapsules；
The volume ratio of the Blueberry pigment/chitosan emulsion and the sodium tripolyphosphate-mixed solution of sodium alginate is 11:20
~40；
(4) microcapsules are dry:
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, i.e. acquisition target product is blue
Certain kind of berries pigment microcapsule.
2. preparation method according to claim 1, it is characterised in that: centrifugation described in step (3) is in 10000r/min
Under the conditions of be centrifuged 10min.
3. preparation method according to claim 1, it is characterised in that: the quality of chitosan solution described in step (1) is dense
Degree is 1%, and the mass concentration of sodium tripolyphosphate is 2%, sodium alginate in the sodium tripolyphosphate-mixed solution of sodium alginate
Mass concentration is 0.5%；
The volume ratio 1:10 of Blueberry pigment and the mixed liquor in step (2)；
The volume of Blueberry pigment described in step (3)/chitosan emulsion and the sodium tripolyphosphate-mixed solution of sodium alginate
Than for 11:30.
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| CN109393482A (en) * | 2018-12-07 | 2019-03-01 | 吉林大学 | A kind of blueberry pyrans anthocyanidin aglycon microcapsules and preparation method |
| CN110041726B (en) | 2019-04-30 | 2020-07-21 | 沈阳农业大学 | Preparation method of high-stability liquid blueberry anthocyanin |
| CN110952375A (en) * | 2019-11-19 | 2020-04-03 | 浙江华丰纸业科技有限公司 | Food-grade oilproof paper and preparation method thereof |
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| CN102210645B (en) * | 2011-05-31 | 2013-01-23 | 吉林大学 | Lutein ophthalmic nanocapsule in-situ gel preparation and preparation method thereof |
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| CN103468020A (en) * | 2013-09-26 | 2013-12-25 | 江苏省中国科学院植物研究所 | Blueberry pigment extraction method |
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