CN107674451A - 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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- CN107674451A CN107674451A CN201710907995.3A CN201710907995A CN107674451A CN 107674451 A CN107674451 A CN 107674451A CN 201710907995 A CN201710907995 A CN 201710907995A CN 107674451 A CN107674451 A CN 107674451A
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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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
- General Preparation And Processing Of Foods (AREA)
Abstract
The present invention relates to a kind of Blueberry pigment microcapsules and preparation method thereof, belong to food processing technology field, the wall material of the microcapsules is made up of chitosan, sodium tripolyphosphate and sodium alginate, and core is water miscible Blueberry pigment；The microcapsules emulsify core using high-pressure homogeneous, then form microcapsules by complex coacervation, then be made through vacuum freeze drying.Preparation process of the present invention is simple, preparation condition is gentle, easy to spread, and obtained microcapsules good dispersion, stability are high, are suitable for the industries such as food, health products, 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 technology
Pigment in Blueberry belongs to is muttered (C with flavylium ion6-C3-C6) be parent nucleus flavone compound, its
As natural and free radical scavenger, there is anti-oxidant, promotion erythrolabe to synthesize again, improve immunity, anti-painstaking effort
Pipe disease, anti-ageing a variety of physiological active functionses of waiting for a long time, have broad application prospects in fields such as food, cosmetics, medicines.But
Blueberry pigment is water colo(u)r, is yellow melt salt cation, and alkalescence and oxidisability are strong, and the phenolic hydroxyl group on its parent nucleus is in acidity and also
Originality, the displacement of B- rings electronics easily occurs for conjugated double bond on its pyranoid ring, so the envirment factor such as acid, alkali, oxidant, light radiation
It can be acted on blueberry anthocyanin, the change of the chemical constitutions such as quinoid alkali, pseudobase, chalcone, addition, open loop, aquation occurs.
The unstability of this chemical constitution of Blueberry pigment has a strong impact on the performance of its physiologically active, or even makes active disappearance, makes it should
With being greatly limited, and microcapsules technology is then the effective way for solving this problem.
Microcapsules technology is that the core with functional activity is embedded in small and sealing wall material, prevents core and light
With the direct contact of the external environment such as heat, the stability of core is improved, is obtained extensively in fields such as food, cosmetics, medicines
Using.At present, core belongs to the microcapsules technology of the molten class material of oil comparative maturity, such as Application No.
CN200810015871.5 Chinese patent discloses " a kind of Xanthophyll micro-capsule and preparation method thereof ", and lutein is dissolved in by it
Organic solvent, emulsifying in the gumwater containing emulsifying agent and antioxidant is added to, is then added to chitosan or gelatin
Encystation is condensed in solution, heated-air drying obtains microcapsules.It is external and the microcapsules that core belongs to water-soluble substances are then studied less
The microcapsule product of the water-soluble core of commercialization mainly has ferrous sulfate, citric acid etc., the domestic research to this aspect
Mainly there are sodium acid carbonate, vitamin C, l-cn etc..Application No. CN200720154938.4 Chinese patent discloses " one
Kind oligomeric proanhocyanidins microcapsule ", its microcapsules wrap up in capsule by one layer of maltodextrin and Arabic gum for the capsule suitcase of wall material
Content is formed, and wherein content is glucosidase procyanidins pulverulent solids.Different cores and different Microencapsulation Methods
There is different requirements for microencapsulation wall, using Blueberry pigment as core, chitosan, sodium tripolyphosphate and sodium alginate are wall
Material, report yet there are no using research of the multiple cohesion-Vacuum Freezing ＆ Drying Technology in terms of Blueberry pigment embedding.
The content of the invention
It is soluble in water and be easy in the presence of illumination, high temperature and oxygen to occur oxidative degradation for Blueberry pigment, 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
It is a kind of keep water colo(u)r stability and expand use range microencapsulation technology, with increase its dispersiveness and to heat, light
With the tolerance of oxygen etc..
To solve the above problems, the present invention adopts the following technical scheme that：
The invention discloses a kind of Blueberry pigment microcapsules, its feature is：The wall material of the microcapsules is by chitosan, three
Polyphosphate sodium and sodium alginate composition, core is water miscible Blueberry pigment.
The preparation method of Blueberry pigment microcapsules of the present invention is：Core is emulsified using high-pressure homogeneous, then by coagulating again
Poly- method forms microcapsules, then through vacuum freeze drying, that is, obtains target product Blueberry pigment microcapsules.Specifically, including wall
The preparation of material solution, the emulsification of core, microcapsules are formed and microcapsules dry four steps, comprise the following steps that：
(1) preparation of wall material solution：
Under 30 DEG C~40 DEG C water bath conditions, add 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 added in deionized water, with magnetic stirrer to solution into transparence
State, sodium tripolyphosphate-mixed solution of sodium alginate is obtained, the wherein mass concentration of sodium tripolyphosphate is 1~3%, sodium alginate
Mass concentration be 0.4~0.6%；
(2) emulsification of core：
It is 10 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratioes:1:1, in 30 DEG C~40 DEG C water-bath bars
Under part, Tween-80 and sucrose fatty ester SE-5 are added in the chitosan solution configured to step (1), after stirring, to institute
Obtain in mixed liquor and add Blueberry pigment, be stirred well to Blueberry pigment dissolving, further pressed using high-pressure homogeneous mulser
Emulsified 2 times of power 40Mpa conditions, obtain Blueberry pigment/chitosan emulsion；Wherein, Blueberry pigment and the body of the mixed liquor
Product ratio 1:5~15；
(3) microcapsules are formed：
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with 10mL/min speed be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, centrifugation, settle 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 dried：
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, that is, obtain target production
Reddish blue certain kind of berries pigment microcapsule.
Preferably, the extracting method of the Blueberry pigment is：Blueberry is freezed 5~10 days under the conditions of -18 DEG C, Ran Houqu
Go out simultaneously thaw at RT 1h, according still further to solid-liquid ratio 1g:10mL is added in pH=3 edible alcohol, is placed in 40 DEG C of water bath with thermostatic control
120min is extracted in pot, is filtered, collects filtrate, remaining filter residue repeats once by the same terms, merges filtrate twice simultaneously
Centrifugation, then rotary evaporation concentration, that is, obtain Blueberry pigment medicinal extract.
Preferably, the centrifugation described in step (3) is that 10min is centrifuged under the conditions of 10000r/min.
Preferably, the mass concentration of the chitosan solution described in step (1) is 1%, the sodium tripolyphosphate-sodium alginate
In mixed solution the mass concentration of sodium tripolyphosphate be 2%, the mass concentration of sodium alginate be 0.5%；Blueberry color in step (2)
The plain and volume ratio of the mixed liquor 1:10；Blueberry pigment/chitosan emulsion described in step (3) and the tripolyphosphate
The volume ratio of sodium-mixed solution of sodium alginate is 11:30.
Beneficial effects of the present invention are embodied in：
1st, preparation process of the present invention is simple, preparation condition is gentle, easy to spread, obtained microcapsules good dispersion,
Stability is high, is suitable for the industries such as food, health products, cosmetics.
2nd, Blueberry pigment extract is passed through multiple cohesion-Vacuum Freezing ＆ Drying Technology system by the present invention using microencapsulation technology
Into microcapsules, do not retain functional components therein only effectively, and keep the intrinsic flavor of blueberry and nutrition, 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 ambient temperature, so as to extend the supply season of product, production and marketing peak is balanced, there is very big market
Potentiality.
3rd, Blueberry pigment microcapsule preparation method of the invention has advantages below：
(1) blueberry is freezed but not broken use is acidified edible alcohol extraction, Blueberry pigment yield and purity are high；
(2) chitosan, sodium tripolyphosphate and sodium alginate is used to meet the needs of water-soluble core class product for wall material；
(3) Vacuum Freezing ＆ Drying Technology is used, at utmost keeps the bioactivity of Blueberry pigment.
Brief description of the drawings
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 the gained Blueberry pigment microcapsules of embodiment 2.
Embodiment
Technical scheme is described in detail by the following examples.
Blueberry pigment medicinal extract extracts as follows used in following embodiments：Blueberry is freezed 5~10 under the conditions of -18 DEG C
My god, simultaneously thaw at RT 1h is then taken out, according still further to solid-liquid ratio (ratio of blueberry quality and edible alcohol volume) 1g:10mL is added to
In pH=3 edible alcohol, it is placed in 40 DEG C of thermostat water bath and extracts 120min, filter, collect filtrate, remaining filter residue is pressed
The same terms repeat once, merge filtrate twice and centrifugation, and then rotary evaporation is concentrated into condenser pipe and no longer goes out alcohol,
Obtain Blueberry pigment medicinal extract.
Embodiment 1
The present embodiment prepares Blueberry pigment microcapsules as follows：
(1) preparation of wall material solution：
Under 30 DEG C~40 DEG C water bath conditions, add chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 0.5%；
Sodium tripolyphosphate and sodium alginate are added in deionized water, with magnetic stirrer to solution into transparence
State, sodium tripolyphosphate-mixed solution of sodium alginate is obtained, the wherein mass concentration of sodium tripolyphosphate is the 1%, matter of sodium alginate
It is 0.4% to measure concentration；
(2) emulsification of core：
It is 10 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratioes:1:1, in 30 DEG C~40 DEG C water-bath bars
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, Blueberry pigment dissolving is stirred well to, is further existed using high-pressure homogeneous mulser
Emulsified 2 times of pressure 40Mpa conditions, obtain Blueberry pigment/chitosan emulsion；Wherein, Blueberry pigment and the volume of mixed liquor
Than for 1:15；
(3) microcapsules are formed：
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with 10mL/min speed be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, centrifuge (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 dried：
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, that is, obtain target production
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：
Under 30 DEG C~40 DEG C water bath conditions, add chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 1%；
Sodium tripolyphosphate and sodium alginate are added in deionized water, with magnetic stirrer to solution into transparence
State, sodium tripolyphosphate-mixed solution of sodium alginate is obtained, the wherein mass concentration of sodium tripolyphosphate is the 2%, matter of sodium alginate
It is 0.5% to measure concentration；
(2) emulsification of core：
It is 10 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratioes:1:1, in 30 DEG C~40 DEG C water-bath bars
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, Blueberry pigment dissolving is stirred well to, is further existed using high-pressure homogeneous mulser
Emulsified 2 times of pressure 40Mpa conditions, obtain Blueberry pigment/chitosan emulsion；Wherein, Blueberry pigment and the volume of mixed liquor
Than for 1:10；
(3) microcapsules are formed：
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with 10mL/min speed be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, centrifuge (10000r/min,
10min), settle microcapsules；
The volume ratio of Blueberry pigment/chitosan emulsion and sodium tripolyphosphate-mixed solution of sodium alginate is 11:30；
(4) microcapsules are dried：
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, that is, obtain target production
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：
Under 30 DEG C~40 DEG C water bath conditions, add chitosan into deionized water, stirring obtains quality to being completely dissolved
The chitosan solution of concentration 2%；
Sodium tripolyphosphate and sodium alginate are added in deionized water, with magnetic stirrer to solution into transparence
State, sodium tripolyphosphate-mixed solution of sodium alginate is obtained, the wherein mass concentration of sodium tripolyphosphate is the 3%, matter of sodium alginate
It is 0.6% to measure concentration；
(2) emulsification of core：
It is 10 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratioes:1:1, in 30 DEG C~40 DEG C water-bath bars
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, Blueberry pigment dissolving is stirred well to, is further existed using high-pressure homogeneous mulser
Emulsified 2 times of pressure 40Mpa conditions, obtain Blueberry pigment/chitosan emulsion；Wherein, Blueberry pigment and the volume of mixed liquor
Than for 1:5；
(3) microcapsules are formed：
Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, with 10mL/min speed be added dropwise into
In sodium tripolyphosphate-mixed solution of sodium alginate of step (1) configuration, microcapsules are formed, centrifuge (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 dried：
Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, that is, obtain target production
Reddish blue certain kind of berries pigment microcapsule.
The various embodiments described above are carried out with physical features observation to compare, the results are shown in Table 1, it can be seen that the gained sample of embodiment 2
It is uniform particle sizes, scattered.Particle size and the particle size distribution figure of the gained microcapsules of embodiment 2 are as shown in Fig. 2 after tested, it is wrapped
Rate is buried up to 76.36%.
Sample obtained by each embodiment is divided in valve bag, and placed 1 year under room temperature environment, its outward appearance is without change
Change, indicate 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, and affiliated those skilled in the art are to being retouched
The specific embodiment stated is made various modifications or supplement or substituted using similar mode, without departing from the design of invention
Or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (6)
- A kind of 1. Blueberry pigment microcapsules, it is characterised in that：The wall material of the microcapsules is by chitosan, sodium tripolyphosphate and marine alga Sour sodium composition, core is water miscible Blueberry pigment.
- A kind of 2. preparation method of the Blueberry pigment microcapsules described in claim 1, it is characterised in that：Make core using high-pressure homogeneous Material emulsifies, and then forms microcapsules by complex coacervation, then through vacuum freeze drying, that is, it is micro- to obtain target product Blueberry pigment Capsule.
- 3. preparation method according to claim 2, it is characterised in that：Preparation, core including wall material solution emulsify, are micro- Capsule is formed and microcapsules dry four steps, specific as follows：(1) preparation of wall material solution：Under 30 DEG C~40 DEG C water bath conditions, add chitosan into deionized water, stirring obtains mass concentration to being completely dissolved 0.5~2% chitosan solution；Sodium tripolyphosphate and sodium alginate are added in deionized water, with magnetic stirrer to solution into pellucidity, Sodium tripolyphosphate-mixed solution of sodium alginate is obtained, the wherein mass concentration of sodium tripolyphosphate is 1~3%, matter of sodium alginate It is 0.4~0.6% to measure concentration；(2) emulsification of core：It is 10 according to chitosan, Tween-80, sucrose fatty ester SE-5 mass ratioes:1:1, under 30 DEG C~40 DEG C water bath conditions, Tween-80 and sucrose fatty ester SE-5 are added in the chitosan solution configured to step (1), after stirring, is mixed to gained Close in liquid and add Blueberry pigment, Blueberry pigment dissolving is stirred well to, further using high-pressure homogeneous mulser in pressure Emulsified 2 times of 40Mpa conditions, obtain Blueberry pigment/chitosan emulsion；Wherein, Blueberry pigment and the volume of the mixed liquor Than 1:5~15；(3) microcapsules are formed：Blueberry pigment/chitosan emulsion obtained by step (2) is placed in atomizer, is added dropwise with 10mL/min speed into step (1) in sodium tripolyphosphate-mixed solution of sodium alginate of configuration, microcapsules is formed, centrifugation, settle 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 dried：Microcapsules after sedimentation are placed in 85 DEG C of refrigerators of ﹣ after freezing at least 2h, then vacuum freeze drying, that is, it is blue to obtain target product Certain kind of berries pigment microcapsule.
- 4. preparation method according to claim 3, it is characterised in that the extracting method of the Blueberry pigment is：By blueberry Freezed 5~10 days under the conditions of -18 DEG C, simultaneously thaw at RT 1h is then taken out, according still further to solid-liquid ratio 1g:10mL is added to pH=3 Edible alcohol in, be placed in 40 DEG C of thermostat water bath and extract 120min, filter, collect filtrate, remaining filter residue presses identical bar Part repeats once, merges filtrate twice and centrifugation, and then rotary evaporation concentrates, that is, obtains Blueberry pigment medicinal extract.
- 5. preparation method according to claim 3, it is characterised in that：Centrifugation described in step (3) is in 10000r/min Under the conditions of centrifuge 10min.
- 6. preparation method according to claim 3, it is characterised in that：The quality of chitosan solution described in step (1) is dense Spend for 1%, in the sodium tripolyphosphate-mixed solution of sodium alginate mass concentration of sodium tripolyphosphate be 2%, sodium alginate Mass concentration is 0.5%；Blueberry pigment and the volume ratio 1 of the mixed liquor in step (2):10；The volume of Blueberry pigment/chitosan emulsion described in step (3) 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 |
| CN109717688A (en) * | 2018-05-21 | 2019-05-07 | 泰山医学院 | A kind of rehabilitation cup of Parkinsonian |
| 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 |
| WO2020220478A1 (en) * | 2019-04-30 | 2020-11-05 | 沈阳农业大学 | Method for preparing high-stability liquid blueberry anthocyanins |
| CN116807938A (en) * | 2023-07-06 | 2023-09-29 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
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| CN116807938A (en) * | 2023-07-06 | 2023-09-29 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
| CN116807938B (en) * | 2023-07-06 | 2024-04-16 | 希肤科技（上海）有限公司 | Composite mask cloth with color-changing function and preparation method thereof |
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| CN107674451B (en) | 2019-08-23 |
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