CN101219125B - Cold water dispersion type xanthophyll micro-capsule and its preparing method - Google Patents
Cold water dispersion type xanthophyll micro-capsule and its preparing method Download PDFInfo
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- CN101219125B CN101219125B CN2008100173471A CN200810017347A CN101219125B CN 101219125 B CN101219125 B CN 101219125B CN 2008100173471 A CN2008100173471 A CN 2008100173471A CN 200810017347 A CN200810017347 A CN 200810017347A CN 101219125 B CN101219125 B CN 101219125B
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Abstract
The invention discloses a cool water dispersible lutein microcapsule. The lutein microcapsule comprises lutein powder used as core material, modified starch and natural colloid used as wall material, and appropriate amount of emulsifier added, which are mixed and added with proper amount of water, heated and stirred, and then filtered and spray dried to obtain the lutein microcapsule. The invention has easy material acquiring, can be applied to food or pharmaceutical industry, and has good safety without using organic solvents thus the nature of the lutein is well kept. In the invention, the core material and the wall material are mixed directly in one step, and emulsified by controlling the temperature; the lutein liquid is embedded into semi-permeable or hermetic solid microcapsule powder by adopting spay drying. The obtained microcapsule powder has good water-solubility, high stability and encapsulation rate.
Description
Technical field
The present invention relates to a kind of cold water dispersion type xanthophyll micro-capsule, the invention still further relates to the method for preparing of this microcapsule.
Background technology
Phylloxanthin (Lutein) has another name called " plant progesterone ", is a kind of oxygen containing carotenoid, extensively is present in Flos Tagetis Erectae, Fructus Musae, Fructus actinidiae chinensis and the corn.Phylloxanthin can be used as natural colorant; Have lovely luster, strong coloring force, safety non-toxic, be rich in advantages such as nutrition; This chemical compound is again a kind of antioxidant of excellent performance simultaneously; Can resist oxygen-derived free radicals and in human body, cause cell and organ injury, cardiovascula sclerosis, coronary heart disease and tumor disease that the prevention body aging causes.In addition, phylloxanthin still is the main carotenoid antioxidant content in ocular tissue's retina, visual deterioration and the blind disease that can prevent senile eyeball macula retinae to degenerate and cause.Phylloxanthin has the conjugated polyene structure, and its unstable chemcial property very easily receives the degraded of light, heat, acid and oxygen and loses biological activity; Phylloxanthin is insoluble in water simultaneously, is slightly soluble in fat and oil.Above factor has greatly hindered the practical application of phylloxanthin.Microencapsulation technology then is the effective ways that address these problems.
Microcapsule technology be with solid particle, liquid droplet or gas as capsular core material, outside it, form one deck continuously and the process of thin microcapsule wall.Through microcapsule technology phylloxanthin is processed cold water dispersion type dry powder; Can be in cold water or normal-temperature water homodisperse; Increased its range of application, avoided phylloxanthin to contact simultaneously, kept its stability in transportation, storage and use with the direct of environment; And phylloxanthin is an amorphous form in these microcapsule dry powder, helps the absorption of human body utilization.Under the intravital specified conditions effect of people, when the wall material dissolved, melts or breaks, core discharged, and utilization is absorbed by the body.
Foreign patent about this technology: US 6863914; Open day: on March 5th, 2005; Disclose a kind of stable aqueous dispersions of phylloxanthin class material and the method for preparing that stable water can disperse dried powder, this method is dissolved in phylloxanthin in the mixed liquor of organic solvent and water earlier, again with the aqueous solution of mixed liquor and protective colloid; Carry out spray drying behind the high pressure homogenize, obtain the cold water dispersion type xanthophyll powder.This method with an organic solvent owing to organic solvent residual, makes it to be unfavorable in medicine, food industry applications; And (pressure carries out under high temperature (170～200 ℃) 2～8MPa), stable unfavorable to phylloxanthin to adopt high pressure equipment in this homogenizing process; High to equipment requirements; The operation, control difficulty big, energy consumption is big, is not inconsistent with scientific development direction now.
At number of patent application 200610049837.0; Name is called among " Xanthin micro-capsule and preparation method thereof " (open day on JIUYUE 12nd, 2007, publication number 101032683A), discloses a kind of method for preparing of Xanthophyll micro-capsule; The microencapsulation technology that is provided; Adopt two-step method, earlier phylloxanthin is mixed with micropore starch or crosslinking microporous starch, add cellulose family, saccharide, eucolloid class or proteinic aqueous solution again; Make colloid through mechanical lapping or homogenizing, again colloid is carried out spray drying and make microcapsule.
This method adopts the mode of mechanical lapping to prepare colloid, makes the wayward and operation of process, does not use emulsifying agent; Be difficult to guarantee colloidally evenly make the spray drying operation easier big, influence embedding rate; And the raw material type that this method is used is many, the products obtained therefrom complicated component.
Summary of the invention
The object of the present invention is to provide a kind of cold water dispersion type xanthophyll micro-capsule, selecting edible modified starch and eucolloid is the wall material, makes water as solvent, does not contain organic solvent, and composition is simple, and chemical property is stable.
Another object of the present invention is to provide the method for preparing of above-mentioned microcapsule; Adopt one-step method directly phylloxanthin core, wall material, emulsifying agent and water to be mixed; Carry out emulsifying through the control temperature; Refilter, adopt spray drying method the phylloxanthin mixed solution to be prepared into the solid microscapsule powder of semi permeability or sealing.
The technical scheme that the present invention adopted is, cold water dispersion type xanthophyll micro-capsule is made up of following composition:
Core: phylloxanthin powder;
Wall material: form by modified starch 20%～90% and eucolloid 10%～80% by weight percentage;
Emulsifying agent: tween is serial, OP is serial, span is serial.
Wherein, the weight ratio of core, wall material and emulsifying agent is 0.5～2.0: 5.0～9.0: 0.5～3.0.
Another technical scheme that the present invention adopted is, the method for preparing of above-mentioned microcapsule is carried out according to the following steps:
A. be 0.5～2.0: 5.0～9.0 with weight ratio: 0.5～3.0 gets core, wall material and emulsifying agent respectively, and its mesospore material is made up of 20%～90% modified starch and 10%～80% eucolloid by weight percentage;
B. above-mentioned raw materials is mixed, add the water of 3～15 times of mixture total weight amounts;
C. with the mixture heated of step b, stirred 1～8 hour down for 30 ℃～80 ℃ in temperature, and control 300～600 rev/mins of rotating speeds, filter;
D. filtrating is carried out spray drying, promptly obtain the cold water dispersion type xanthophyll micro-capsule powder.
The present invention is solvent with water, does not have organic problem of solvent residue, and gained Xanthin micro-capsule dry powder particle size is 1～100um, even particle distribution, and water solublity is good, stability is high, strong coloring force, bag reason rate is high.The raw material that uses is few, and technical process is simple, and technical process does not have waste liquid, waste pollution; Use equipment is few, easy operating, and production cost is low, suitable realization industrialization.
The specific embodiment
Below in conjunction with specific embodiment the present invention is elaborated.
Cold water dispersion type xanthophyll micro-capsule of the present invention; With the phylloxanthin powder is core; Do the wall material with modified starch and eucolloid, and add emulsifying agent and water, control ratio is: the weight ratio of core, wall material and emulsifying agent is 0.5～2.0: 5.0～9.0: 0.5～3.0; Wherein, the wall material is made up of 20%～90% modified starch and 10%～80% eucolloid by weight percentage.The preferred sodium alginate of eucolloid, arabic gum or gelatin, emulsifying agent select tween series, OP is serial or span is serial.
It is the wall material that the present invention selects natural edible modified starch and eucolloid; The characteristics such as adsorptivity, permeability, dissolubility, hygroscopicity and adhesion strength of utilizing these materials to have; The wall material of forming can be effectively with phylloxanthin absorption and embedding under the effect of emulsifying agent; Make the microcapsule phylloxanthin of preparation keep the inherent character of phylloxanthin, and changed some unfavorable characteristic, and make water as solvent in the preparation process; Thereby avoided the use of organic solvent, made the preparation that is prepared into safer human body.
The present invention adds emulsifying agent in raw material, the effect that emulsifying agent is played therein is: 1) protection raw material; 2) make phylloxanthin disperse more evenly, need not processes such as grinding; 3) association rate of raw material and protective colloid is increased; 4) can also play material liquid in dry run and remain steady statue, not have deposition and lamination, thereby guarantee spray-diredly to carry out smoothly.Therefore, the Xanthophyll micro-capsule good water solubility that the present invention makes, stability is high, and embedding rate is high.
Xanthophyll micro-capsule of the present invention, can adopt following method to prepare:
A. be 0.5～2.0: 5.0～9.0 with weight ratio: 0.5～3.0 gets core, wall material and emulsifying agent respectively, and its mesospore material is made up of 20%～90% modified starch and 10%～80% eucolloid by weight percentage;
B. above-mentioned raw materials is mixed, and add the water of 3～15 times of mixture total weight amounts;
C. with the mixed system heating of step b, under 30 ℃～80 ℃ of temperature, stirred fast 1～8 hour, 300～600 rev/mins of control rotating speeds filter;
D. the filtrating that will filter gained carry out spray-dried powdersization, promptly obtains cold water dispersion type xanthophyll micro-capsule.
Spray drying step wherein, using the spray drying device controlled pressure is 1～10Mpa, and inlet temperature is 120 ℃～200 ℃, and outlet temperature is 50 ℃～100 ℃.
Resulting cold water dispersion type xanthophyll micro-capsule is a yellow powder, and particle diameter is 1～100um, can in normal-temperature water, dissolve, and forms stable orange-yellow dispersion liquid.
Employed raw material is simple and easy among the present invention, all can be used for food, medicine and health product in a large number, not with an organic solvent; The natural sex that has kept phylloxanthin does not use high-temperature high-pressure apparatus, and equipment is simple; Be convenient to operation, be easy to control the particle diameter and the embedding rate of Xanthophyll micro-capsule, process is simple; Help keeping the intrinsic color and luster of phylloxanthin, the cold water dispersion type xanthophyll micro-capsule chemical property of gained is stable.
Embodiment 1
Get 100 gram phylloxanthin powder, 360 gram modified starches, 1440 gram gelatin, 100 gram OP-10 mixing; Add the water of 12 times of above mixture total weight amounts, stirred 5 hours down at 60 ℃, the control rotating speed is at 500 rev/mins; After cooling; Solution is filtered, and filtrating is carried out the spray powder drying under the condition of spray dryer pressure 8Mpa, 170 ℃ of inlet temperatures, 80 ℃ of outlet temperatures, and promptly getting mean diameter is 70 μ m cold water dispersion type xanthophyll micro-capsule powder.
The stability of sample test data that below obtains for embodiment 1:
| Test period (moon) | Outward appearance | Cold water dispersion type xanthophyll content (%) | |
| 0±2℃ | 25±2℃ | ||
| 0 | The crocus fine powder | 10.21 | 10.20 |
| 1 | The crocus fine powder | 10.21 | 10.19 |
| 2 | The crocus fine powder | 10.19 | 10.17 |
| 3 | The crocus fine powder | 10.18 | 10.16 |
| 4 | The crocus fine powder | 10.18 | 10.14 |
| 5 | The crocus fine powder | 10.16 | 10.13 |
| 6 | The crocus fine powder | 10.16 | 10.11 |
Be capsular experimental result below for gelatin/modified starch/OP-10 prepares phylloxanthin
| Phylloxanthin (g) | Modified starch (g) | Gelatin (g) | OP-10(g) | Content (%) | Particle diameter (μ m) |
| ?100 | ?600 | 200 | 100 | 8.1 | ?70 |
| ?100 | ?400 | 400 | 100 | 8.5 | ?70 |
| ?100 | ?200 | 600 | 100 | 9.1 | ?50 |
| ?60 | ?200 | 600 | 100 | 5.1 | ?50 |
| ?90 | ?200 | 600 | 100 | 8.3 | ?50 |
| ?120 | ?200 | 600 | 100 | 11.1 | ?60 |
| ?150 | ?200 | 600 | 100 | 13.5 | ?70 |
| ?180 | ?200 | 600 | 100 | 15.9 | ?70 |
| ?100 | ?200 | 600 | 60 | 9.7 | ?80 |
| ?100 | ?200 | 600 | 90 | 9.2 | ?50 |
| ?100 | ?200 | 600 | 120 | 9.0 | ?50 |
| ?100 | ?200 | 600 | 150 | 8.8 | ?40 |
| ?100 | ?200 | 600 | 180 | 8.5 | ?30 |
Embodiment 2
Get 100 gram phylloxanthin powder, 1170 gram modified starches, 130 gram sodium alginates, 600 gram polysorbate60s mixing; Add the water of 3 times of above mixture total weight amounts, stirred 1 hour down at 80 ℃, the control rotating speed is at 300 rev/mins; After cooling; Solution is filtered, and filtrating is carried out the spray powder drying under the condition of spray dryer pressure 1Mpa, 200 ℃ of inlet temperatures, 100 ℃ of outlet temperatures, and promptly getting mean diameter is 100 μ m cold water dispersion type xanthophyll micro-capsule powder.
The experimental result that below prepares Xanthophyll micro-capsule for sodium alginate/modified starch/polysorbate60
| Phylloxanthin (g) | Modified starch (g) | Sodium alginate (g) | Polysorbate60 (g) | Content (%) | Particle diameter (μ m) |
| 100 | 540 | 180 | 200 | 7.0 | 100 |
| 100 | 480 | 240 | 200 | 7.5 | 100 |
| 100 | 360 | 360 | 200 | 8.4 | 70 |
| 100 | 240 | 480 | 200 | 8.2 | 80 |
| 60 | 360 | 360 | 200 | 5.1 | 60 |
| 120 | 360 | 360 | 200 | 10.2 | 70 |
| 160 | 360 | 360 | 200 | 14.3 | 90 |
| 200 | 360 | 360 | 200 | 16.9 | 100 |
| 100 | 360 | 360 | 60 | 10.5 | 100 |
| 100 | 360 | 360 | 100 | 9.8 | 80 |
| 100 | 360 | 360 | 150 | 9.3 | 60 |
| 100 | 360 | 360 | 200 | 8.8 | 60 |
| 100 | 360 | 360 | 250 | 8.0 | 50 |
| 100 | 360 | 360 | 300 | 7.6 | 50 |
Embodiment 3
Get 400 gram phylloxanthin powder, 400 gram modified starches, 600 gram arabic gums, 600 gram sorbester p17s mixing; Add the water of 15 times of above mixture total weight amounts, stirred 8 hours down at 30 ℃, the control rotating speed is at 600 rev/mins; After cooling; Solution is filtered, and filtrating is carried out the spray powder drying under the condition of spray dryer pressure 10Mpa, 120 ℃ of inlet temperatures, 50 ℃ of outlet temperatures, and promptly getting mean diameter is 60 μ m cold water dispersion type xanthophyll micro-capsule powder.
Be capsular experimental result below for arabic gum/modified starch/sorbester p17 prepares phylloxanthin
| Phylloxanthin (g) | Modified starch (g) | Arabic gum (g) | Sorbester p17 (g) | Content (%) | Particle diameter (μ m) |
| 100 | 700 | 100 | 100 | 7.7 | 80 |
| 100 | 500 | 300 | 100 | 8.1 | 80 |
| 100 | 300 | 500 | 100 | 9.1 | 50 |
| 60 | 300 | 500 | 100 | 4.9 | 40 |
| 90 | 300 | 500 | 100 | 8.4 | 50 |
| 120 | 300 | 500 | 100 | 11.0 | 50 |
| 150 | 300 | 500 | 100 | 13.3 | 70 |
| 180 | 300 | 500 | 100 | 15.8 | 80 |
| 100 | 300 | 500 | 60 | 9.3 | 80 |
| 100 | 300 | 500 | 90 | 9.0 | 60 |
| 100 | 300 | 500 | 120 | 8.9 | 50 |
| 100 | 300 | 500 | 150 | 8.6 | 40 |
| 100 | 300 | 500 | 180 | 8.4 | 40 |
Claims (4)
1. water-dispersion type Xanthophyll micro-capsule, form by following composition:
Core: phylloxanthin powder;
The wall material: be made up of modified starch 20%～90% and eucolloid 10%～80% by weight percentage, eucolloid is sodium alginate, arabic gum or gelatin;
Emulsifying agent: polysorbate60, OP-10 or sorbester p17;
Wherein, the weight ratio of core, wall material and emulsifying agent is 0.5～2.0: 5.0～9.0: 0.5～3.0.
2. the method for preparing of the said Xanthophyll micro-capsule of claim 1 is characterized in that, this method is carried out according to the following steps,
A. be 0.5～2.0: 5.0～9.0 with weight ratio: 0.5～3.0 gets core, wall material and emulsifying agent respectively, and the wall material is made up of 20%～90% modified starch and 10%～80% eucolloid by weight percentage;
B. above-mentioned raw materials is mixed, add the water of 3～15 times of mixture total weight amounts;
C. with the mixture heated of step b, stirred 1～8 hour down for 30 ℃～80 ℃ in temperature, and control 300～600 rev/mins of rotating speeds, filter;
D. filtrating is carried out spray drying, promptly obtain the cold water dispersion type xanthophyll micro-capsule powder.
3. according to the described method for preparing of claim 2, it is characterized in that in the described spray drying step, controlled pressure is 1～10Mpa, inlet temperature is 120 ℃～200 ℃, and outlet temperature is 50 ℃～100 ℃.
4. according to the described method for preparing of claim 2, it is characterized in that described eucolloid is sodium alginate, arabic gum or gelatin.
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| CN101921495B (en) * | 2009-06-12 | 2013-04-24 | 中国中化股份有限公司 | Method for preparing lutein oleoresin microcapsule |
| CN101817998B (en) * | 2010-04-23 | 2012-09-26 | 华南师范大学 | Method for preparing purple sweet potato pigment microcapsules |
| CN102784600B (en) * | 2012-08-04 | 2014-12-24 | 盐城工学院 | Preparation method of lutein microcapsule |
| CN105072926B (en) * | 2013-03-28 | 2019-04-05 | 帝斯曼知识产权资产管理有限公司 | It is suitble to the lutein composition of infant food preparation |
| CN103193693A (en) * | 2013-04-26 | 2013-07-10 | 辽宁省农业科学院食品与加工研究所 | Preparation process of marigold lutein |
| CN103406079B (en) * | 2013-06-28 | 2016-07-06 | 大连医诺生物有限公司 | Do not use the method that organic solvent prepares cold water dispersion type carotenoid micro-capsule powder |
| CN103349287B (en) * | 2013-07-15 | 2015-04-22 | 佛山职业技术学院 | Method for microencapsulating pitaya peel pigment |
| CN106307492B (en) * | 2016-08-19 | 2019-08-30 | 华侨大学 | A kind of yeast microcapsules of lutein and preparation method thereof |
| JP2024509226A (en) * | 2021-12-28 | 2024-02-29 | 大▲連▼医▲諾▼生物股▲ふん▼有限公司 | Carotenoid preparations, preparation methods, and their applications |
| CN115251376A (en) * | 2022-07-28 | 2022-11-01 | 青岛康小鹿生物科技有限公司 | Lutein ester nano microcapsule and preparation method thereof |
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