CN1836652A - Water-dispersed carotenoid powder preparation method - Google Patents
Water-dispersed carotenoid powder preparation method Download PDFInfo
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- CN1836652A CN1836652A CNA2005100494322A CN200510049432A CN1836652A CN 1836652 A CN1836652 A CN 1836652A CN A2005100494322 A CNA2005100494322 A CN A2005100494322A CN 200510049432 A CN200510049432 A CN 200510049432A CN 1836652 A CN1836652 A CN 1836652A
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Abstract
The improved water soluble carotenoid powder preparing process includes the following steps: dissolving crude carotenoid in halohydrocarbon or ester solvent containing antioxidant and emulsifier, spraying into alcohol or isopropanol under stirring to separate out amorphous carotenoid powder, filtering out the separated carotenoid with filter film or sintered filter rod, washing the filter cake with alcohol or isopropanol, filtering, adding the filter cake into water solution of protecting colloid and stirring to pulp, homogenize and emulsify, eliminating residual solvent to prepare water dispersed solution, spraying to pelletize, and fluidizing to dry. The said process has easy elimination of solvent, less residue, high efficiency, and easy control of grain size and color of the carotenoid product.
Description
Technical field
The present invention relates to the preparation of carotenoid powder, specifically a kind of preparation method of water-dispersed carotenoid powder.
Background technology
Carotenoid extensively is present in occurring in nature, and its most important representative is beta-carotene, astaxanthin, canthaxanthin.For food, cosmetics, feedstuff, pharmaceuticals industry, these materials are important coloring agent.In addition, some in them still are the precursor of vitamin A.Carotenoid is water insoluble, and dissolubility is also very little in oil, and most of carotenoid to heat, oxygen is responsive, therefore can't be directly with coarse-grained crystal and very difficultly absorbed by animal.No matter be to use, generally all need carotenoid is existed with fine particulate form, and need to protect, with the opposing oxidation with protective colloid at food or in other field.And, wish that carotenoid can improve bioavailability after preparationization for to be colored as the purpose purposes, and to improve coloring effect, reduce consumption, reduce the loss in the use.
In use, often need carotenoid is made the dispersible preparation of water.For this purpose, more existing reported in literature the preparation method of this class preparation.
WO91/06292 and WO94/19411 have introduced and have used colloid mill that beta-carotene is ground to form the microgranule of 2～10 μ m, and drying is made the carotenoid powder of aqueous dispersion then.But polishing efficient is low, energy consumption is big, and the carotenoid particle diameter is difficult to reach below the 1 μ m.
US3998753 has put down in writing the dispersible carotenoid preparation method of a kind of water, wherein the granularity of carotenoid is less than 1 μ m, this method is the solution that elder generation is made into carotenoid and other additives organic solvent, join then in the aqueous solution that contains gelatin, dispersant, stabilizing agent, make system form emulsion through high speed shear; Remove organic solvent, spray drying obtains required powder.
The method of the carotenoid powder of the preparation aqueous dispersion that EP-0065193 (or US4522743) is put down in writing; be that carotenoid was dissolved in 10 seconds in the mixable solvent of volatile water in 50～200 ℃; descend and the aqueous solution rapid mixing that contains protecting colloid in 0～50 ℃ then; carotenoid promptly with the size dispersion of＜0.5 μ m in protecting colloid; remove solvent, drying can get carotenoid powder.(pressure carries out 3.0～6.0MPa), under the high temperature (170～200 ℃) this arts demand, and to the equipment requirements height, operation, control difficulty are big at high pressure equipment.
Above solvent method or high-temperature solvent method all need to remove a large amount of solvents contained in the system in protecting colloid; required time is long; be difficult for removing clean; and in the presence of protecting colloid, heat precipitation; system is very easily bubbled; efficient during precipitation is very low, the particle diameter of wayward required carotenoid powder and color and luster.
Summary of the invention
Technical problem to be solved by this invention is to overcome the defective that above-mentioned prior art exists, and provides that a kind of solvent easily removes, the also preparation method of the water-dispersed carotenoid powder of required particle diameter easy to control and color and luster.
For this reason, the present invention is by the following technical solutions: the preparation method of water-dispersed carotenoid powder, it is characterized in that may further comprise the steps: 1) the carotenoid coarse crystallization is dissolved in the halogenated hydrocarbons or esters solvent that contains antioxidant, emulsifying agent, the solution of gained joins in the ethanol or isopropyl alcohol of stirring with Sprayable, and carotenoid is separated out with the amorphous powder form; 2) filter the carotenoid of separating out with filter membrane or sintering filter stick, filter cake is with ethanol or washed with isopropyl alcohol, and filter is done; 3) described filter cake adding is contained in the aqueous solution of protecting colloid, first stirring to pulp after emulsifying then removes residual solvent, is made aqueous dispersions then; 4) with the nebulization pelletize of described dispersion liquid, get final product through fluidized drying again.Core of the present invention is that the carotenoid solutions that will contain antioxidant, dispersant earlier joins in the ethanol or isopropyl alcohol of high-speed stirred with the form of high-pressure pump with spraying, carotenoid is separated out with the form of amorphous powder, control the granularity and the color and luster of the carotenoid powder of separating out by the concentration of regulating carotenoid solutions, the size of spraying droplet, the speed of stirring, low concentration, droplet be little, stir the fast little carotenoid powder of granularity that all helps forming.The particle diameter of the water-dispersed carotenoid powder that the present invention finally obtains is at＜2 μ m.
The preparation method of described water-dispersed carotenoid powder, the speed controlling of stirring is at 〉=500 rev/mins.
The preparation method of described water-dispersed carotenoid powder, the aperture of filter membrane or sintering filter stick is less than 0.3 μ m.
The preparation method of described water-dispersed carotenoid powder, halogenated hydrocarbons are dichloromethane, chloroform or dichloroethanes.
The preparation method of described water-dispersed carotenoid powder, esters are ethyl acetate, propyl acetate, isopropyl acetate or butyl acetate.
The preparation method of described water-dispersed carotenoid powder, emulsifying agent are fatty glyceride or span.
The preparation method of described water-dispersed carotenoid powder, antioxidant are ethoxyquin or tocopherol.
The preparation method of described water-dispersed carotenoid powder, protecting colloid are gelatin, isinglass or modified starch.
The preparation method of described water-dispersed carotenoid powder, carotenoid are beta-carotene, astaxanthin or canthaxanthin.
The invention has the beneficial effects as follows: operate without high pressure equipment and under normal condition substantially, equipment requirements is low, operates, controls simple relatively; Easily remove solvent, less residue removes soon the efficient height; The particle diameter of required carotenoid easy to control and color and luster.
Below in conjunction with embodiment the present invention is described in detail.
The specific embodiment
Embodiment 1
100g astaxanthin coarse crystallization, 10g ethoxyquin, 20g stearic acid monoglycerides are dissolved in the 3L dichloromethane, make astaxanthin solution.Be furnished with high-speed stirred at 50L and (add 20L ethanol in 〉=500rpm) the still, open stirring, slowly join in the still through shower nozzle with the form of spraying above-mentioned astaxanthin solution with high-pressure pump then, regulate spray velocity, so that the diameter of the amorphous astaxanthin particle of being separated out＜2 μ m, having sprayed the back is the filter filtration of the microporous filter membrane of 0.3 μ m with the aperture, the filter cake washing with alcohol, press dry, and promptly gets astaxanthin amorphous powder (the mean diameter 0.9 μ m) filter cake of super-refinement.With above-mentioned filter cake with contain in the aqueous solution that 300g gelatin, 100g sucrose, 10gVC sodium salt, 2500ml water be made into, stirring to pulp, homogenize 5 hours in high pressure homogenisers then, emulsified dispersed liquid elder generation vacuum precipitation, pelletize in the mist projection granulating device then, fluid bed drying promptly gets the water dispersible astaxanthin powder of astaxanthin-containing 12.1%.
Embodiment 2
With 50g beta-carotene coarse crystallization, 10g tocopherol, the heating of 10g Arlacel-60 is dissolved in the 2L butyl acetate, makes beta-carotene solution.Be furnished with at 50L and add 20L isopropyl alcohol, 2L water in the still of high-speed stirred (3500rpm), open stirring, with high-pressure pump above-mentioned beta-carotene solution is slowly joined in the still with Sprayable then, regulate spray velocity, make precipitation particles diameter＜2 μ m.Sintering filter stick with micro-pore diameter 0.3 μ m filters, and filter cake 90% isopropyl alcohol is washed, and press dry, and gets beta-carotene amorphous powder (the mean diameter 0.7 μ m) filter cake of super-refinement.With above-mentioned filter cake with contain in the aqueous solution of 200g modified starch, 5gVC sodium salt, 1500ml water group, stirring to pulp, homogenize 10 hours in high pressure homogenisers then, emulsified dispersed liquid is mist projection granulating behind precipitation, fluid bed drying promptly gets the water dispersible β-Radix Dauci Sativae powder that contains beta-carotene 10.5%.
Embodiment 3
100g canthaxanthin coarse crystal, 20g tocopherol, 10g ethoxyquin, the heating of 15g Arlacel-40 are dissolved in the 3L chloroform wiring solution-forming.Be furnished with at 50L and add 20L95% ethanol in the still of high-speed stirred, open stirring, with high-pressure pump the form of above-mentioned solution with spraying slowly joined in the still then, regulate spray velocity, make the precipitation particles diameter less than 2 μ m.With micro-pore diameter is the sintering filter stick filtration of 0.3 μ m, and 95% ethanol filter wash cake press dry, and getting mean diameter is the canthaxanthin filter cake of 0.55 μ m.With above-mentioned filter cake with contain in the aqueous solution that 300g isinglass, 100g sucrose, 20gVC sodium salt, 2500ml water be made into, stirring to pulp, homogenize 5 hours in high pressure homogenisers then, emulsified dispersed liquid vacuum removal residual solvent, mist projection granulating, fluidized drying promptly get the water dispersible Mylabris bloom of content 11.3%.
Claims (10)
1, the preparation method of water-dispersed carotenoid powder, it is characterized in that may further comprise the steps: 1) the carotenoid coarse crystallization is dissolved in the halogenated hydrocarbons or esters solvent that contains antioxidant, emulsifying agent, the solution of gained joins in the ethanol or isopropyl alcohol of stirring with Sprayable, and carotenoid is separated out with the amorphous powder form; 2) filter the carotenoid of separating out with filter membrane or sintering filter stick, filter cake is with ethanol or washed with isopropyl alcohol, and filter is done; 3) described filter cake adding is contained in the aqueous solution of protecting colloid, first stirring to pulp after emulsifying then removes residual solvent, is made aqueous dispersions then; 4) with the nebulization pelletize of described dispersion liquid, get final product through fluidized drying again.
2, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that controlling the particle diameter of the carotenoid powder of separating out＜2 μ m by the concentration of regulating carotenoid solutions, the size of spraying droplet, the speed of stirring.
3, the preparation method of water-dispersed carotenoid powder according to claim 1, the speed controlling that it is characterized in that described stirring is at 〉=500 rev/mins.
4, the preparation method of water-dispersed carotenoid powder according to claim 1, the aperture that it is characterized in that described filter membrane or sintering filter stick is less than 0.3 μ m.
5, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described halogenated hydrocarbons is dichloromethane, chloroform or dichloroethanes.
6, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described esters is ethyl acetate, propyl acetate, isopropyl acetate or butyl acetate.
7, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described emulsifying agent is fatty glyceride or span.
8, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described antioxidant is ethoxyquin or tocopherol.
9, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described protecting colloid is gelatin, isinglass or modified starch.
10, the preparation method of water-dispersed carotenoid powder according to claim 1 is characterized in that described carotenoid is beta-carotene, astaxanthin or canthaxanthin.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100494322A CN100421650C (en) | 2005-03-23 | 2005-03-23 | Water-dispersed carotenoid powder preparation method |
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| CNB2005100494322A CN100421650C (en) | 2005-03-23 | 2005-03-23 | Water-dispersed carotenoid powder preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010111912A1 (en) * | 2009-03-30 | 2010-10-07 | 浙江新和成股份有限公司 | Method of preparing nano-dispersed high-all-trans-carotenoid microcapsules |
| CN102773052A (en) * | 2012-08-09 | 2012-11-14 | 沈阳天峰生物制药有限公司 | Method for preparing cold-water-dispersible carotenoid micro-capsule product |
| CN104146988A (en) * | 2014-07-04 | 2014-11-19 | 浙江新维普添加剂有限公司 | Method for preparing high-all-trans finely-dispersible carotenoid preparation |
| CN104274428A (en) * | 2013-07-09 | 2015-01-14 | 浙江新维普添加剂有限公司 | Preparation method for oil-dispersible carotenoid preparation |
| CN111903846A (en) * | 2020-07-31 | 2020-11-10 | 浙江新和成股份有限公司 | Stable carotenoid microcapsule with high bioavailability and preparation method thereof |
| CN114287625A (en) * | 2021-12-28 | 2022-04-08 | 大连医诺生物股份有限公司 | Carotenoid preparation and application thereof |
| CN115349630A (en) * | 2022-06-20 | 2022-11-18 | 海宁凤鸣叶绿素有限公司 | Preparation method of water-dispersible lutein microcapsule powder |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2234957C (en) * | 1995-10-17 | 2006-12-19 | Inge B. Henriksen | Insoluble drug delivery |
| EP0807431B1 (en) * | 1996-05-14 | 2004-03-24 | DSM IP Assets B.V. | Process for the manufacture of carotenoid compositions |
| DE19637517A1 (en) * | 1996-09-13 | 1998-03-19 | Basf Ag | Production of powdered, cold water dispersible carotenoid preparations and the use of the new carotenoid preparations |
-
2005
- 2005-03-23 CN CNB2005100494322A patent/CN100421650C/en active Active
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8540908B2 (en) | 2009-03-30 | 2013-09-24 | Zhejiang Nhu Company Ltd. | Method of preparing nano-dispersed high-all-trans-carotenoid microcapsules |
| DE112010000006T5 (en) | 2009-03-30 | 2012-06-21 | Beijing University Of Chemical Technology | Process for the preparation of nano-dispersed high-all-trans carotenoid microcapsules |
| WO2010111912A1 (en) * | 2009-03-30 | 2010-10-07 | 浙江新和成股份有限公司 | Method of preparing nano-dispersed high-all-trans-carotenoid microcapsules |
| DE112010000006B4 (en) * | 2009-03-30 | 2013-05-08 | Beijing University Of Chemical Technology | Process for the preparation of nano-dispersed high-all-trans carotenoid microcapsules |
| CN102773052B (en) * | 2012-08-09 | 2015-02-04 | 沈阳天峰生物制药有限公司 | Method for preparing cold-water-dispersible carotenoid micro-capsule product |
| CN102773052A (en) * | 2012-08-09 | 2012-11-14 | 沈阳天峰生物制药有限公司 | Method for preparing cold-water-dispersible carotenoid micro-capsule product |
| CN104274428A (en) * | 2013-07-09 | 2015-01-14 | 浙江新维普添加剂有限公司 | Preparation method for oil-dispersible carotenoid preparation |
| WO2015003536A1 (en) | 2013-07-09 | 2015-01-15 | 浙江新维普添加剂有限公司 | Method for preparing oil-dispersible carotenoid preparation |
| CN104274428B (en) * | 2013-07-09 | 2016-04-13 | 浙江新维普添加剂有限公司 | The preparation method of oil-dispersing property carotenoid formulation |
| JP2016523933A (en) * | 2013-07-09 | 2016-08-12 | ゼァージァン ニュー ウェイプ アディティブ カンパニー リミテッド | Process for producing oil-dispersible carotenoid formulations |
| CN104146988A (en) * | 2014-07-04 | 2014-11-19 | 浙江新维普添加剂有限公司 | Method for preparing high-all-trans finely-dispersible carotenoid preparation |
| CN111903846A (en) * | 2020-07-31 | 2020-11-10 | 浙江新和成股份有限公司 | Stable carotenoid microcapsule with high bioavailability and preparation method thereof |
| CN111903846B (en) * | 2020-07-31 | 2023-10-31 | 浙江新和成股份有限公司 | Stable carotenoid microcapsule with high bioavailability and preparation method thereof |
| CN114287625A (en) * | 2021-12-28 | 2022-04-08 | 大连医诺生物股份有限公司 | Carotenoid preparation and application thereof |
| CN114287625B (en) * | 2021-12-28 | 2024-04-05 | 大连医诺生物股份有限公司 | Carotenoid preparation and application thereof |
| CN115349630A (en) * | 2022-06-20 | 2022-11-18 | 海宁凤鸣叶绿素有限公司 | Preparation method of water-dispersible lutein microcapsule powder |
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