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CN103406079A - Method for preparing cold water dispersing type carotenoid micro-capsule powder without using organic solvent - Google Patents

Method for preparing cold water dispersing type carotenoid micro-capsule powder without using organic solvent Download PDF

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CN103406079A
CN103406079A CN2013103927630A CN201310392763A CN103406079A CN 103406079 A CN103406079 A CN 103406079A CN 2013103927630 A CN2013103927630 A CN 2013103927630A CN 201310392763 A CN201310392763 A CN 201310392763A CN 103406079 A CN103406079 A CN 103406079A
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carotenoid
cold water
organic solvent
emulsion
protective colloid
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CN103406079B (en
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吴文忠
陈剑彬
王建华
陈碧聪
吕忠武
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Dalian promise biological Limited by Share Ltd
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DALIAN INNOBIOACTIVES Co Ltd
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Abstract

The invention provides a method for preparing cold water dispersing type carotenoid micro-capsule powder without using an organic solvent. The method concretely comprises the following steps: (a) enabling carotenoid crystal to suspend in a water solution containing antioxidant, protective colloid and at least one non-ionic emulsifier; (b) grinding and homogenizing the solution obtained in the step (a) under the nitrogen protection to enable crystal particles to be ground and stably suspend; (c) carrying out micronization on the suspended particles of the obtained solution by a heating device to form an emulsion; (d) dissolving the protective colloid into the emulsion obtained in the step (c), carrying out secondary embedding, dewatering and drying to obtain powder particles. The method can solubilize carotenoid without using the organic solvent or vegetable oil, thus solving the problems of residual solvent, low carrying capacity and the like caused by the existing solvent method and a high temperature melting method. In all the steps of the method, the organic solvent is not used, so that the method is environment-friendly in technology; the process of high-temperature treatment is not needed, so that trans isomer is not produced, and the method is high in carrying capacity and small in loss of active ingredients.

Description

With an organic solvent do not prepare the method for cold water dispersion type carotenoid microcapsule powder
Technical field
The present invention relates to a kind of method that does not with an organic solvent prepare cold water dispersion type carotenoid microcapsule powder, more particularly, the method prepares a kind of cold water dispersion instant, the stable carotenoid microcapsule powder of active component.And this technique is abandoned the shortcoming of organic solvent or oil phase high-temperature fusion method, more is conducive to food security.
Background technology
Carotenoid is the general name of the important natural colouring matter of a class, is prevalent in animal, higher plant, fungi and algae.Carotenoid is the isoprenoid polymer that contains 40 carbon.Carotenoid has formed one group of color from the yellow to the redness, except a few carotenoid such as phytoene, phytofluene are colourless, most carotenoid is yellow, orange or red, their color changes because the number of conjugated double bond is different, the number of conjugated double bond is more, and color is more shifted to redness.Up to now, found natural carotenoid has reached kind more than 700, according to the difference of chemical constitution, it can be divided into to two classes, a class is carrotene (as beta carotene, lycopene), and another kind of is lutein (as lutein, zeaxanthin, astaxanthin).
Carotenoid is the main source of vitamin A in human body.Carotenoid is water insoluble, in fat or oils, also only have extremely low dissolving, and these carotenoid is extremely unstable to light, oxygen, heat etc.Therefore these limited dissolubilities and to the hypersensitivity of environment, hindered the direct application of its product at food, medicine, feedstuff industry.And the carotenoid absorption of human body of the coarse crystallization form of natural structure is difficulty comparatively, and bioavilability is extremely low.While as colouring agent, using, Color does not produce a desired effect yet.People seek the configuring technical of various ways to solve the application of carotenoid.Especially carotenoid is made to cold water-dispersible powderous preparations, broader application makes it become welcome addition manner.And existing more following documents are explored in this field.
US 2861891 is dissolved in carotenoid high temperature (140 ℃～150 ℃) in vegetable oil, and this immiscible material and colloid aqueous solution emulsification, spray-drying are made to dry powder.But carotenoid solubility in vegetable oil is limited, limit it and prepared the more microcapsule powder product of high-load, and add vegetable oil in the carotenoid microcapsule powder, the heating of carrying out high temperature like this also can cause the alltrans isomers obviously to descend, and the problem such as product poor fluidity, surperficial oil impregnate, crushing resistance be poor.
CN 1942106A provides the method for producing carotenoid dry powder, and carotenoid crystals is suspended in the isopropanol/water azeotropic mixture, and dissolves at the temperature of the pressure of 55 bar and 165 ℃.Then with the aqueous solution emulsification of casein sodium and trehalose, concentrated and drying.Although the method can make the carotenoid crystals particle diameter remain on the level of 100～200nm, but there is the mixed emulsion of a large amount of organic solvents and water-soluble colloid in its preparation process, cause the colloid sex change, the product water dissolubility descends, embedding rate reduces, thereby affects the cold water-dispersible energy of product and the stability of active component.
CN 1836652A provides a kind of preparation method of water-dispersed carotenoid powder, that the carotenoid coarse crystal is dissolved in the halogenated hydrocarbons or esters solvent that contains emulsifying agent, antioxidant, and be sprayed in ethanol or isopropyl alcohol, the carotenoid that filtration washing is separated out adds homogeneous in colloid aqueous solution, then is spray dried to powder.The standby complex technical process of this legal system; need to use a large amount of organic solvents; when organic solvent and protective colloid aqueous solution precipitation, system is very easily bubbled; wayward in production; although in the method provided than CN1942106A, quantity of solvent reduces, but still can cause the molten residual problem of organic solvent in finished product.
Summary of the invention
The invention provides a kind of method that does not with an organic solvent prepare cold water dispersion type carotenoid microcapsule powder, the method is abandoned the method for above-mentioned organic solvent solubilising and high-temperature fusion, and can realize carotenoid content higher in microcapsule formulation, cold water-dispersible, and higher stability rapidly.
The objective of the invention is to be realized by following technical scheme.
A kind of method that does not with an organic solvent prepare cold water dispersion type carotenoid microcapsule powder of the present invention, comprise the steps:
A) carotenoid crystals is suspended in the aqueous solution that contains antioxidant, protective colloid and at least a nonionic emulsifier;
B) carotenoid crystals suspension step a) obtained grinds under nitrogen protection, homogeneous, and crystal grain is pulverized and stable suspersion;
C) by step b) the carotenoid crystals stable suspension by firing equipment miniaturization suspended particulate, form emulsion, crystal is amorphous;
D) protective colloid is dissolved in step c) gained emulsion and carries out the secondary embedding, then dehydrate powdered particle.
In the present invention, described nonionic emulsifier derives from food, medicine surfactant.Preferably one or more mixtures that form with arbitrary proportion that are selected from sucrose fatty ester, polyglyceryl fatty acid ester, polysorbate, single double glyceride, phosphatide.The mixture that one or more in preferably sucrose fatty acid ester, polyglyceryl fatty acid ester, polysorbate, single bi-tristearin form with arbitrary proportion.A kind of or two or more mixtures that form with arbitrary proportion in sucrose fatty ester, polysorbate, single double glyceride most preferably.
Described sucrose fatty ester, also claim fatty acid cane sugar ester, sucrose ester, and being called for short SE (SUGAR ESTERS) is simple substance or the mixture generated through esterification by sucrose and aliphatic acid.Comprise sucrose stearate, sucrose oleate, sucrose palmitate, Surfhope SE Cosme C 1216, its hydrophilic lipophilic balance (HLB value) preferably 6～16.
Described polyglyceryl fatty acid ester, also claim polyglycerol ester, comprises that the degree of polymerization is at trimerization to ten poly-oleic acid, stearic acid, lauric fatty acid ester.Its hydrophilic lipophilic balance (HLB value) preferably 8～18.
Described polysorbate, i.e. polyoxyethylene sorbitan fatty acid ester.
Described single double glyceride, comprise glyceryl monolaurate, single, double tristerin, the mixture of one or more arbitrary proportions in single, double olein.
In the present invention, step is mass ratio preferably 0.01～20:1, the more preferably 0.01～10:1 of described nonionic emulsifier and carotenoid crystals a).
In the present invention, described protective colloid is selected from Arabic gum, xanthans, carragheen modified starch, gelatin, casein sodium, soybean protein isolate, whey isolate protein, sodium alginate etc.The mixture of one or both arbitrary proportions in the preferred Arabic gum of the present invention, modified starch.The mass ratio of protective colloid and carotenoid crystals is 40～2:1.
To be that acacia gum is refining form described Arabic gum, or through the Arabic gum of octenyl succinic acid anhydride (OSA) modification.
Described modified starch is the natural origin starch that octenyl succinic acid anhydride (OSA) was processed, and comprises corn, waxy corn, cassava, barley, wheat etc.
In the present invention, described carotenoid is one or more mixtures that form with arbitrary proportion in beta carotene, lutein, zeaxanthin, lycopene, astaxanthin, kryptoxanthin, capsorubin, cantharides xanthin.In microcapsule powder of the present invention, the preferred class carotene carotene content is 1～20%.
In cold water-dispersible carotenoid microcapsule powder of the present invention not special requirement contain or do not contain filler.Contain and filler applicatory comprises the starch derivatives such as maltodextrin, oligomeric maltose, corn syrup, monosaccharide and disaccharide, polysaccharide etc.
In the present invention, in the grinding described in step b), the mode that preferably adopts ball mill or sand mill to grind.
In the present invention, preferably 90～140 ℃ of the heating-up temperatures described in step c), heat time heating time preferred 2s～60s.
In the present invention, in the drying described in step d), preferably adopt the mode of spray-drying or the fluidized drying of spray starch bed.
Another object of the present invention is to provide the cold water dispersion type carotenoid microcapsule powder prepared by said method.The cold water dispersion type carotenoid microcapsule powder that method of the present invention obtains, its active component particle diameter, between 100-400nm, are the microcapsule granules that jitter time is less than 20 seconds in water.
The preparation method of cold water dispersion type carotenoid microcapsule powder of the present invention, grind the mixed liquor of carotenoid coarse crystal and emulsifying agent, so that the carotenoid crystals miniaturization, its crystal diameter is less than 0.6 micron.Preferably the mass ratio of nonionic emulsifier and carotenoid crystals is 0.01～10:1, and appropriate emulsifying agent plays vital effect to the dispersion of crystal grain, and it prevents the reunion of micro crystal.Otherwise, cause the invalid enforcement of process of lapping.In addition, protective colloid and emulsifying agent be combined to form special hydrophilic wetting surface structure, and guarantee the outstanding cold water-dispersible of micro-capsule product of the present invention.
But carotenoid microcapsule powder of the present invention is a kind of Subnano-class carotenoid cold water dispersion type microcapsule powder, the size of emulsion particle diameter after the quality of emulsification formula has directly determined to grind, and milling apparatus and firing equipment coupling more can further reduce the particle diameter of emulsion between 100-400nm.The carotenoid microcapsule powder product of making in this way not only can disperse and can reach cold water instant dissolving by cold water.The more important thing is that less particle diameter can guarantee that product physical aspect in actual application keeps stable, thereby more be conducive to its commercialization.
Beneficial effect of the present invention:
1. the preparation method of cold water dispersion type carotenoid microcapsule powder of the present invention, in whole step not with an organic solvent, the technique environmental protection, no solvent residue, more be conducive to food security.
2. preparation method of the present invention, without pyroprocess, add without vegetable oil, avoids the carotenoid cis-trans isomerism to carry out, and the product embedding rate is high.
3. the cold water dispersion type carotenoid microcapsule powder for preparing of method of the present invention has the cold water dispersion instant more more outstanding than conventional products, and its particle diameter, between 100-400nm, is conducive to human body and absorbs fast.
4. carotenoid microcapsule powder good stability of the present invention, test through the product accelerated stability, and product content is stable, is applicable to the several formulations form.
The accompanying drawing explanation
Fig. 1. the accelerated stability test result of cold water dispersion type lycopene microcapsule powder
The specific embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.If no special instructions, the experimental technique used is conventional method, and material therefor, reagent etc. all can be bought from biological or chemical company.
Following embodiment described " in water dispersed " refers to that cold water dispersion type carotenoid microcapsule granule, to the speed of disperseing in water, is also the speed of wetting of particulates " sinking ".And by following determination of experimental method: get the 150ml beaker, and add wherein 25 ℃ of water of 100ml, standing 15～45s in water without bubble, water surface calmness.Sample thief 2g (being accurate to 0.01g) is poured into water rapidly from beaker central authorities tops 50mm, and the timing sample all wetting also " sinkings " to the time at glass end, record required time T(s), i.e. jitter time in water.
Embodiment 1
100g lutein crystal, 11g sucrose stearate, 2g d-alpha tocopherol, 3g glyceryl monolaurate, 49g Arabic gum are placed in to 1000ml water, are warming up to 40 ℃, be stirred to crystal dispersion suspension homogeneous, obtain the lutein suspension; Under nitrogen protection, with sand mill circular grinding 120min, homogeneous, crystal grain is pulverized and stable suspersion this suspension; This lutein crystal stable suspension is passed through to pipeline heater, heter temperature is at 125 ± 2 ℃, time 25s, make the more miniaturization of crystal suspended particulate, form emulsion, emulsion Lutein crystal particle diameter is 260nm (D50), after emulsion is cooled to 60 ℃, add Arabic gum 400g, oligomeric maltose 100g is stirred to fully and dissolves, and the gained emulsion is spray dried to dry powder, more further the agglomeration granulation makes the cold water dispersion type xanthophyll microcapsule powder, its lutein content is 11.3%, and wherein trans-lutein content is greater than 92.0%.In water, jitter time is 8s.
Embodiment 2
By 123g beta carotene crystal, 10g polyoxyethylene sorbitan monoleate, the mono-bi-tristearin of 6g, 96g modified starch (Hi Cap100 is provided by National Starch USA), the 6gdl-alpha tocopherol is placed in 2200ml water, be warming up to 46 ℃, be stirred to crystal dispersion suspension homogeneous, obtain the beta carotene suspension; Under nitrogen protection, with ball mill circular grinding 120min, homogeneous, crystal grain is pulverized and stable suspersion this suspension; This beta carotene crystalchecked suspension is passed through to pipeline heater, heter temperature is at 113 ℃, and time 43s, make the more miniaturization of crystal suspended particulate, form emulsion, in emulsion, the beta carotene crystal particle diameter is 120nm (D50), after emulsion is cooled to 40 ℃, adds modified starch 620g, oligomeric maltose 70g is stirred to fully and dissolves, the gained emulsion is spray dried to dry powder, the final cold water dispersion type beta-carotin microcapsule powder that obtains, and its content beta-carotene is 12.8%.In water, jitter time is 6s.
Embodiment 3
By 62g lycopene crystal, 5g polyglyceryl fatty acid ester, the mono-bi-tristearin of 3g, 9g mixed tocopherol, 113g modified starch (Hi Cap100 is provided by National Starch USA) are placed in 1900ml water, be warming up to 43 ℃, be stirred to crystal dispersion suspension homogeneous, obtain the lycopene crystal suspension; Under nitrogen protection, with sand mill circular grinding 120min, homogeneous, pulverize and stable suspersion crystal grain by this suspension; This lycopene crystalchecked suspension is passed through to pipeline heater, heter temperature is at 123 ℃, time 35s, make the more miniaturization of crystal suspended particulate, form emulsion, in emulsion, the lycopene crystal particle diameter is 380nm (D50), after emulsion is cooled to 40 ℃, add modified starch 790g, oligomeric maltose 170g is stirred to fully and dissolves, and the gained emulsion adopts centrifugal atomizer to spray in starch bed, and separating starch obtains thick product particle, further drying makes the cold water dispersion type microcapsule particle again, and its content of lycopene is 5.23%.In water, jitter time is 11s.And product stability is good.
Embodiment 4
By 87g zeaxanthin crystal, 5.4g polyglyceryl fatty acid ester, the mono-bi-tristearin of 3.2g, 9.1g mixed tocopherol, 120g modified starch (Hi Cap100 is provided by National Starch USA) are placed in 1200ml water, be warming up to 43 ℃, be stirred to crystal dispersion suspension homogeneous, obtain the zeaxanthin crystal suspension; Under nitrogen protection, with sand mill circular grinding 120min, homogeneous, pulverize and stable suspersion crystal grain by this suspension; This zeaxanthin crystalchecked suspension is passed through to pipeline heater, heter temperature is at 133 ℃, time 15s, make the more miniaturization of crystal suspended particulate, form emulsion, in emulsion, the zeaxanthin crystal particle diameter is 450nm (D50), after emulsion is cooled to 40 ℃, add modified starch 860g, be stirred to fully and dissolve, the gained emulsion adopts centrifugal atomizer to spray in starch bed, and separating starch obtains thick product particle, further drying makes the cold water dispersion type microcapsule particle again, and its zeaxanthin content is 5.61%.In water, jitter time is 8s.And product stability is good.
Embodiment 5 cold water dispersion type lycopene microcapsule powder accelerated stability tests
Cold water dispersion type lycopene microcapsule powder prepared by the method for employing embodiment 3, carry out accelerated test, detects its stability.
With reference to " Chinese pharmacopoeia 2005 editions, appendix XIXC bulk drug and pharmaceutical preparation stability test guideline.
Concrete grammar is: lycopene microcapsule powder opening is placed in to suitable clean container, placed 15 days under 60 ℃, in sampling every day, detect by stability high spot reviews project content of lycopene.The results are shown in Figure 1.
As shown in Figure 1, the lycopene microcapsule powder made by method of the present invention was placed 15 days in 60 ℃, open containers, in whole standing time, content of lycopene does not have to change substantially, after 15 days, also well keep original (0 day) content, the lycopene excellent stability of method microencapsulation of the present invention is described.
Embodiment 6 cold water dispersion type lycopene microcapsule powders contrast with the lycopene high-temperature stability of not microencapsulation
Adopt the cold water dispersion type lycopene microcapsule powder (sample 1) of embodiment 3 preparations and the lycopene of microencapsulation (sample 2) not to carry out the high temperature accelerated test, contrast its stability.
Concrete grammar: the two contrast product 5g that takes a sample respectively is placed in to surface plate, is paved into the thin layer that 1～2mm is thick, then be placed in 6h in 105 ℃ of hot bellows, per hour measure content one time, result such as table 1.
Table 1. lycopene microcapsule powder and the not high-temperature stability contrast of the lycopene of microencapsulation
Figure BDA0000374988180000081
As shown in Table 1, cold water dispersion type lycopene microcapsule powder (sample 1) prepared by method of the present invention is after high temperature is placed 6 hours, content of lycopene does not have to change substantially, its degradation rate is less than 10%, and in contrast to this, the lycopene of microencapsulation is not under identical condition, its content of lycopene significantly reduces, degradation rate reaches more than 50%, illustrates that lycopene is with after method microencapsulation of the present invention, and its stability significantly increases.

Claims (9)

1. a method that does not with an organic solvent prepare cold water dispersion type carotenoid microcapsule powder, is characterized in that, comprises the steps:
A) carotenoid crystals is suspended in the aqueous solution that contains antioxidant, protective colloid and at least a nonionic emulsifier;
B) carotenoid crystals suspension step a) obtained grinds under nitrogen protection, homogeneous, and crystal grain is pulverized and stable suspersion;
C) by step b) carotenoid crystals stablize suspension by firing equipment miniaturization suspended particulate, form emulsion;
D) protective colloid is dissolved in step c) gained emulsion and carries out the secondary embedding, dehydrate powdered particle.
2. method according to claim 1, is characterized in that, described nonionic emulsifier is one or more mixtures that form with arbitrary proportion in sucrose ester, polyglyceryl fatty acid ester, polysorbate, single double glyceride.
3. method according to claim 1 and 2, is characterized in that, the nonionic emulsifier of step described in a) and the mass ratio of carotenoid crystals are 0.01～20:1.
4. method according to claim 1, is characterized in that, described protective colloid is one or both mixtures that form with arbitrary proportion in Arabic gum, modified starch.
5. method according to claim 1, it is characterized in that, described carotenoid crystals is one or more mixtures that form with arbitrary proportion in beta carotene, lutein, zeaxanthin, lycopene, astaxanthin, fucoxanthine, kryptoxanthin, capsorubin, cantharides xanthin.
6. method according to claim 1, is characterized in that, ball mill or sand mill are adopted in the grinding described in step b).
7. method according to claim 1, is characterized in that, the heating-up temperature described in step c) is 90～140 ℃, heat time heating time 2s～60s.
8. method according to claim 1, is characterized in that, the drying described in step d) adopts spray-drying or the fluidized drying of spray starch bed.
9. the cold water dispersion type carotenoid microcapsule powder for preparing of method as described as any one of claim 1～8.
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