CN103315370A - A stable method for microencapsulating carotenoid - Google Patents
A stable method for microencapsulating carotenoid Download PDFInfo
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- CN103315370A CN103315370A CN2013102004360A CN201310200436A CN103315370A CN 103315370 A CN103315370 A CN 103315370A CN 2013102004360 A CN2013102004360 A CN 2013102004360A CN 201310200436 A CN201310200436 A CN 201310200436A CN 103315370 A CN103315370 A CN 103315370A
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- 235000012682 canthaxanthin Nutrition 0.000 claims description 14
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- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 claims description 3
- 235000013793 astaxanthin Nutrition 0.000 claims description 3
- 239000001168 astaxanthin Substances 0.000 claims description 3
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 claims description 3
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Abstract
The invention discloses a stable method for microencapsulating carotenoid. The method comprises 1) a step of completely dissolving a protecting colloid, sucrose or glucose, ascorbyl palmitate and EDTA into water, and adjusting pH to 10-11 to obtain a water phase A; 2) a step of completely dissolving carotenoid and an antioxidant into a solvent to obtain an oil phase B; 3) a step of adding the oil phase B into the water phase A under a condition of high-speed shearing and high-speed stirring; emulsifying the mixture to form an initial emulsion by stirring at a high speed; and heating and removing the solvent to obtain a microemulsion; and 4) a step of adding the obtained microemulsion into a spray drying system; and obtaining carotenoid particles or powder after spray drying. The carotenoid particles or powder prepared by the method have advantages of good dispersibility, high stability, good light permeability and small particle sizes.
Description
Technical field
The present invention relates to the preparation method of a Carotenoids particle or powder, particularly relate to a kind of microencapsulation method of stable carotenoid.
Background technology
At present, carotenoid, beta carotene for example, canthaxanthin, astaxanthin etc. is familiar with by people as the important function of feed coloring agent, food color or food additives.In recent years, a lot of reports about the carotenoid function have been arranged.But carotenoid is water-fast material, and fusing point is high, and to light, heat, oxygen sensitivity.These characteristics of carotenoid are unfavorable for the painted of water-bearing media especially, and this is because its water insolubility, thus to reach homogeneous or fully strong coloring effect be extremely difficult.And for canthaxanthin (canthaxanthin), these characteristics, particularly water insolubility make it only have extremely limited biological effectiveness in containing the pharmaceutical dosage form of described carotenoid.In addition, because the canthaxanthin crystal can only seldom can be absorbed the coloring effect that maybe can only give extreme difference, so above-mentioned these performances also hinder it to be directly used in the painted of animal yolk, skin or food.
From document, can understand the whole bag of tricks for the preparation of the dispersible carotenoid compositions of water, but these methods there is some defective.
As in European patent application EP-0065193B1, put down in writing the method for the finely divided carotenoid powder of a kind of continuous production, wherein the carotenoid grain graininess is at 0.5 micron.With this carotenoid in 50-200 ℃ of organic solvent that is dissolved in the volatile water solubility.Under 0-50 ℃, form emulsion by the aqueous solution rapid mixing with the swelling colloid, make powder by spray-drying again.
Number be in the patent of invention of " 97110894 " in Chinese patent application; put down in writing a kind of method for preparing carotenoid compositions; the aqueous suspension of carotenoid and protective colloid is heated to 180 ℃-250 ℃ makes this carotenoid fusing; then by the high-pressure homogeneous emulsion that obtains, obtain the carotenoid powder by drying again.
The defective that said method exists is: temperature is higher in the process conditions, and effective absorption that this has caused the loss of carotenoid and has affected animal because carotenoid is at high temperature extremely unstable, very easily occurs to decompose or isomerization.And the particle diameter of the emulsion carotenoid of these method preparations is larger.In addition, the higher waste that also causes the energy of temperature.
Summary of the invention
For the deficiencies in the prior art; the objective of the invention is for a kind of microencapsulation method of stable carotenoid is provided; adopt the carotenoids crude granule of the method preparation or powder to have good dispersion, stability is high, translucidus good and grain diameter is little characteristics, and have obvious low-cost characteristics.
Purpose of the present invention adopts following technical scheme:
A kind of microencapsulation method of stable carotenoid is characterized in that carrying out according to the following steps:
1) protecting colloid, sucrose or glucose, vitamin(e) C palmitate, EDTA are dissolved in the water fully, then regulate pH to 10-11; Obtain water A;
2) carotenoid, antioxidant are dissolved in the solvent fully, obtain oil phase B;
3) under the high condition that stirs of high shear, with step 2) the oil phase B of gained joins among the water A of step 1) gained, and the weight ratio of oil phase B and water A is 223.5-381.5:178.5-186.5; Form colostrum through high-speed stirred emulsification, then heat up and remove solvent, obtain microemulsion; Wherein, the gained microemulsion is a kind of microemulsion of Subnano-class, and its average grain diameter is 130-200nm, and the pH of microemulsion is 9-10;
4) microemulsion with the step 3) gained adds in the spray drying system, through after the spray-drying, makes carotenoids crude granule or powder; The average grain diameter of carotenoid is 130-200nm in gained carotenoids crude granule or the powder.
Realize that purpose of the present invention can also reach by taking following technical scheme:
Realization one embodiment of the present invention are: the carotenoid content in described carotenoids crude granule or the powder accounts for the 1%-18% of particle gross weight.
Realization one embodiment of the present invention are: in step 1), described water A comprises the component of following weight portion: 33.5 parts of protecting colloids, sucrose or glucose 43.3-51.3 part, 1.5 parts of vitamin(e) C palmitates (VC palmitate), EDTA(ethylenediamine tetra-acetic acid) 100 parts of 0.2 parts, water.
Realization one embodiment of the present invention are: in step 1), described protecting colloid is gelatin.
Realization one embodiment of the present invention are: in step 1), regulate pH with 20%NaOH solution, PH is controlled at 10.4 ± 0.2.
Realization one embodiment of the present invention are: in step 2) in, described oil phase B comprises the component of following weight portion: carotenoid 10.5-18 part, antioxidant 3-3.5 part and solvent 210-360 part.
Realization one embodiment of the present invention are: in step 2) in, described carotenoid is one or more the mixing in beta carotene, canthaxanthin (canthaxanthin), APOESTER, astaxanthin, luteole, the lycopene etc.Described carotenoid is natural or artificial synthetic, has very strong pigmentation, and above-mentioned carotenoid can use separately or mix use, and this is mainly determined by the color of needs.
Realization one embodiment of the present invention are: in step 2) in, described solvent is carrene or chloroform.
Realization one embodiment of the present invention are: in step 3), the high stirring of high shear refers to: shearing power is 0.5-100Kw, and mixing speed is 2900-18000 rev/min; Mixing time is 15 minutes, is warming up to 50 ℃.
Realization one embodiment of the present invention are: in step 4), described spray drying device is a kind of mist projection granulating tower, is provided with the cornstarch that circulates in the mist projection granulating tower; The gained microemulsion mixes with cornstarch after pumping into the mist projection granulating tower, through after the spray-drying, makes carotenoids crude granule or powder, contains the cornstarch of 15%-35% in the particle.
Among the present invention:
EDTA is residual micro heavy in the complexing water or in the supplementary material effectively.
Gelatin is the water soluble protein mixture, collagen in skin, ligament, the tendon is through acid or alkali partial hydrolysis or boil in water and produce, crisp or meal shape that colourless or little Huang is transparent, swelling forms gel (moisture for conducting oneself with dignity 5～10 times) in 35～40 ℃ of water, is widely used as packaging material in the preparation of microcapsules.The effect that gelatin plays in technique is:
Crosslinked action: the chief component of gelatin is that amino acid forms identical and peptide molecule mixture that molecular weight distribution is very wide, and molecular weight is generally several ten thousand to tens0000.Be staggered in without several peptide chains and form together network structure, have very strong embedding ability.Its core mechanism is Maillard reaction, the amino in the Amino Acids in Proteins molecule and the carbonyl generation Maillard reaction in the reduced sugar, thus occur crosslinked.
The emulsifying agent effect: a large amount of hydroxyls is arranged on the gelatin molecule structure, also have in addition many carboxyls and amino, this is so that gelatin has extremely strong hydrophily and lipophile.Therefore gelatin is a kind of good emulsifying agent.
Good water dispersible packaging material: carotenoids crude granule or the powder of preparation have good water dispersible take gelatin as packaging material among the present invention, can form emulsion homogeneous, stable, light-permeable in water.
In the technique that the present invention relates to, the pH of water also is an important influence factor, and final emulsion equals 7.0 or be unsettled when following at pH.In addition, the particle of being made by spray-drying by emulsion or powder equal 7.0 or also be unsettled when following at pH, and the translucidus for its aqueous solution also has adverse effect simultaneously.Therefore, the pH of water should be controlled at 10-11, and the best is 10.4 ± 0.2.In this this water scope, the pH of final emulsion is about 9-10.Carotenoids crude granule or the powder of this technique preparation have higher stability, translucidus.
Beneficial effect of the present invention is:
1, in the whole technical process of the present invention; adopted lower temperature 50 C; the pH of water A should be controlled at 10-11; the best is 10.4 ± 0.2; in this water scope; the pH of final emulsion is about 9-10, so that carotenoids crude granule or the powder of preparation have higher stability, translucidus.The present invention has been applied to has the high emulsifier unit that stirs (2900-18000rpm) and high shear force.High shear, high to stir for obtaining little emulsion droplet be vital, and emulsion droplet is less, behind the solvent flashing in the microemulsion particle diameter of carotenoid also less.The average grain diameter of carotenoid is between 130-200nm in the microemulsion for preparing under these process conditions.Simultaneously, carotenoids crude granule or powder that the present invention prepares take gelatin as packaging material have good water dispersible, can form emulsion homogeneous, stable, light-permeable in water.
2, prepared particle or powder very easily disperse in water, the formation homogeneous, light-permeable, red liquid has significant pigmentation, is widely used in food, yolk, zoodermic painted.
Description of drawings
Fig. 1 is the size distribution schematic diagram of the canthaxanthin of the specific embodiment of the invention 1.
Fig. 2 is the size distribution schematic diagram of the beta carotene of the specific embodiment of the invention 2.
The specific embodiment
Specific embodiment 1:
A kind of microencapsulation method of stable carotenoid, carry out according to the following steps:
1, with the 33.5g gelatin, 43.3g sucrose, 1.5gVc palmitate, 0.2gEDTA are dissolved in the 100.0g water fully, form the water A of homogeneous, regulate pH to 10.0-10.5 with 20%NaOH solution.
2, with 18.0g canthaxanthin crystal, the 3.0g ethoxyquin, 0.5gVE oil is dissolved in the 360.0g carrene, is stirred to fully dissolving, obtains oil phase B.
3, stir under the condition of high shear at height, oil phase B is joined among the water A, then then emulsification 15 minutes under the mixing speed of 2900-18000rpm be warming up to 50 ℃ and remove solvents, forms microemulsion.Wherein, the gained microemulsion is a kind of microemulsion of Subnano-class, and its average grain diameter is 130-200nm, and the pH of microemulsion is 9-10; High stirring high shear refers to: shearing power is 0.5-100Kw, and mixing speed is 2900-18000 rev/min.
4, in the mist projection granulating tower, be provided with the cornstarch that circulates; The gained microemulsion mixes with cornstarch after pumping into the mist projection granulating tower, through after the spray-drying, makes the canthaxanthin particle, contains the cornstarch of 15%-35% in the particle.
With reference to table 1 and Fig. 1, account for 10.8% of particle gross weight through canthaxanthin in the canthaxanthin particle of above technique preparation, washing out content with carrene is that the absorbance value of 0.03%, 1% aqueous solution is 1250, and carrene remnants are less than 1ppm, and average grain diameter is 166nm.Grain size analysis is reported as follows:
The grain size analysis of canthaxanthin report in the table 1 canthaxanthin microcapsules
In Fig. 1: d[0.1]: 0.124um, d[0.5]: 0.166um, d[0.9]: 0.222um.
Specific embodiment 2:
1, with the 33.5g gelatin, 51.g sucrose, 1.5gVc palmitate, 0.2gEDTA are dissolved in the 100.0g water fully, form the water of homogeneous, regulate pH to 10.0-10.5 with 20%NaOH solution.
2, with 10.5g beta carotene crystal, 1.0gBHT, 2.0gVE oil is dissolved in the 210.0g chloroform, is stirred to fully dissolving.
3, stir under the condition of high shear at height, oil phase B is joined among the water A, then then emulsification 15 minutes under the mixing speed of 2900-18000rpm be warming up to 50 ℃ and remove solvents, forms microemulsion.Wherein, the gained microemulsion is a kind of microemulsion of Subnano-class, and its average grain diameter is 130-200nm, and the pH of microemulsion is 9-10; High stirring high shear refers to: shearing power is 0.5-100Kw, and mixing speed is 2900-18000 rev/min.
4, above-mentioned microemulsion is made the beta carotene particle by spray-drying.
With reference to table 2 and Fig. 2, in the particle through the beta carotene of above technique preparation-and carrotene accounts for 10.3% of particle gross weight, and washing out content with chloroform is that the absorbance value of 0.02%, 1% aqueous solution is 1028, chloroform remnants are less than 1ppm, and average grain diameter is 175nm.Grain size analysis is reported as follows:
The grain size analysis of beta carotene report in the table 2 beta carotene particle
In Fig. 2: d[0.1]: 0.130um, d[0.5]: 0.175um, d[0.9]: 0.240um.
For a person skilled in the art, can make other various corresponding changes and distortion according to technical scheme described above and design, and these all changes and distortion should belong within the protection domain of claim of the present invention all.
Claims (10)
1. the microencapsulation method of a stable carotenoid is characterized in that carrying out according to the following steps:
1) protecting colloid, sucrose or glucose, vitamin(e) C palmitate, EDTA are dissolved in the water fully, then regulate pH to 10-11; Obtain water A;
2) carotenoid, antioxidant are dissolved in the solvent fully, obtain oil phase B;
3) under the high condition that stirs of high shear, with step 2) the oil phase B of gained joins among the water A of step 1) gained, and the weight ratio of oil phase B and water A is 223.5-381.5:178.5-186.5; Form colostrum through high-speed stirred emulsification, then heat up and remove solvent, obtain microemulsion; Wherein, the gained microemulsion is a kind of microemulsion of Subnano-class, and its average grain diameter is 130-200nm, and the pH of microemulsion is 9-10;
4) microemulsion with the step 3) gained adds in the spray drying system, through after the spray-drying, makes carotenoids crude granule or powder; The average grain diameter of carotenoid is 130-200nm in gained carotenoids crude granule or the powder.
2. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: the carotenoid content in described carotenoids crude granule or the powder accounts for the 1%-18% of particle gross weight.
3. the microencapsulation method of a kind of stable carotenoid according to claim 1; it is characterized in that: in step 1), described water A comprises the component of following weight portion: 100 parts in 33.5 parts of protecting colloids, sucrose or glucose 43.3-51.3 part, 1.5 parts of vitamin(e) C palmitates, EDTA0.2 part, water.
4. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: in step 1), described protecting colloid is gelatin.
5. the microencapsulation method of a kind of stable carotenoid according to claim 1 is characterized in that: in step 1), regulate pH with 20%NaOH solution, PH is controlled at 10.4 ± 0.2.
6. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: in step 2) in, described oil phase B comprises the component of following weight portion: carotenoid 10.5-18 part, antioxidant 3-3.5 part and solvent 210-360 part.
7. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: in step 2) in, described carotenoid is one or more the mixing in beta carotene, canthaxanthin, APOESTER, astaxanthin, luteole, the lycopene.
8. the microencapsulation method of a kind of stable carotenoid according to claim 1 is characterized in that: in step 2) in, described solvent is carrene, chloroform, acetone, isopropyl alcohol.
9. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: in step 3), the high stirring of high shear refers to: shearing power is 0.5-100Kw, and mixing speed is 2900-18000 rev/min; Mixing time is 15 minutes, is warming up to 50 ℃.
10. the microencapsulation method of a kind of stable carotenoid according to claim 1, it is characterized in that: in step 4), described spray drying device is a kind of mist projection granulating tower, is provided with the cornstarch that circulates in the mist projection granulating tower; The gained microemulsion mixes with cornstarch after pumping into the mist projection granulating tower, through after the spray-drying, makes carotenoids crude granule or powder, contains the cornstarch of 15%-35% in the particle.
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