CN101548962A - Preparation method of lutein microcapsule - Google Patents
Preparation method of lutein microcapsule Download PDFInfo
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- CN101548962A CN101548962A CNA2009100265514A CN200910026551A CN101548962A CN 101548962 A CN101548962 A CN 101548962A CN A2009100265514 A CNA2009100265514 A CN A2009100265514A CN 200910026551 A CN200910026551 A CN 200910026551A CN 101548962 A CN101548962 A CN 101548962A
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Abstract
The invention relates to a preparation method of the lutein microcapsule with the advantages of simple operation, low costs and high purity. the preparation method comprises the following processing steps of: taking marigold flowers, adding 0.5 to 3 times amount water and 0.005 to 0.1 times amount cellulose, fermenting for 10 to 30 hours under the condition of 30 to 60 DEG C, adding 2 to 30 times amount ethanol, adjusting the PH with NaOH to be alkaline, heating reflux, filtering while hot, adjusting the PH with HCl to be neutral, decompressing and recycling the ethanol, adding the liquid into the macroporous absorption resin column, eluting impurity with water, eluting with 30 to 90% ethanol, collecting eluate, concentrating, adding hexane, methanol, and water with appropriate amount, refrigerating, completely crystallizing, separating the crystallization, washing , drying, grinding, passing 100 mesh sieve, adding modified starch, gelatin and water to make suspension, colloidal milling, and spray drying. The industrialization amplification is easily realized by using the method for preparing the lutein microcapsule.
Description
Technical field
The present invention relates to a kind of preparation method of Xanthin micro-capsule, especially a kind of method of from marigold flower, extracting phylloxanthin and preparing its microcapsule.
Background technology
Phylloxanthin (lutein) belongs to carotenoid, extensively is present in the crops such as Flos Tagetis Erectae, corn, Brassica oleracea L.var.capitata L., Herba Spinaciae, Caulis et Folium Lactucae sativae, Semen phaseoli radiati, Brassica campestris L, and be a kind of natural pigment, its lovely luster, strong coloring force, good in oxidation resistance, the safety non-toxic evil has abundant nutritive value.Be widely used in a plurality of fields such as food, health product, cosmetics, medicine, Nicotiana tabacum L. and moving bird feed.
Show that according to Physiologic Studies phylloxanthin can prevent senile eyeball macula retinae to degenerate visual deterioration that (AMD) cause is with blind, and is particularly useful to the old people.If can in food, in time replenish phylloxanthin, can delay generation the eyes degenerative disorders.
Phylloxanthin character instability is very easily decomposed under naturalness, and the therefore general in the world mode of making microcapsule that adopts is isolated with itself and air.
In the prior art, extract phylloxanthin and mainly adopt saponification and extract method separately, technology is loaded down with trivial details, the production cost height, and product purity is low.
Summary of the invention
Technical problem to be solved by this invention provide a kind of easy and simple to handle, production cost is low, the preparation method of stay-in-grade Xanthin micro-capsule.
For solving the problems of the technologies described above, the present invention adopts following technical proposal:
Get marigold flower, add the cellulase that water that 0.5-3 doubly measures and 0.005-0.1 doubly measure, 30-60 ℃ of condition bottom fermentation 10-30 hour, add 2-30 and doubly measure ethanol, regulate pH to alkalescence, the heating cocurrent flow with NaOH, filtered while hot is regulated pH to neutral with HCl, decompression recycling ethanol, medicinal liquid adds on the macroporous adsorptive resins, the water elution remove impurity, the 30-90% ethanol elution is collected eluent, concentrate, it is an amount of to add normal hexane-methanol-water, and cold preservation makes crystallization complete, fractional crystallization, washing, pulverize, cross 100 mesh sieves, add modified starch, gelatin, water is made suspension, colloid mill is milled, and spray drying promptly.
The condition of fermentation technology is as follows: get marigold flower, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours.
Refluxing with concentration of ethanol is 90%, and consumption is 20 times of amounts.
Regulate pH to 13 with NaOH before refluxing.
The model of macroporous adsorbent resin is a kind of among H-1020, X-5, AB-8, H-103, D-101, DA-201, DS-401, the DM-301.
The eluting concentration of ethanol is 70%.
Crystallization is a normal hexane with the ratio of normal hexane-methanol-water: methanol: water=2: 1: 0.5.
The ratio of suspension is a phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3.
Adopt technique scheme to prepare Xanthin micro-capsule, easy and simple to handle, pollute less, equipment drops into for a short time, is beneficial to big production operation.
Below in conjunction with the specific embodiment the present invention is further elaborated, but the scope of protection of present invention is not limited to following embodiment.
The specific embodiment
Embodiment 1
Get marigold flower 10Kg, add the water of 0.5 times of amount and the cellulase of 0.005 times of amount, 60 ℃ of condition bottom fermentations 30 hours, add 2 times of amount 90% ethanol, regulate pH to 14, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the X-5 type macroporous adsorptive resins, the water elution remove impurity, 90% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 76.3g, detects through HPLC, and its content is 31.3%.
Embodiment 2
Get marigold flower 10Kg, add the water of 3 times of amounts and the cellulase of 0.1 times of amount, 30 ℃ of condition bottom fermentations 10 hours, add 30 times of amount 90% ethanol, regulate pH to 10, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the H-1020 type macroporous adsorptive resins, the water elution remove impurity, 30% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 81.6g, detects through HPLC, and its content is 42.5%.
Embodiment 3
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the AB-8 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 79.8g, detects through HPLC, and its content is 44.2%.
Embodiment 4
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the H-103 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 71.2g, detects through HPLC, and its content is 40.1%.
Embodiment 5
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the D-101 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 77.7g, detects through HPLC, and its content is 41.5%.
Embodiment 6
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the DA-201 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 73.3g, detects through HPLC, and its content is 40.1%.
Embodiment 7
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the DS-401 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 74.7g, detects through HPLC, and its content is 42.23%.
Embodiment 8
Get marigold flower 10Kg, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours, add 20 times of amount 90% ethanol, regulate pH to 13, reflux 4 hours with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression is with receiving ethanol, and medicinal liquid adds on the DM-301 type macroporous adsorptive resins, the water elution remove impurity, 70% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water (2: 1: 0.5), cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, promptly get the phylloxanthin fine powder, in phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3 ratio is made suspension, colloid mill is milled, spray drying promptly gets Xanthin micro-capsule 74.8g, detects through HPLC, and its content is 43.5%.
Claims (8)
1, a kind of preparation method of Xanthin micro-capsule is characterized in that described method comprises the following steps: to get marigold flower, the cellulase that water that adding 0.5-3 doubly measures and 0.005-0.1 doubly measure, 30-60 ℃ of condition bottom fermentation 10-30 hour, add 2-30 and doubly measure ethanol, regulate pH to alkalescence, reflux with NaOH, filtered while hot, regulate pH to neutral with HCl, decompression recycling ethanol, medicinal liquid add on the macroporous adsorptive resins, the water elution remove impurity, the 30-90% ethanol elution is collected eluent, concentrates, it is an amount of to add normal hexane-methanol-water, cold preservation makes crystallization complete, fractional crystallization, washing, dry, pulverize, cross 100 mesh sieves, add modified starch, gelatin, water is made suspension, colloid mill is milled, and spray drying promptly.
2, the preparation method of a kind of Xanthin micro-capsule according to claim 1 is characterized in that the condition of described fermentation technology is as follows: get marigold flower, add the water of 1 times of amount and the cellulase of 0.01 times of amount, 50 ℃ of condition bottom fermentations 20 hours.
3, the preparation method of a kind of Xanthin micro-capsule according to claim 1 is characterized in that described backflow concentration of ethanol is 90%, and consumption is 20 times of amounts.
4, the preparation method of a kind of Xanthin micro-capsule according to claim 1 is characterized in that described alkalescence is pH=13.
5, the preparation method of a kind of Xanthin micro-capsule according to claim 1, the model that it is characterized in that described macroporous adsorbent resin are a kind of among H-1020, X-5, AB-8, H-103, D-101, DA-201, DS-401, the DM-301.
6, the preparation method of a kind of Xanthin micro-capsule according to claim 1 is characterized in that described eluting concentration of ethanol is 70%.
7, the preparation method of a kind of Xanthin micro-capsule according to claim 1, the ratio that it is characterized in that described normal hexane-methanol-water is a normal hexane: methanol: water=2: 1: 0.5.
8, the preparation method of a kind of Xanthin micro-capsule according to claim 1, the ratio that it is characterized in that described suspension is a phylloxanthin: modified starch: gelatin: water=5: 3: 2: 3.
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| CNA2009100265514A CN101548962A (en) | 2009-05-12 | 2009-05-12 | Preparation method of lutein microcapsule |
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| CNA2009100265514A CN101548962A (en) | 2009-05-12 | 2009-05-12 | Preparation method of lutein microcapsule |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103735616A (en) * | 2014-01-20 | 2014-04-23 | 大连医诺生物有限公司 | Microencapsulated preparation for protecting eyesight and preparation method thereof |
| CN104738643A (en) * | 2015-03-03 | 2015-07-01 | 深圳市妍倩科技有限公司 | Food with antioxidant function |
| CN107495372A (en) * | 2017-09-27 | 2017-12-22 | 广州市范乐医药科技有限公司 | A kind of preparation method of Xanthophyll micro-capsule |
| CN107669657A (en) * | 2016-08-02 | 2018-02-09 | 浙江医药股份有限公司新昌制药厂 | A kind of preparation method high-stability microencapsulated containing more double bond fat soluble nutrient |
| CN111548294A (en) * | 2020-04-10 | 2020-08-18 | 天津大学 | Lutein methanol solvate crystal and preparation method thereof |
-
2009
- 2009-05-12 CN CNA2009100265514A patent/CN101548962A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103735616A (en) * | 2014-01-20 | 2014-04-23 | 大连医诺生物有限公司 | Microencapsulated preparation for protecting eyesight and preparation method thereof |
| CN104738643A (en) * | 2015-03-03 | 2015-07-01 | 深圳市妍倩科技有限公司 | Food with antioxidant function |
| CN107669657A (en) * | 2016-08-02 | 2018-02-09 | 浙江医药股份有限公司新昌制药厂 | A kind of preparation method high-stability microencapsulated containing more double bond fat soluble nutrient |
| CN107669657B (en) * | 2016-08-02 | 2021-08-31 | 浙江医药股份有限公司新昌制药厂 | Preparation method of high-stability microcapsule containing double-bond fat-soluble nutrient |
| CN107495372A (en) * | 2017-09-27 | 2017-12-22 | 广州市范乐医药科技有限公司 | A kind of preparation method of Xanthophyll micro-capsule |
| CN111548294A (en) * | 2020-04-10 | 2020-08-18 | 天津大学 | Lutein methanol solvate crystal and preparation method thereof |
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Application publication date: 20091007 |