CN102503997A - Method for catalytic extraction of anthocyanidin through supercritical enzymatic mode - Google Patents

Method for catalytic extraction of anthocyanidin through supercritical enzymatic mode Download PDF

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Publication number
CN102503997A
CN102503997A CN2011103391412A CN201110339141A CN102503997A CN 102503997 A CN102503997 A CN 102503997A CN 2011103391412 A CN2011103391412 A CN 2011103391412A CN 201110339141 A CN201110339141 A CN 201110339141A CN 102503997 A CN102503997 A CN 102503997A
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China
Prior art keywords
anthocyanogen
extraction
pomace
overcritical
enzyme process
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CN2011103391412A
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Chinese (zh)
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赵海田
王振宇
姚磊
程翠林
马凤鸣
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Harbin Institute of Technology
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Harbin Institute of Technology
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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Abstract

The invention relates to a method for catalytic extraction of anthocyanidin through a supercritical enzymatic mode, which is characterized in that the method includes the following steps: step 1, drying the pomace of berry; step 2, grinding the dried pomace; step 3, adding cellulose into the pomace obtained in the step 2; step 4, extracting the pomace obtained in the step 3 by supercritical CO2; step 5, separating the liquid from the solid in the extracts obtained in the step 4; step 6, concentrating the distilled liquid obtained in the step 5 under vacuum condition; and step 7, freezing and drying the concentrated liquid obtained in the step 6 under vacuum condition to obtain anthocyanidin powder. The method has the advantages that long chain macromolecular substances such as the cellulose can be decomposed, and the release of the anthocyanidin can be accelerated, and therefore, the extraction ratio can be improved.

Description

The method of a kind of overcritical enzyme process catalysis extraction anthocyanogen
Technical field
The present invention relates to a kind of method that extracts anthocyanogen, especially relate to the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen.
Background technology
Supercutical fluid has the advantage of gas and liquid concurrently; Density is near density of liquid; Viscosity is near the viscosity of gas, and spread coefficient is bigger about 100 times than liquid between gas and liquid; This means that it has dissolving power and the very high mass transfer velocity that is comparable to liquid, can reach balance during extraction very soon.Supercritical fluid extraction has mass transfer velocity fast, and product need not be handled a large amount of dilute aqueous solns when reclaiming, and product separates easy, advantage such as no solvent residue in the product.
Anthocyanogen is a kind of natural water-soluble natural food dye that is distributed widely in; Belong to the flavones polyphenolic compound; Be under state of nature, to form glucosides, constituted blueness, redness, purple and the yellow etc. of many kinds in flower, fruit, the vegetables with various sugar by the pattern pyridine.Rough estimates, anthocyanogen is contained in 73 platymisciums in 27 sections, has 250 kinds of anthocyanogen of surpassing from plant, to separate and obtains.Natural plant antioxidant has become current research focus; Many researchs show that anthocyanogen has more physiological active functions; Comprise that lipid content, resistance anti-oxidant, that remove in radical, reduction serum and the liver are different and antitumor, prevent body endoperoxides effect etc.Anthocyanogen is as a kind of natural food colour, and safe, nontoxic, aboundresources have the huge applications potentiality in food, makeup, medicine and other fields.
The process for extracting of anthocyanogen mainly contains: organic solvent extraction method, enzymolysis process, ultrasonic extraction, microwave method and supercritical extraction etc.Total anthocyanogen about 91% in the berry is present in the pericarp, and in the skin slag after squeezing the juice also residual nearly 75%.Because anthocyanogen will be present in the cell or be adsorbed on the cell walls, conventional solvent extraction method is difficult to anthocyanogen is fully extracted, and extraction yield is lower.
Summary of the invention
The present invention solves the conventional solvent extraction method of existing in prior technology to be difficult to anthocyanogen fully extracted the technical problem that extraction yield is lower; Providing a kind of can decompose long-chain macromolecular substance such as Mierocrystalline cellulose, quickens the release that pattern has, thereby improves the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen of extraction yield.
Above-mentioned technical problem of the present invention mainly is able to solve through following technical proposals:
The method of a kind of overcritical enzyme process catalysis extraction anthocyanogen is characterized in that, may further comprise the steps:
Step 1, the berry pomace is dry;
Step 2 is pulverized the pomace of completing steps 1;
Step 3 adds cellulase in the pomace with completing steps 2;
Step 4 is carried out supercritical CO with the pomace of completing steps 3 2Extraction;
Step 5 is carried out solid-liquid separation with the extracted component of completing steps 4;
Step 6 is carried out vacuum concentration with the extracting solution of completing steps 5;
Step 7 obtains the anthocyanogen powder with the liquid concentrator of completing steps 6 after carrying out lyophilize under the vacuum state.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 1, pomace carries out the exsiccant method and does, pomace is put into baking oven, keeps 40 ℃~50 ℃ of temperature, and drying time is 10~12 hours.
Method above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen in the described step 2, is broken to the 40-60 order with dry consequence ground-slag.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 3, the cellulase of adding is a trichoderma reesei cellulase, and the mass ratio that adds trichoderma reesei cellulase and pomace is: 1: 125.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 4, as entrainment agent, the enzymolysis extraction time is 100~150 minutes with 500mL20~40% ethanolic soln, extracting pressure 20~40MPa, temperature 30-40 ℃.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 5, take centrifugal separation method to carry out the solid-liquid separation of extracted component, 4000 rpms of centrifugal conditions, centrifugation time 15 minutes.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 6, the conditional request of vacuum concentration is: thickening temperature remains on 40~60 ℃, and vacuum tightness 0.070~0.090Mpa, concentration time are 1~2 hour.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 7, the vacuum lyophilization temperature is-50~-40 ℃, vacuum tightness 0.070~0.090Mpa, 24 hours time.
Therefore, the present invention has following advantage: can long-chain macromolecular substance such as Mierocrystalline cellulose be decomposed, quicken the release that pattern has, thereby improve extraction yield.
Embodiment
Through embodiment, do further bright specifically below to technical scheme of the present invention.
Embodiment:
The method of a kind of overcritical enzyme process catalysis extraction anthocyanogen may further comprise the steps:
Step 1, the berry pomace is dry: pomace is put into baking oven, keep 40 ℃~50 ℃ of temperature, drying time is 10~12 hours.
Step 2 is crushed to the 40-60 order with the pomace of completing steps 1;
Step 3 adds cellulase in the pomace with completing steps 2, and in the present embodiment, the cellulase of adding is a trichoderma reesei cellulase, and the mass ratio that adds trichoderma reesei cellulase and pomace is: 1: 125, and the g of unit.
In the method for above-mentioned a kind of overcritical enzyme process catalysis extraction anthocyanogen, in the described step 4,
Step 4 is carried out supercritical CO with the pomace of completing steps 3 2Extraction: as entrainment agent, the enzymolysis extraction time is 100~150 minutes with 500mL20~40% ethanolic soln, extracting pressure 20~40MPa, temperature 30-40 ℃;
Step 5 takes centrifugal separation method to carry out the solid-liquid separation of extracted component, 4000 rpms of centrifugal conditions, centrifugation time 15 minutes the extracted component of completing steps 4;
Step 6 is carried out vacuum concentration with the extracting solution of completing steps 5, and thickening temperature remains on 40~60 ℃, and vacuum tightness 0.070~0.090Mpa, concentration time are 1~2 hour;
Step 7 obtains the anthocyanogen powder with the liquid concentrator of completing steps 6 after carrying out lyophilize under the vacuum state, the vacuum lyophilization temperature is-50~-40 ℃, vacuum tightness 0.070~0.090Mpa, 24 hours time.
Specific embodiment described herein only is that the present invention's spirit is illustrated.Person of ordinary skill in the field of the present invention can make various modifications or replenishes or adopt similar mode to substitute described specific embodiment, but can't depart from spirit of the present invention or surmount the defined scope of appended claims.

Claims (8)

1. the method for an overcritical enzyme process catalysis extraction anthocyanogen is characterized in that, may further comprise the steps:
Step 1, the berry pomace is dry;
Step 2 is pulverized the pomace of completing steps 1;
Step 3 adds cellulase in the pomace with completing steps 2;
Step 4 is carried out supercritical CO with the pomace of completing steps 3 2Extraction;
Step 5 is carried out solid-liquid separation with the extracted component of completing steps 4;
Step 6 is carried out vacuum concentration with the extracting solution of completing steps 5;
Step 7 obtains the anthocyanogen powder with the liquid concentrator of completing steps 6 after carrying out lyophilize under the vacuum state.
2. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1 is characterized in that in the described step 1, pomace carries out the exsiccant method and does, pomace is put into baking oven, keeps 40 ℃~50 ℃ of temperature, and drying time is 10~12 hours.
3. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1 is characterized in that, in the described step 2, dry consequence ground-slag is broken to the 40-60 order.
4. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1; It is characterized in that in the described step 3, the cellulase of adding is a trichoderma reesei cellulase; The mass ratio that adds trichoderma reesei cellulase and pomace is: 1: 125, and the g of unit.
5. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1 is characterized in that, in the described step 4; With 500mL20~40% ethanolic soln as entrainment agent; The enzymolysis extraction time is 100~150 minutes, extracting pressure 20~40MPa, temperature 30-40 ℃.
6. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1 is characterized in that, in the described step 5, takes centrifugal separation method to carry out the solid-liquid separation of extracted component, 4000 rpms of centrifugal conditions, centrifugation time 15 minutes.
7. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1; It is characterized in that in the described step 6, the conditional request of vacuum concentration is: thickening temperature remains on 40~60 ℃; Vacuum tightness 0.070~0.090Mpa, concentration time are 1~2 hour.
8. the method for a kind of overcritical enzyme process catalysis extraction anthocyanogen according to claim 1 is characterized in that in the described step 7, the vacuum lyophilization temperature is-50~-40 ℃, vacuum tightness 0.070~0.090Mpa, 24 hours time.
CN2011103391412A 2011-11-01 2011-11-01 Method for catalytic extraction of anthocyanidin through supercritical enzymatic mode Pending CN102503997A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104323061A (en) * 2014-09-22 2015-02-04 浙江省农业科学院 Method for preparing blueberry jam with high content of anthocyanin
CN106967307A (en) * 2017-05-09 2017-07-21 中国热带农业科学院南亚热带作物研究所 A kind of extracting method of miracle fruit pericarp pigment
CN111990615A (en) * 2020-08-10 2020-11-27 广东省农业科学院蚕业与农产品加工研究所 Preparation method of anthocyanin litchi soft can with ultrahigh-pressure photo-dynamic cold sterilization function
CN113245343A (en) * 2021-04-26 2021-08-13 菏泽尧舜牡丹生物科技有限公司 Efficient utilization method of squeezed peony residues

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
赵鑫: "天然花青苷提取纯化及降血脂作用的研究", 《中国优秀博硕士学位论文全文数据库 (硕士) 医药卫生科技辑》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104323061A (en) * 2014-09-22 2015-02-04 浙江省农业科学院 Method for preparing blueberry jam with high content of anthocyanin
CN106967307A (en) * 2017-05-09 2017-07-21 中国热带农业科学院南亚热带作物研究所 A kind of extracting method of miracle fruit pericarp pigment
CN111990615A (en) * 2020-08-10 2020-11-27 广东省农业科学院蚕业与农产品加工研究所 Preparation method of anthocyanin litchi soft can with ultrahigh-pressure photo-dynamic cold sterilization function
CN113245343A (en) * 2021-04-26 2021-08-13 菏泽尧舜牡丹生物科技有限公司 Efficient utilization method of squeezed peony residues

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Application publication date: 20120620