CN106634035A - Extraction method of fructus-clausenae-lanii-peel uranidin - Google Patents
Extraction method of fructus-clausenae-lanii-peel uranidin Download PDFInfo
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- CN106634035A CN106634035A CN201611240990.1A CN201611240990A CN106634035A CN 106634035 A CN106634035 A CN 106634035A CN 201611240990 A CN201611240990 A CN 201611240990A CN 106634035 A CN106634035 A CN 106634035A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses an extraction method of fructus-clausenae-lanii-peel uranidin. The extraction method comprises the following steps: 1), taking fructus-clausenae-lanii peel, and washing cleanly and smashing the fructus-clausenae-lanii peel; 2), adding the smashed fructus-clausenae-lanii peel into distilled water for mixing, putting an obtained first mixture at a low temperature for refrigeration until the first mixture is completely frozen, afterwards, taking out the first mixture for thawing at a room temperature, and adding cellulase into the first mixture for enzymolysis, so as to obtain a fructus-clausenae-lanii-peel extracting solution; 3), centrifugally separating the fructus-clausenae-lanii-peel extracting solution to abandon a precipitated part impurity, so as to obtain a fructus-clausenae-lanii-peel uranidin crude extracting solution; 4), enabling the fructus-clausenae-lanii-peel uranidin crude extracting solution to pass through a 100nm to 200nm microfiltration membrane, so as to obtain primary effluent liquid; 5), enabling the primary effluent liquid to pass through an ultrafiltration membrane of which the cutoff molecular weight is 3KDa to 5KDa, so as to obtain final effluent liquid; 6), carrying out vacuum freeze drying on the final effluent liquid, so as to obtain the fructus-clausenae-lanii-peel uranidin. The method provided by the invention is simple; the uranidin obtained through extraction is brilliant yellow; particles are loose; the solubility is good.
Description
Technical field
The invention belongs to technical field of pigment extraction, and in particular to the method that Clausena lansium (Lour.) Skeels peel extracts flavochrome.
Background technology
With deepening continuously for medical science, toxicology and biological test research work, Use out of range synthetic dyestuff is to human body
The harm of health is increasingly paid close attention to by people, therefore synthetic dyestuff is more and more stricter as the consumption of food additive.My god
So pigment bright color is tempting, is rich in natural sense, especially the composition of some natural pigment inherently people's diet, has
There are certain nutritive value and medicine healthy sofa effect.In natural pigment, yellow tone is relatively soft compared with other tones
With, it is tempting, consumer can be made to produce strong desire to buy, with a large amount of needs of foreign market, natural yellow pigment presents
The impetus that supply falls short of demand.
Method for extracting pigment common are solvent extraction method, ultrasonic extraction, microwave loss mechanisms, supercritical extraction, enzyme
Extraction method and biotechnology extraction method etc..At present natural yellow pigment is mainly from Fructus Gardeniae, Rhizoma Curcumae Longae, mandarin orange, Flos Carthami, Semen Maydiss, Fructus Cucurbitae moschatae etc.
It is middle to extract, but the flavochrome less stable obtained by most of extraction.Such as Gardenia Yellow is for dough product coloring
When, easily there is green change, stability is not high；Curcumin is stronger to the stability of reducing agent, and coloring is strong, but to light, heat, iron ion
It is sensitive；Citrus Huang, fugitive color very sensitive to light.Therefore, the natural yellow pigment for developing good stability is sending out for food coloring industry
One of exhibition trend, it is significant to flavochrome market.
Clausena Rutaceae clausena plant, is a kind of special product fruit tree of China torrid zone and subtropical zone, and the country is main
It is distributed in the ground such as Guangdong, Guangxi, Fujian, Taiwan, Yunnan, Hainan.Clausena lansium (Lour.) Skeels have a very high medical value, the fruit of Clausena lansium (Lour.) Skeels, leaf,
Root, seed can be used as medicine.The chemical constitution study of Clausena lansium (Lour.) Skeels is concentrated on root, stem and leaf at present, and the research to peel is main
It is its volatile oil and bacteriostatic active ingredients.
Number of patent application 201210373268.0 discloses a kind of method of the extraction purification cycloclausenamide from Clausena lansium (Lour.) Skeels,
The method is crushed with Folium clausenae lansii as raw material, plus appropriate ammonia mixes ammonification thoroughly, adds and is concentrated after methanol solution immersion, adds chlorine
Imitative solution ultrasonic dissolution, then Jing high-speed counter-current chromatographs isolate and purify.
Number of patent application 201310258584.8 discloses one kind isolating biologically active parent Clausena lansium (Lour.) Skeels acyl from Semen clausenae lansii
Amine B prepares pesticide.
Number of patent application 201410274121.5 discloses a kind of preparation method of Folium clausenae lansii extract, by using ultrasound
Auxiliary low-carbon alcohols organic solvent extraction Folium clausenae lansii active component, the alkaloid highest in the extract.
Jing retrievals show, at present in existing Clausena lansium (Lour.) Skeels extract patented technology, active matter mainly in Folium clausenae lansii and core
Extracting method, it is less for the research that Clausena lansium (Lour.) Skeels pericarp pigment is extracted.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of Fructus clausenae lansii Beijing opera method for extracting pigment, and the method is simple, carries
Yellow crude granule obtained by taking is loose, dissolubility is good.
A kind of Fructus clausenae lansii Beijing opera method for extracting pigment is the technical scheme is that, is comprised the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water mixing, freezing is put in, until fully charge, then takes out
Melt under room temperature, add cellulase degradation, obtain Clausena lansium (Lour.) Skeels Fruit peel extract；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 100～200nm micro-filtration membrane；
5) by first effluent by the ultrafilter membrane that molecular cut off is 3～5KDa, final effluent is obtained；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product.
In the Clausena lansium (Lour.) Skeels flavochrome extracting method, step 2) distilled water and the solid-liquid ratio of Clausena lansium (Lour.) Skeels peel be 1:60～100 (g/
ML), it is positioned over low temperature -15～-20 DEG C and is frozen up to fully charge, then take out and melt at room temperature, adds 0.6～1.0%
Cellulase, in 40～55 DEG C 20～35min is digested.
Preferably, in the Fructus clausenae lansii Beijing opera method for extracting pigment, Clausena lansium (Lour.) Skeels peel is 1 with the solid-liquid ratio of distilled water:80(g/
ML), it is positioned over -20 DEG C of low temperature and is frozen up to fully charge, then take out and melt at room temperature, adds 0.8% cellulase, in
50 DEG C of enzymolysis 25min.
Preferably, in the Fructus clausenae lansii Beijing opera method for extracting pigment, step 4) in by crude extract by 200nm micro-filtration membrane,
Obtain first effluent.
Preferably, in the Fructus clausenae lansii Beijing opera method for extracting pigment, step 5) in by first effluent by retaining molecule
The ultrafilter membrane of amount 3KDa, obtains final effluent.
In the Fructus clausenae lansii Beijing opera method for extracting pigment, step 6) the vacuum lyophilization parameter：Pre-freezing temperature -30
～-15 DEG C, 2～6h of pre-freeze time, 3～8mm of material thickness, 35～70Pa of drying chamber pressure, 30～50 DEG C of heating-up temperature is dried
6～12h of time.
Preferably, in the Fructus clausenae lansii Beijing opera method for extracting pigment, vacuum lyophilization parameter：- 20 DEG C of pre-freezing temperature, in advance
Jelly time 4h, material thickness 4mm, drying chamber pressure 60Pa, 35 DEG C of heating-up temperature, drying time 10h.
Clausena lansium (Lour.) Skeels fresh fruit is perishable, be difficult storage, in recent years, researcher with Clausena lansium (Lour.) Skeels as raw material deep processing production fruit wine, preserved fruit,
The products such as beverage, generate substantial amounts of peel, and the present invention extracts flavochrome, can improve the value of Clausena lansium (Lour.) Skeels using Clausena lansium (Lour.) Skeels peel, real
Existing refuse reclamation.
Freeze-thawing method is referred to will treat that cell, in (- 15～-20 DEG C) freezings of low temperature, is then put in room temperature and melts rapidly, such as
This is repeated multiple times, is destroyed cell, intracellular organic matter dissolution.The mechanism of freezing-thawing method is：1) can make in refrigerating process
The hydrophobic bond structure breaking of cell membrane, so as to increase the hydrophilic of cell；2) intracellular water crystallization forms ice crystal grain when freezing, and makes
The salinity of remaining cytosol increases and causes cell expansion to crush.
The invention has the beneficial effects as follows：The present invention combines the Huang in enzymatic isolation method extraction Clausena lansium (Lour.) Skeels peel using freeze-thawing method
Pigment, without the need for organic solvent, method is simple, and extraction time is short；Using membrane filtration separating-purifying, products obtained therefrom is in glassy yellow,
Grain is loose, and dissolubility is good.
Specific embodiment
With reference to specific embodiment, the present invention is further described, but embodiment of the present invention is not limited only to this.
Embodiment 1
A kind of Fructus clausenae lansii Beijing opera method for extracting pigment, comprises the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water, and solid-liquid ratio is 1:60 (g/mL), are positioned over -15 DEG C of freezings of low temperature straight
To fully charge, then take out and melt at room temperature, add 0.6% cellulase, in 40 DEG C 35min is digested；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 100nm micro-filtration membrane；
5) first effluent is obtained into final effluent by the ultrafilter membrane that molecular cut off is 5KDa；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product, yield is 4.76%；
The vacuum lyophilization parameter is：- 30 DEG C of pre-freezing temperature, pre-freeze time 2h, material thickness 8mm, is dried chamber pressure
Power 70Pa, 50 DEG C of heating-up temperature, drying time 6h.
Yield=(Fructus clausenae lansii Beijing opera pigment quality/Clausena lansium (Lour.) Skeels pericarp quality) × 100%.
Embodiment 2
A kind of Fructus clausenae lansii Beijing opera method for extracting pigment, comprises the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water, and solid-liquid ratio is 1:80 (g/mL), are positioned over -20 DEG C of freezings of low temperature straight
To fully charge, then take out and melt at room temperature, add 0.8% cellulase, in 50 DEG C 25min is digested；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 200nm micro-filtration membrane；
5) first effluent is obtained into final effluent by the ultrafilter membrane that molecular cut off is 3KDa；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product, yield is 6.28%；
The vacuum lyophilization parameter is：- 20 DEG C of pre-freezing temperature, pre-freeze time 4h, material thickness 4mm, is dried chamber pressure
Power 60Pa, 35 DEG C of heating-up temperature, drying time 10h.
Embodiment 3
A kind of Fructus clausenae lansii Beijing opera method for extracting pigment, comprises the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water, and solid-liquid ratio is 1：100 (g/mL), are positioned over -18 DEG C of freezings of low temperature
Until fully charge, then takes out and melt at room temperature, 1.0% cellulase is added, in 55 DEG C 20min is digested；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 150nm micro-filtration membrane；
5) first effluent is obtained into final effluent by the ultrafilter membrane that molecular cut off is 4KDa；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product, yield is 5.74%；
The vacuum lyophilization parameter is：- 15 DEG C of pre-freezing temperature, pre-freeze time 6h, material thickness 3mm, is dried chamber pressure
Power 35Pa, 30 DEG C of heating-up temperature, drying time 12h.
Embodiment 4
A kind of Fructus clausenae lansii Beijing opera method for extracting pigment, comprises the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water, and solid-liquid ratio is 1:70 (g/mL), are positioned over -15 DEG C of freezings of low temperature straight
To fully charge, then take out and melt at room temperature, add 0.7% cellulase, in 45 DEG C 30min is digested；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 200nm micro-filtration membrane；
5) first effluent is obtained into final effluent by the ultrafilter membrane that molecular cut off is 4KDa；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product, yield is 5.19%；
The vacuum lyophilization parameter is：- 30 DEG C of pre-freezing temperature, pre-freeze time 3h, material thickness 6mm, is dried chamber pressure
Power 45Pa, 45 DEG C of heating-up temperature, drying time 8h.
Comparative example
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water, and solid-liquid ratio is 1:80 (g/mL), add 0.8% cellulase, in
50 DEG C of enzymolysis 30min；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 200nm micro-filtration membrane；
5) first effluent is obtained into final effluent by the ultrafilter membrane that molecular cut off is 3KDa；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product, yield is 3.28%；
The vacuum lyophilization parameter is：- 20 DEG C of pre-freezing temperature, pre-freeze time 4h, material thickness 4mm, is dried chamber pressure
Power 60Pa, 35 DEG C of heating-up temperature, drying time 10h.
The flavochrome productivity ratio that the Fructus clausenae lansii Beijing opera method for extracting pigment of embodiment 1-4 and comparative example is extracted is compared with can see
Go out, the yield that enzymolysis and extraction flavochrome is used alone in comparative example is less than embodiment 1-4, illustrate to be combined using cell-thawing method
Enzymatic isolation method can improve flavochrome yield.
Impact of the drying meanss of embodiment 5 to Fructus clausenae lansii Beijing opera pigment quality
Using Fructus clausenae lansii Beijing opera method for extracting pigment step 1 of the present invention) to step 5) flavochrome solution is prepared, then distinguish
Process is dried using vacuum lyophilization, spray drying and hot air drying, to being dried gained flavochrome quality evaluation is carried out,
As a result it is as shown in table 1.
Vacuum lyophilization parameter：- 20 DEG C of pre-freezing temperature, pre-freeze time 4h, material thickness 4mm, drying chamber pressure 60Pa,
35 DEG C of heating-up temperature, drying time 10h.
Spray drying parameters are：170 DEG C of intake air temperature, 75～80 DEG C of air outlet temperature, pan feeding flow 30mL/min.Heat
Wind baking temperature is 60 DEG C, normal pressure.
The quality evaluation of the Clausena lansium (Lour.) Skeels peel uranidin that the different drying meanss of table 1 are obtained
As it can be seen from table 1 in three kinds of drying meanss, flavochrome graininess that vacuum lyophilization is obtained, color and luster and
Dissolubility is integrally better than spray drying and hot air drying.Thus illustrate, gained Clausena lansium (Lour.) Skeels peel is dried using vacuum freeze-drying method
Flavochrome quality is good.
Embodiment described above is better embodiment of the present invention, every principle and the situation of objective without departing from the present invention
Under, the embodiment of the present invention is modified, is replaced, belong within the scope of the present invention.
Claims (5)
1. a kind of Fructus clausenae lansii Beijing opera method for extracting pigment, it is characterised in that comprise the following steps：
1) Clausena lansium (Lour.) Skeels peel is taken, is cleaned, crushed；
2) the Clausena lansium (Lour.) Skeels peel after crushing adds distilled water mixing, freezing is put in, until fully charge, then takes out in room temperature
Lower thawing, adds cellulase degradation, obtains Clausena lansium (Lour.) Skeels Fruit peel extract；
3) sediment fraction impurity is abandoned in centrifugation, obtains Clausena lansium (Lour.) Skeels peel uranidin crude extract；
4) Clausena lansium (Lour.) Skeels peel uranidin crude extract is obtained into first effluent by 100～200nm micro-filtration membrane；
5) by first effluent by the ultrafilter membrane that molecular cut off is 3～5KDa, final effluent is obtained；
6) by final effluent vacuum lyophilization, Clausena lansium (Lour.) Skeels peel uranidin is obtained final product；
The step 2) solid-liquid ratio of distilled water and Clausena lansium (Lour.) Skeels peel is 1:60～100 (g/mL), are positioned over low temperature -15～-20 DEG C
Fully charge is frozen up to, is then taken out and is melted at room temperature, add 0.6～1.0% cellulase, in 40～55 DEG C 20 are digested
～35min；
The step 6) vacuum lyophilization parameter is：Pre-freezing temperature -30～-15 DEG C, 2～6h of pre-freeze time, material thickness 3～
8mm, 35～70Pa of drying chamber pressure, 30～50 DEG C of heating-up temperature, drying time 6～12h.
2. Fructus clausenae lansii Beijing opera method for extracting pigment according to claim 1, it is characterised in that Clausena lansium (Lour.) Skeels peel and distilled water
Solid-liquid ratio is 1:80 (g/mL), are positioned over -20 DEG C of low temperature and are frozen up to fully charge, then take out and melt at room temperature, add
0.8% cellulase, in 50 DEG C 25min is digested.
3. Fructus clausenae lansii Beijing opera method for extracting pigment according to claim 1, it is characterised in that vacuum lyophilization parameter：
- 20 DEG C of pre-freezing temperature, pre-freeze time 4h, material thickness 4mm, drying chamber pressure 60Pa, 35 DEG C of heating-up temperature, drying time 10h.
4. the Fructus clausenae lansii Beijing opera method for extracting pigment according to any one of claim 1-3, it is characterised in that lead to crude extract
200nm micro-filtration membrane is crossed, first effluent is obtained.
5. the Fructus clausenae lansii Beijing opera method for extracting pigment according to any one of claim 1-3, it is characterised in that by primary outflow
The ultrafilter membrane that liquid passes through molecular cut off 3KDa, obtains final effluent.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113667030A (en) * | 2021-08-11 | 2021-11-19 | 华南理工大学 | Method for decoloring and purifying osmanthus fragrans crude polysaccharide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104419216A (en) * | 2013-09-08 | 2015-03-18 | 青岛鹏远康华天然产物有限公司 | Extraction process of purple sweet potato pigment |
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2016
- 2016-12-28 CN CN201611240990.1A patent/CN106634035A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104419216A (en) * | 2013-09-08 | 2015-03-18 | 青岛鹏远康华天然产物有限公司 | Extraction process of purple sweet potato pigment |
Non-Patent Citations (1)
| Title |
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| 陈婉瑞等: "黄皮果皮色素的提取工艺及其稳定性研究", 《韩山师范学院学报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113667030A (en) * | 2021-08-11 | 2021-11-19 | 华南理工大学 | Method for decoloring and purifying osmanthus fragrans crude polysaccharide |
| CN113667030B (en) * | 2021-08-11 | 2022-10-25 | 华南理工大学 | Method for decoloring and purifying osmanthus fragrans crude polysaccharide |
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Application publication date: 20170510 |