CN102382485A - Method for extracting anthocyanin from mulberries - Google Patents
Method for extracting anthocyanin from mulberries Download PDFInfo
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- CN102382485A CN102382485A CN2011102846302A CN201110284630A CN102382485A CN 102382485 A CN102382485 A CN 102382485A CN 2011102846302 A CN2011102846302 A CN 2011102846302A CN 201110284630 A CN201110284630 A CN 201110284630A CN 102382485 A CN102382485 A CN 102382485A
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Abstract
The invention belongs to the field of extraction and separation methods and particularly relates to a method for extracting anthocyanin from mulberries, which solves the technical problems of instability of anthocyanin in mulberries, limit and seasonality of ripening of the mulberries. Particularly, the method includes steps of utilizing the mulberries as raw materials, juicing the mulberries, extracting dregs by acid water, hydrochloric acid-ethanol, ethanol and the like, absorbing concentrated extracted solution by macroporous resin and concentrating eluent mist to be powder after desorbing, and finally obtaining mulberry extractives, wherein the content of the anthocyanin in the mulberry extractive is more that 30% by weight.
Description
Technical field
The invention belongs to the Fructus Mori extract production technique, particularly a kind of to extract the production technique of cyanidin(e) in the limited mulberry fruit resource, this invention belongs to the extraction separation field of biotechnology natural active matter.
Background technology
Mulberries are the mature fruit of Moraceae deciduous tree mulberry tree, and mulberries are sorosis, mulberry jujube again, and the peasant likes its sophisticated fresh fruit edible, and the flavor sweet juice is many, are one of fruit of the normal food of people.Sophisticated mulberries matter is glossy, sour and sweet palatability, with individual big, meat is thick, look purplish red, the sufficient person of sugar is good.Gather during annual 4-6 month fruit maturation, clean, decon, dry or slightly steam after dry edible.Can arrive big persevering Chinese medicinal materials library inquiry Chinese medicinal materials mulberry fruit.
Contain a large amount of cyanidin(e) in the mulberry fruit, cyanidin(e) is one type of water colo(u)r that extensively is present in the plant, belongs to flavonoids.Common in plant have 6 kinds, i.e. pelargonidin, cyanidin, delphinidin, p(a)eonidin, morning glory pigment and syringidin.Cyanidin(e) is a kind of strong inhibitor, and it can protect human body to avoid a kind of damage that is called the objectionable impurities of radical.Cyanidin(e) can also strengthen blood vessel elasticity, improves the recycle system and the slickness of promoting skin, and inflammation-inhibiting and allergy are improved the snappiness in joint.Cyanidin(e) is present in fruit, vegetables, the flowers, and it is relevant with it that they present multicoloured color major part, under the different pH value condition of vegetable cell vacuole, makes petal present multicoloured color.And the application of cyanidin(e) also very extensively, mainly in foodstuff additive.
This invention anthocyan extract is to be raw material with fruits and vegetables, forms through special process is refining.Mostly used pigment is synthetic colour in the foodstuffs industry at present; Toxicity is in various degree nearly all arranged; Life-time service can endanger people's health; Therefore natural pigment has just more and more caused the concern of scientific research field: owing to also do not have the pure article of cyanidin(e) on the home market so far, with exploitation indispensable sign condition and theoretical foundation is provided to the further investigation of anthocyanin class pigment so extract highly purified cyanidin(e), and helps its industrial utilization.And this project system gets cyanidin(e) extract finished product and development prospect is wide.
Summary of the invention
Technical problem to be solved by this invention is the production technique of the cyanidin(e) of extraction separation higher weight content from the mulberry fruit limited resources.Because mostly used pigment is synthetic colour in the foodstuffs industry at present, and toxicity is in various degree nearly all arranged, life-time service can endanger people's health, so natural pigment has just more and more caused the concern of scientific research field.Owing to also do not have the pure article of cyanidin(e) on the home market so far, with exploitation indispensable sign condition and theoretical foundation is provided to the further investigation of anthocyanin class pigment so extract highly purified cyanidin(e), then this invention has extremely wide prospect.
The extraction of cyanidin(e) in the mulberries provided by the present invention is through scum juice, extraction, purifying, concentrated, the drying and other steps preparation with fresh mulberries.
The technical scheme that the present invention taked is:
1, a kind of is the method that raw material comes extraction separation cyanidin(e) with the mulberry fruit.It is characterized in that: be raw material with the mulberry fruit; Mulberry fruit elder generation scum juice, again with bits with extractions such as sour water, hydrochloric acid-ethanol, ethanol, extracting solution concentrates and then adsorbs with macroporous resin; Concentrate eluant is sprayed to powder and promptly gets Fructus Mori extract after the desorption, and wherein the weight content of cyanidin(e) is more than 30%;
2, be the method that raw material comes extraction separation cyanidin(e) with the mulberry fruit according to claim 1, comprise the steps:
1) pre-treatment: with mulberries raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 2～5 times of bits weight, and volume ratio is to extract 2 times in 0.5～1% hydrochloric acid-20～70% ethanol, and temperature is 40～60 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with resin; Use washed with de-ionized water resin to effluent to be pale pink; Carrying out wash-out with 30%～100% Different concentrations of alcohol solution gradation successively then separates; Required component concentrating under reduced pressure is sprayed to Powdered, wherein the weight content of cyanidin(e) is more than 30%.
It is model resins such as AB-8, HP-20, D101, HZ816, XAD-2, XAD-4, XAD-16, DM-130, LSD-10, LSD-40, LSA-21, LSA-30, FU-02 that column chromatography resin according to the invention is selected from model.
The invention has the beneficial effects as follows:
Main active substances is an anthocyan in the mulberry fruit, contains 3 kinds of anthocyanogen compositions in the mulberry fruit: press content height successively row be Cyanidin-3-glucoside, Flos Pelargonii-3-glucoside, green winter eggplant-3-rutinoside.Cyanidin(e) is a kind of strong inhibitor, and it can protect human body to avoid a kind of damage that is called the objectionable impurities of radical.Cyanidin(e) can also strengthen blood vessel elasticity, improves the recycle system and the slickness of promoting skin, and inflammation-inhibiting and allergy are improved the snappiness in joint.
It is acid alcohol that the present invention extracts solvent, because cyanidin(e) receives Influence of Temperature destruction very big, if only very low with extraction yield under cryogenic condition such as sour water or low-carbon alcohol, and high temperature has destroyed cyanidin(e).The present invention uses acid alcohol under suitable temperature, to optimize extraction yield; Can ensured sustained development production, practice thrift cost, the column chromatography eluting solvent be pure; Unlikelyly bring any inorganics residual and relate to quality problems, so this invention have very high economic benefit and social benefit to finished product.
Description of drawings
Accompanying drawing 1 is a Fructus Mori extract HPLC finger printing,
Detect wavelength: 520nm; Chromatographic column: C18-ODS post 250 * 4.6mm 5 μ;
Flow velocity: 1.0ml/min; Column oven: 30 ℃;
Gradient elution: A:0.5% phosphoric acid B: water: acetonitrile: Glacial acetic acid min. 99.5: phosphoric acid=50:48.5:1.0:0.5;
Time (min) 0 26 30 35 40;
B（%） 20 60 ?20 20 ?Stop。
Embodiment
Embodiment 1:
1) pre-treatment: with 100g mulberry fruit raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 2 times of bits weight, extract 2 times in volume ratio 0.5% hydrochloric acid-40% ethanol, temperature is 40 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with XAD-16 model resin; Use washed with de-ionized water resin to effluent to be pink; Carrying out wash-out with 30% alcohol, 100% Different concentrations of alcohol solution gradation successively then separates; 30% alcohol moiety concentrating under reduced pressure is sprayed to Powdered 4.1 g, and wherein the weight content of cyanidin(e) is 25%.
Embodiment 2:
1) pre-treatment: with 100g mulberries raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 3 times of bits weight, extract 2 times in volume ratio 0.5% hydrochloric acid-60% ethanol, temperature is 50 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with D101 model resin; Use washed with de-ionized water resin to effluent to be pink; Carrying out wash-out with 20% alcohol, 60% alcohol, 100% Different concentrations of alcohol solution gradation successively then separates; 60% alcohol moiety concentrating under reduced pressure is sprayed to Powdered 3.8 g, and wherein the weight content of cyanidin(e) is 28%.
Embodiment 3:
1) pre-treatment: with 100g mulberries raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 4 times of bits weight, extract 2 times in volume ratio 1% hydrochloric acid-50% ethanol, temperature is 55 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with LSD-10 model resin; Using the washed with de-ionized water resin is colourless to effluent; Carrying out wash-out with 10% alcohol, 50% alcohol, 100% Different concentrations of alcohol solution gradation successively then separates; 50% alcohol moiety concentrating under reduced pressure is sprayed to Powdered, wherein the weight content of cyanidin(e) is 30%.
Embodiment 4:
1) pre-treatment: with 100g mulberry fruit raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 5 times of bits weight, extract 2 times in volume ratio 1% hydrochloric acid-70% ethanol, temperature is 45 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with HP-20 model resin; Using the washed with de-ionized water resin is colourless to effluent; Carrying out wash-out with 20% alcohol, 50% alcohol, 100% Different concentrations of alcohol solution gradation successively then separates; 50% alcohol moiety concentrating under reduced pressure is sprayed to Powdered 3.3g, and wherein the weight content of cyanidin(e) is 27%.
Embodiment 5:
1) pre-treatment: with 100g mulberry fruit raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 3 times of bits weight, extract 2 times in volume ratio 0.5% hydrochloric acid-70% ethanol, temperature is 55 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries liquid concentrator and 3) in liquid concentrator adsorb with DM-130 model resin; Use washed with de-ionized water resin to effluent to be pink; Carrying out wash-out with 10% alcohol, 20% alcohol, 60% alcohol, 100% Different concentrations of alcohol solution gradation successively then separates; 60% alcohol moiety concentrating under reduced pressure is sprayed to Powdered 2.6 g, and wherein the weight content of cyanidin(e) is 33%.
Claims (5)
1. one kind is the method that raw material comes extraction separation cyanidin(e) with the mulberry fruit; It is characterized in that: be raw material with the mulberry fruit; Mulberry fruit elder generation scum juice, again with bits with extractions such as sour water, hydrochloric acid-ethanol, ethanol, extracting solution concentrates and then adsorbs with macroporous resin; Concentrate eluant is sprayed to powder and promptly gets Fructus Mori extract after the desorption, and wherein the weight content of cyanidin(e) is more than 30%.
2. be the method that raw material comes extraction separation cyanidin(e) with the mulberry fruit according to claim 1, comprise the steps:
1) pre-treatment: with mulberries raw material scum juice;
2) extract: the mulberries bits behind the scum juice are placed 1 ~ 10 times of bits weight, and with extracting 2 times in sour water, hydrochloric acid-ethanol, the ethanol etc., temperature is 30 ~ 95 ℃;
3) concentrate, filter: extracting solution is concentrated, filters;
4) with mulberries juice and 3) in liquid concentrator adsorb with resin; Use washed with de-ionized water; Carry out wash-out with 30%～100% Different concentrations of alcohol solution gradation successively then and separate, required component concentrating under reduced pressure is sprayed to Powdered, wherein the weight content of cyanidin(e) is more than 30%.
3. as in the claim 2 2) described preparation method, it is characterized in that the mulberries bits behind the scum juice are placed 2 ~ 5 times of bits weight, and with hydrochloric acid-extraction using alcohol 2 times, temperature is 30 ~ 95 ℃.
4. the preparation method described in claim 3 is characterized in that, used hydrochloric acid-volumes of aqueous ethanol ratio is 0.5 ~ 1% hydrochloric acid-20 ~ 70% extraction using alcohol 2 times, and temperature is 30 ~ 95 ℃.
5. the preparation method described in claim 3 is characterized in that, the temperature that bits extract is 40 ~ 60 ℃.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2011102846302A CN102382485A (en) | 2011-09-23 | 2011-09-23 | Method for extracting anthocyanin from mulberries |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659743A (en) * | 2012-05-08 | 2012-09-12 | 李丹 | Extraction rectification method of anthocyanin in mulberry |
| CN102993765A (en) * | 2012-08-23 | 2013-03-27 | 江苏苏南药业实业有限公司 | Method for extracting effective components of mulberry |
| CN103319911A (en) * | 2013-07-17 | 2013-09-25 | 黄香利 | Technology for extracting mulberry haematochrome from mulberry residue |
| CN103468019A (en) * | 2013-09-13 | 2013-12-25 | 浙江农林大学 | Natural pigment prepared by using fruit residues and applications thereof |
| CN103462037A (en) * | 2013-09-13 | 2013-12-25 | 浙江农林大学 | Natural food additive |
| CN103652849A (en) * | 2013-08-23 | 2014-03-26 | 云南省林业科学院 | Indosasa hispida McClure 'rainbow' anthocyanin extract |
| CN104961783A (en) * | 2015-04-17 | 2015-10-07 | 浙江惠松制药有限公司 | Method for effectively extracting anthocyanidin and anthocyanin |
| CN105061529A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Extraction process of mulberry anthocyanin |
| CN105062125A (en) * | 2015-07-29 | 2015-11-18 | 胡伟民 | Mulberry red pigment extraction and purification method |
| CN105385188A (en) * | 2015-12-09 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of mulberry red pigment |
| CN105524035A (en) * | 2015-12-01 | 2016-04-27 | 大兴安岭林格贝寒带生物科技股份有限公司 | Manufacturing method of mulberry anthocyanidin |
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| CN107011697A (en) * | 2017-04-01 | 2017-08-04 | 江苏科技大学 | A kind of preparation method of mulberry red pigment powder |
| CN108795097A (en) * | 2018-05-21 | 2018-11-13 | 汕头大学 | A kind of isolation and purification method of kapok carthamin |
-
2011
- 2011-09-23 CN CN2011102846302A patent/CN102382485A/en active Pending
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102659743A (en) * | 2012-05-08 | 2012-09-12 | 李丹 | Extraction rectification method of anthocyanin in mulberry |
| CN102993765A (en) * | 2012-08-23 | 2013-03-27 | 江苏苏南药业实业有限公司 | Method for extracting effective components of mulberry |
| CN103319911A (en) * | 2013-07-17 | 2013-09-25 | 黄香利 | Technology for extracting mulberry haematochrome from mulberry residue |
| CN103652849A (en) * | 2013-08-23 | 2014-03-26 | 云南省林业科学院 | Indosasa hispida McClure 'rainbow' anthocyanin extract |
| CN103652849B (en) * | 2013-08-23 | 2015-03-25 | 云南省林业科学院 | Indosasa hispida McClure 'rainbow' anthocyanin extract |
| CN103468019A (en) * | 2013-09-13 | 2013-12-25 | 浙江农林大学 | Natural pigment prepared by using fruit residues and applications thereof |
| CN103462037A (en) * | 2013-09-13 | 2013-12-25 | 浙江农林大学 | Natural food additive |
| CN103462037B (en) * | 2013-09-13 | 2015-11-25 | 浙江农林大学 | A kind of natural additive for foodstuff |
| CN104961783B (en) * | 2015-04-17 | 2018-07-10 | 浙江惠松制药有限公司 | A kind of effective extraction anthocyanidin and the method for anthocyanin |
| CN104961783A (en) * | 2015-04-17 | 2015-10-07 | 浙江惠松制药有限公司 | Method for effectively extracting anthocyanidin and anthocyanin |
| CN105062125A (en) * | 2015-07-29 | 2015-11-18 | 胡伟民 | Mulberry red pigment extraction and purification method |
| CN105061529A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Extraction process of mulberry anthocyanin |
| CN105524035A (en) * | 2015-12-01 | 2016-04-27 | 大兴安岭林格贝寒带生物科技股份有限公司 | Manufacturing method of mulberry anthocyanidin |
| CN105524035B (en) * | 2015-12-01 | 2018-04-17 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of manufacture method of mulberries anthocyanidin |
| CN105385188A (en) * | 2015-12-09 | 2016-03-09 | 重庆三零三科技有限公司 | Preparation method of mulberry red pigment |
| CN106046848A (en) * | 2016-06-06 | 2016-10-26 | 西昌学院 | Method for extracting and purifying anthocyanin from mulberry pomace |
| CN107011697A (en) * | 2017-04-01 | 2017-08-04 | 江苏科技大学 | A kind of preparation method of mulberry red pigment powder |
| CN108795097A (en) * | 2018-05-21 | 2018-11-13 | 汕头大学 | A kind of isolation and purification method of kapok carthamin |
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Application publication date: 20120321 |