CN105524035B - A kind of manufacture method of mulberries anthocyanidin - Google Patents
A kind of manufacture method of mulberries anthocyanidin Download PDFInfo
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- CN105524035B CN105524035B CN201510889948.1A CN201510889948A CN105524035B CN 105524035 B CN105524035 B CN 105524035B CN 201510889948 A CN201510889948 A CN 201510889948A CN 105524035 B CN105524035 B CN 105524035B
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- anthocyanidin
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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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
Abstract
The invention belongs to field of natural organic chemistry, is related to the anthocyanidin extracting and developing method in mulberries.This method is first extracted in alkaline conditions using tea polyphenols as antioxidant, is then cleaned in acid condition using flocculant, is recycled cationic exchanger resin purification liquid, is obtained the anthocyanidin product of high-purity.Advantages of the present invention：1st, the present invention uses water as Extraction solvent in alkaline conditions, compared with traditional extraction using ethanol, greatly reduces production cost；2nd, natural is added in extraction process, the loss of anthocyanidin can be effectively reduced；3rd, the impurity in extracting solution is precipitated using flocculant, contributes to the raising of anthocyanidin product purity；4th, using cation exchange resin purification liquid, the purity of anthocyanidin product is made to be significantly improved.Anthocyanidin prepared by the present invention can be widely applied to the fields such as health food and cosmetics.
Description
Technical field
The invention belongs to field of natural organic chemistry, is related to a kind of industrialization side that anthocyanidin is prepared using mulberries as raw material
Method.
Background technology
Anthocyanidin is a kind of water colo(u)r, can change color with the soda acid of cell liquid.Cell liquid is in acid then inclined
Red, cell liquid is then partially blue in alkalescence, and anthocyanidin is one of primary pigments for forming petal and fruit color.Anthocyanidin is plant two
Level metabolite, is physiologically playing the part of important role, anthocyanidin is the nutritional supplement of pure natural anti-aging, and research has shown that
It is that mankind nowadays find most effective anioxidant phytochemicals, its antioxygenic property is higher by 50 times than vitamin E, compares vitamin
C is higher by 20 times.Its biological effectiveness to human body is 100%, can just be detected in blood within 20 minutes after taking, to increasing
Strong eyesight, anti-eye strain, delay cranial nerve aging to have the effect of notable, while to the microangiopathy as caused by diabetes
Also there is preferable therapeutic effect, moreover it is possible to strengthen a variety of diseases such as cardio-pulmonary function, prevention senile dementia.
(s ā ng shen read s ā ng ren to mulberries again[1]), the ripening fruits of mulberry tree, mulberries are called sorosis, mulberry bubble youngster, peasant
The fresh fruit for liking its ripe is eaten, and sweet juice is more, is one of the fruit of people's often feeding, wherein containing substantial amounts of anthocyanidin.
Currently used extracting method has：Organic solvent extraction, supercritical extraction, microwave method and ultrasonic extraction
Method.Organic solvent extraction is common extraction anthocyanidin method, complete rear, it is necessary to solvent extraction with some organic solvents such as
Petroleum ether, just own institute, ether etc. are extracted to remove the liposoluble substance in crude extract.The advantages of organic solvent extraction is operation
It is easy, it is not necessary to complicated instrument and equipment；Shortcoming is that organic solvent consumption is high, time-consuming, and while extracting will heat and can cause to spend
The oxidative degradation of blue or green element.Microwave method and supercritical ultrasonics technology can not also carry out large-scale industrial production due to the limit value of equipment.It is super
Critical extraction can realize industrialization at present, but due to the particularity of the technology, cause the cyanine using technology production
Element is with high costs, can not be by this product promotion into ordinary consumer.
The advantages of more common purification process is mainly to be carried out using macroporous absorbent resin at present, macroporous absorbent resin be
Large amount of adsorption, can recycle, can be cost-effective on certain cost；Shortcoming is that the impurity of absorption also compares more, purifying
Product purity lifting afterwards is not very notable.
The content of the invention
It is an object of the invention to provide a kind of industrial method that mulberries anthocyanidin is prepared from mulberries.The present invention first adopts
Extracted with alkaline aqueous solution in the presence of natural, recycle flocculant to be removed under the conditions of weakly acidic
It is miscellaneous, then isolated and purified using cation exchange resin, obtain the anthocyanidin product of high-purity.
The technical proposal of the invention is realized in this way, it comprises the following steps：
(1) extract：By mulberries practicality pH value be 10~12 alkaline aqueous solution under the conditions of existing for natural
Extracted, obtain the extracting solution containing anthocyanidin；
(2) it is acidified：Acidic aqueous solution is added into extracting solution, the pH value of extracting solution is maintained between 6~7；
(3) clean：A certain amount of flocculant is added into extracting solution, is stood after stirring evenly under certain condition, then
Solid content impurity therein is removed by centrifuging, obtains solution；
(4) purify：Solution is first adsorbed with cation exchange resin, then with acid solution to cation exchange tree
Fat is eluted, and obtains the solution containing anthocyanidin；
(5) concentrate；It is 4~6 that solution is adjusted to pH value with alkaline solution, is then concentrated under reduced pressure, obtains concentrate；
(6) it is dry：Concentrate obtains mulberries anthocyanidin product using spray drying；
In the step (1), natural include vitamin A, C, E, P, polyphenol, one kind in vegetable active selenium or
Several, usage amount is the 0.1~1% of mulberries material quality, and Extracting temperature is 70~80 DEG C, raw material: extracting solution=1: 5~10
(m/v), extraction time is 60~120min；
In the step (3), the flocculant is ZTC1+1 types, and additive amount 2%, 40 DEG C of temperature, stirs 5min, then
Stand 120min, centrifuge；
In the step (4), the centrifugate obtained by step (3) is purified with cation exchange resin, centrifugate
Upper column flow rate is 1BV/h, then with deionized water rinsing, flow velocity 1.5BV/h, the dosage of deionized water is 2BV；Then with 2~
5% aqueous hydrochloric acid solution is eluted, and the flow velocity of eluent is 1.5BV/h, and the dosage of eluent is 3~5BV.
Embodiment
Embodiment 1
The Extraction solvent buck (pH=12) of the mulberries of 1000kg and 5000kg are put into extractor, and into extractor
The vitamin C that 5kg purity is 95% is put into, Extracting temperature is 70 DEG C, extraction time 90min, extracts 2 times, collects extracting solution；
The extracting solution being collected into is adjusted using acidic aqueous solution (pH=1), it is 6.4 to be allowed to pH value, is then added thereto
ZTC1+1 type flocculants, additive amount 2%, 5min is stirred under conditions of 40 DEG C of temperature, then stands 120min, centrifuge from
The heart, collects centrifugate；Centrifugate to be purified with 001 type cation exchange resin, the upper column flow rate of centrifugate is 1BV/h,
Use deionized water rinsing again, flow velocity 1.5BV/h, the dosage of deionized water is 2BV, then with 4.5% aqueous hydrochloric acid solution into
Row elution, the flow velocity of eluent is 1.5BV/h, and the dosage of eluent is 5BV, obtains the eluent containing anthocyanidin.Will elution
Liquid alkaline aqueous solution readjusts prices pH value between 4~6, then vacuum-concentrcted, and vacuum is -0.08~~0.07Mpa, dense
For contracting temperature at 50 ± 2 DEG C, recycling design, obtains concentrate；Concentrate is dried using spray dryer again, inlet temperature
For 200~210 DEG C, outlet temperature is 80~90 DEG C, obtains the mulberries anthocyanidin product 5.21kg that anthocyanidin content is 27.3%.
Embodiment 2
The Extraction solvent buck (pH=11) of the mulberries of 1000kg and 5000kg are put into extractor, and into extractor
The vitamin E that 10kg purity is 50% is put into, Extracting temperature is 75 DEG C, extraction time 120min, extracts 2 times, collects extraction
Liquid；The extracting solution being collected into is adjusted using acidic aqueous solution (pH=1), it is 6.7 to be allowed to pH value, is then added thereto
ZTC1+1 type flocculants, additive amount 2%, 5min is stirred under conditions of 40 DEG C of temperature, then stands 120min, centrifuge from
The heart, collects centrifugate；Centrifugate is purified with D-85 macropore propionic acid alkene system weak-acid cation-exchange resin, centrifugate
Upper column flow rate is 1BV/h, then with deionized water rinsing, flow velocity 1.5BV/h, the dosage of deionized water is 2BV, Ran Houyong
3.0% aqueous hydrochloric acid solution is eluted, and the flow velocity of eluent is 1.5BV/h, and the dosage of eluent is 4.5BV, is contained
The eluent of anthocyanidin.Eluent alkaline aqueous solution is readjusted prices into pH value between 4~6, then vacuum-concentrcted, vacuum
For -0.08~-0.07Mpa, for thickening temperature at 50 ± 2 DEG C, recycling design, obtains concentrate；It is again that concentrate is dry using spraying
Dry device is dried, and inlet temperature is 200~210 DEG C, and outlet temperature is 80~90 DEG C, and it is 25.3% to obtain anthocyanidin content
Mulberries anthocyanidin product 5.34kg.
Claims (1)
1. a kind of manufacture method of mulberries anthocyanidin, it comprises the following steps：
(1) extract：The alkaline aqueous solution that mulberries practicality pH value is 10~12 is carried out under the conditions of existing for natural
Extraction, obtains the extracting solution containing anthocyanidin；
(2) it is acidified：Acidic aqueous solution is added into extracting solution, the pH value of extracting solution is maintained between 6~7；
(3) clean：A certain amount of flocculant is added into extracting solution, stands after stirring evenly under certain condition, then passes through
Centrifugation removes solid content impurity therein, obtains solution；
(4) purify：Solution is first adsorbed with cation exchange resin, then with acid solution to cation exchange resin into
Row elution, obtains the solution containing anthocyanidin；
(5) concentrate：It is 4~6 that solution is adjusted to pH value with alkaline solution, is then concentrated under reduced pressure, obtains concentrate；
(6) it is dry：Concentrate obtains mulberries anthocyanidin product using spray drying；
In the step (1), natural includes vitamin A, C, E, P, polyphenol, one kind in vegetable active selenium or several
Kind, usage amount is the 0.1~1% of mulberries material quality, and Extracting temperature is 70~80 DEG C, raw material: extracting solution=1: 5~10 (m/
V), extraction time is 60~120min；
In the step (3), the flocculant is ZTC1+1 types, and additive amount 2%, 40 DEG C of temperature, stirs 5min, then stand
120min, centrifuge；
In the step (4), the centrifugate obtained by step (3) is purified with cation exchange resin, the upper prop of centrifugate
Flow velocity is 1BV/h, then with deionized water rinsing, flow velocity 1.5BV/h, the dosage of deionized water is 2BV；Then with 2~5%
Aqueous hydrochloric acid solution is eluted, and the flow velocity of eluent is 1.5BV/h, and the dosage of eluent is 3~5BV.
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| CN201510889948.1A CN105524035B (en) | 2015-12-01 | 2015-12-01 | A kind of manufacture method of mulberries anthocyanidin |
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| CN201510889948.1A CN105524035B (en) | 2015-12-01 | 2015-12-01 | A kind of manufacture method of mulberries anthocyanidin |
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| CN105524035A CN105524035A (en) | 2016-04-27 |
| CN105524035B true CN105524035B (en) | 2018-04-17 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106579443A (en) * | 2016-12-29 | 2017-04-26 | 界首市菁华科技信息咨询服务有限公司 | Method for extracting anthocyanin from mulberries |
| CN115572493A (en) * | 2022-09-23 | 2023-01-06 | 廊坊师范学院 | Method for preparing natural plant toner from fruit and vegetable raw materials |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
| CN102382485A (en) * | 2011-09-23 | 2012-03-21 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting anthocyanin from mulberries |
| CN102659743A (en) * | 2012-05-08 | 2012-09-12 | 李丹 | Extraction rectification method of anthocyanin in mulberry |
| CN103130763A (en) * | 2013-02-26 | 2013-06-05 | 海南达川食品有限公司 | Method for preparing anthocyanin by using red-meat pitaya |
| CN103333149A (en) * | 2013-06-20 | 2013-10-02 | 吕梁学院 | Extraction method of date peel cyanidin |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100842448B1 (en) * | 2006-12-14 | 2008-07-01 | 대한민국 | The method for manufacturing the cyanidin-3-glucoside derived from a mulberry with the food coloring powder |
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- 2015-12-01 CN CN201510889948.1A patent/CN105524035B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102212053A (en) * | 2011-04-16 | 2011-10-12 | 湖州柳荫生物科技有限公司 | Method for extracting mulberry cyanidin |
| CN102382485A (en) * | 2011-09-23 | 2012-03-21 | 天津市尖峰天然产物研究开发有限公司 | Method for extracting anthocyanin from mulberries |
| CN102659743A (en) * | 2012-05-08 | 2012-09-12 | 李丹 | Extraction rectification method of anthocyanin in mulberry |
| CN103130763A (en) * | 2013-02-26 | 2013-06-05 | 海南达川食品有限公司 | Method for preparing anthocyanin by using red-meat pitaya |
| CN103333149A (en) * | 2013-06-20 | 2013-10-02 | 吕梁学院 | Extraction method of date peel cyanidin |
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