CN109020941B - A kind of extracting method of purple sweet potato cyanidin - Google Patents
A kind of extracting method of purple sweet potato cyanidin Download PDFInfo
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- CN109020941B CN109020941B CN201811257680.XA CN201811257680A CN109020941B CN 109020941 B CN109020941 B CN 109020941B CN 201811257680 A CN201811257680 A CN 201811257680A CN 109020941 B CN109020941 B CN 109020941B
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- sweet potato
- purple sweet
- purple
- extracting method
- potato cyanidin
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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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- Coloring Foods And Improving Nutritive Qualities (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The present invention relates to compounds to extract field, specifically a kind of extracting method of purple sweet potato cyanidin, its main feature is that the following steps are included: a, adding metal salt solution, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole diethyl phosphate salt in purple sweetpotato slurries and being uniformly mixed, after ultrasonic wave, microwave cooperating act on 5~10min, continue 5~15min of Microwave Extraction, extracting solution takes supernatant after decoloration removal of impurities, clarification, and supernatant is concentrated and dried to obtain extraction cream；B, extraction cream centrifuge separation, collects filtrate, and concentrating filter liquor is dried to obtain purple sweet potato cyanidin extract.Compared with prior art, the features such as extracting method of purple sweet potato cyanidin of the invention has simple process, convenient for operation, and the anthocyanidin recovery rate prepared is high, purity is high, has good application value.
Description
Technical field
The present invention relates to compounds to extract field, specifically a kind of extracting method of purple sweet potato cyanidin.
Background technique
Anthocyanidin (Anthocyanidin), also known as anthocyanidin are a kind of water colo(u)rs, can be with the acid of cell liquid
Alkalinity and change color.Cell liquid is then partially red in acidity, and cell liquid is then partially blue in alkalinity, is the master for constituting petal and fruit color
Want one of pigment.Anthocyanidin is widely present in the vegetable and fruit of a variety of peonys, purple or blue, as lycium ruthenicum,
Grape, blackberry, blueberry, fig, cherry, beet root, eggplant, purple sweetpotato etc., anthocyanidin is mainly deposited with glycoside forms under natural conditions
In, referred to as anthocyanin (Anthocyanin), when which is by blue extract in Marguart name corn flower flower
Put forward, now the general name as allied substances.
Anthocyanidin may be one of discovery most great in history.The free radical scavenging ability of anthocyanidin is vitamin E
50 times and 20 times ascorbic, the absorption of the sad human body 100% of anthocyanidin is taken after twenty minutes, can be detected in blood
It arrives, and maintains to be up to 27 hours in vivo.Different from other antioxidants, cyanine is known as the ability across blood-brain barrier.
Purple sweetpotato is rich in anthocyanidin and has preferable light, thermal stability.Recent studies indicate that purple sweetpotato
Pigment, which has, to be removed free radical, anti-oxidant, anti-mutation, blood pressure lowering, improves the different physiological roles such as liver function, in food, makeup
It is had broad application prospects in the industries such as product and medicine.
The extracting method of anthocyanidin has solvent method, carbon dioxide supercritical extraction method, supercritical ultrasonics technology, biological complex enzyme at present
The disadvantages of method etc., the generally existing recovery rate of these methods is low, extraction operation difficulty is big or extraction cost is high.Accordingly, it is badly in need of one kind
Overcome disadvantage mentioned above, efficiently mentioning for the purple sweet potato cyanidins of advantages such as easy to operate, recovery rate is high, extraction cost is low can be taken into account
Take method.
Summary of the invention
Technical assignment of the invention is in view of the above shortcomings of the prior art, to provide that a kind of extraction cost is low, recovery rate is high
Purple sweet potato cyanidin extracting method.
The present invention provides a kind of extracting methods of purple sweet potato cyanidin, its main feature is that the following steps are included:
A, metal salt solution, 1- ethyl-3-methylimidazole acetate and 1- ethyl -3- methyl are added in purple sweetpotato slurries
Imidazoles diethyl phosphate salt is simultaneously uniformly mixed, after ultrasonic wave, microwave cooperating act on 5~10min, continuation Microwave Extraction 5~
15min, extracting solution take supernatant after decoloration removal of impurities, clarification, and supernatant is concentrated and dried to obtain extraction cream, purple sweetpotato slurries, metal
The weight ratio of salt, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole diethyl phosphate salt be 1:0.6~
1.2:0.8~2.3:0.5~1.5, preferably 1:0.8~1:1.2~1.8:0.8~1.2；
B, extraction cream centrifuge separation, collects filtrate, and concentrating filter liquor is dried to obtain purple sweet potato cyanidin extract.
With metal salt solution, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole diethyl phosphate salt pair
After purple sweet potato powder pretreatment, extracts with ultrasonic wave, microwave cooperating, and cooperate subsequent Microwave Extraction, can mention to greatest extent
Rise the extraction efficiency of purple sweet potato cyanidin.
The purple sweetpotato slurries can be used any one existing mashing mode and be made, preferably are as follows: purple sweetpotato slice, it is sweet with purple
Potato skin dries together, crushes to obtain purple sweet potato powder, and purple sweet potato powder carries out liquid nitrogen at -5 DEG C~-10 DEG C and is beaten to obtain purple sweetpotato slurries.
Drying temperature is preferably 30~50 DEG C, and the time is preferably 20~40h.The partial size of purple sweetpotato is preferably 120~200 mesh.
In step a, the concentration of metal salt solution be preferably 0.1g/L~0.3g/L(optium concentration be 0.15g/L~
0.25g/L), the metal salt is inorganic metal salt, preferably zinc sulfate, magnesium chloride or copper sulphate.Ultrasonic power is preferably
190~210W；Microwave power is preferably 300~400W, and Extracting temperature is preferably 25~30 DEG C.Extracting solution is preferably de- with active carbon
Color removal of impurities, is clarified with tripolite solution.
Carry out solution clarification when, tripolite solution mass concentration is preferably 1.2~2.0%, after uniform stirring stand 5~
20min clarification.
In step b, extraction cream is preferably centrifuged 10~20min with 10000~12000r/min under room temperature；Filtrate is preferred
Be concentrated into original volume 1/3 that rotary evaporation is concentrated into original volume is depressurized at 50~54 DEG C, usually 0.5~1.5h.
When large-scale production, centrifugal operation preferably uses butterfly centrifugal, and centrifuging temperature is 15~20 DEG C, and feed rate is
3.0~3.5 ton/hours.
Drying process preferably uses vacuum freeze drying, and drying temperature is preferably -30~-8 DEG C, and vacuum degree is preferably 60-
70Pa.It dries to purple sweet potato cyanidin moisture content≤2%.
The extracting method of purple sweet potato cyanidin of the invention have compared with prior art it is following prominent the utility model has the advantages that
One, anthocyanidin is extracted using purple sweetpotato skin together, compared with prior art its cost input bottom, saving material, production
Rate is high.
Two, it is beaten using the anthocyanidin powder low temperature liquid nitrogen of small particle, then is used after being mixed with inorganic metal salt, ionic liquid
Combination of ultrasound microwave extracts simultaneously, can increase substantially the recovery rate of cyanine.
Three, it is assisted by metal ion, microwave-ultrasound is used cooperatively, and simple process is convenient for operation, and the anthocyanidin prepared
Yield is high, with high purity, reduces the waste of raw material, and organic solvent-free residual alleviates the pollution to environment, saved and be produced into
This, has higher economic and social benefit.
In specific implementation of the invention, the recovery rate up to 75% or more of anthocyanidin is extracted from purple sweetpotato, and pure
Degree up to 50% or more；And the recovery rate 51% extracted only with microwave and combination of ultrasound, it is assisted only with ultrasound and metal salt
The recovery rate of extraction is 43%, is 46% only with microwave and the recovery rate of metal salt assisted extraction, triplicity extracting method
Recovery rate be much higher than any of which.
In addition, the anthocyanidin of high-purity has higher value medical health care and broader practical application area.
Four, using vacuum freeze drying, have rate of drying fast, procyanidine is avoided to generate variation because heated, guarantee
Quality, and the problem of high temperature causes anthocyanidin degradation and physiological activity to reduce when preventing conventionally spray-dried.
Five, the present invention overcomes temperature in traditional mode of production is higher, dissolution rate is lower, and organic reagent dosage is more, at high cost, effect
The low disadvantage of rate.It is not only easy to operate, be conducive to industrialization, so that purple sweetpotato cell is discharged more anthocyanidin, greatly improve
The extraction efficiency of purple sweet potato cyanidin, both reduces process costs, improves economic benefit, and reduces technological operation hardly possible
Degree makes technology and technique of the present invention have bigger operability and applied.Therefore the achievable scale of the present invention,
Industrialization production increases the economic value of purple sweetpotato, extends purple sweetpotato industrial chain.
Specific embodiment
It is described in detail below with extracting method of the specific embodiment to purple sweet potato cyanidin of the invention.
Unless otherwise instructed, the content of following each ingredients used is mass percentage content.
[embodiment one]
Extraction step:
S1. the preparation of purple sweet potato powder
Purple sweetpotato is sliced, is dried together with purple sweetpotato skin, crushing obtains partial size as 170 mesh purple sweet potato powders；
S2. it extracts and cleans
Purple sweet potato powder carries out liquid nitrogen at -5 DEG C and is beaten to obtain purple sweetpotato slurries, and addition concentration is that 0.2g/L zinc sulfate is water-soluble
Liquid, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole diethyl phosphate salt, and be uniformly mixed, purple sweetpotato slurry
The weight of liquid, zinc sulfate solution, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole diethyl phosphate salt
Than for 1:0.9:1.5:1；
With 200W ultrasonic wave, 350W microwave, is acted synergistically after 8min under the conditions of 25~30 DEG C, continue Microwave Extraction
10min；
By decolorization and impurity removal by active carbon, the tripolite solution that mass concentration is 1.6% is added, is stood after uniform stirring
10min filters to take supernatant, is concentrated and dried to obtain extraction cream；
S3. separation and concentration
Extraction cream obtained by S2 at room temperature, is centrifugated 15min with 11000r/min, abandons precipitating, collect supernatant；
Gained supernatant is concentrated under reduced pressure into the 1/3(1.1h of original volume with Rotary Evaporators at 52 DEG C)；
S4. it dries
Under the conditions of -20 DEG C, vacuum degree 65Pa, vacuum freeze drying obtains purple to purple sweet potato cyanidin moisture content≤2%
Sweet potato anthocyanin extract.
S5. it detects
For purple sweet potato cyanidin extract compared with anthocyanidin standard items pair, the two mass spectrum is very close.Detect to obtain recovery rate
75.6%, purity 52.3%.
[embodiment two]
Extraction step is basically the same as the first embodiment, and difference is that the metal salt added in step S2 is the chlorination of 0.2g/L
Magnesium aqueous solution.
Through detecting, product recovery rate is 76.9%, purity 55.1%.
[embodiment three]
Extraction step is basically the same as the first embodiment, and difference is that the metal salt added in step S2 is the sulfuric acid of 0.2g/L
Copper liquor.
Through detecting, product recovery rate is 75.7%, purity 53.6%.
[comparative example one]
Extraction step is basically the same as the first embodiment, and difference is to be not added with metal salt in step S2.
Through detecting, product recovery rate is 51%, purity 48.2%.
[comparative example two]
Extraction step is basically the same as the first embodiment, and difference is in step S2 not using microwave treatment, only super with 400W
Sonicated 25min.
Through detecting, product recovery rate is 43.2%, purity 41.7%.
[comparative example three]
Extraction step is basically the same as the first embodiment, and difference is in step S2 not using ultrasonication, only with 400W
Microwave treatment 25min.
Through detecting, product recovery rate is 46.8%, purity 39.2%.
Claims (7)
1. a kind of extracting method of purple sweet potato cyanidin, it is characterised in that the following steps are included:
A, metal salt solution, 1- ethyl-3-methylimidazole acetate and 1- ethyl-3-methylimidazole are added in purple sweetpotato slurries
Diethyl phosphate salt is simultaneously uniformly mixed, and after ultrasonic wave, microwave cooperating act on 5~10min, is continued 5~15min of Microwave Extraction, is mentioned
It takes liquid after decoloration removal of impurities, clarification, takes supernatant, supernatant is concentrated and dried to obtain extraction cream, purple sweetpotato slurries, metal salt, 1- second
The weight ratio of base -3- N-Methylimidazoleacetic salt and 1- ethyl-3-methylimidazole diethyl phosphate salt be 1:0.6~1.2:0.8~
2.3:0.5~1.5；Ultrasonic power is 190~210W；Microwave power is 300~400W；Extracting temperature is 25~30 DEG C；
B, extraction cream centrifuge separation, collects filtrate, and concentrating filter liquor, vacuum freeze drying obtain purple sweet potato cyanidin extract,
Drying temperature is -30~-8 DEG C, vacuum degree 60-70Pa.
2. the extracting method of purple sweet potato cyanidin according to claim 1, it is characterised in that:
Purple sweetpotato slice, dries together with purple sweetpotato skin, crushes to obtain purple sweet potato powder, purple sweet potato powder carries out at -5 DEG C~-10 DEG C
Liquid nitrogen is beaten to obtain purple sweetpotato slurries.
3. the extracting method of purple sweet potato cyanidin according to claim 1 or claim 2, it is characterised in that: in step a, metal salt is molten
The concentration of liquid is 0.1g/L~0.3g/L, and the metal salt is zinc sulfate, magnesium chloride or copper sulphate.
4. the extracting method of purple sweet potato cyanidin according to claim 1 or claim 2, it is characterised in that: in step a, extracting solution with
Decolorization and impurity removal by active carbon is clarified with tripolite solution.
5. the extracting method of purple sweet potato cyanidin according to claim 4, it is characterised in that: tripolite solution mass concentration is
1.2~2.0%, 5~20min clarification is stood after uniform stirring.
6. the extracting method of purple sweet potato cyanidin according to claim 1 or claim 2, it is characterised in that: in step b, extract cream with
10000~12000r/min is centrifuged 10~20min under room temperature；
Filtrate depressurizes be concentrated into original volume 1/3 that rotary evaporation is concentrated into original volume at 50~54 DEG C.
7. the extracting method of purple sweet potato cyanidin according to claim 2, it is characterised in that: drying temperature is 30~50 DEG C,
Time is 20~40h.
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| CN201811257680.XA CN109020941B (en) | 2018-10-26 | 2018-10-26 | A kind of extracting method of purple sweet potato cyanidin |
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| CN115089729A (en) * | 2022-06-29 | 2022-09-23 | 西安交通大学 | Preparation method of beta-cyclodextrin purple sweet potato anthocyanin microcapsules |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333149A (en) * | 2013-06-20 | 2013-10-02 | 吕梁学院 | Extraction method of date peel cyanidin |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103333149A (en) * | 2013-06-20 | 2013-10-02 | 吕梁学院 | Extraction method of date peel cyanidin |
Non-Patent Citations (3)
| Title |
|---|
| 不同提取条件对圆茄子花青素提取率的影响;张亦竹，等;《生物学通报》;20141231;第49卷(第10期);摘要 |
| 离子液体超声辅助提取黑果腺肋花楸果中花青素的工艺研究;宋健刚，等;《吉林化工学院学报》;20180930;第35卷(第9期);第28页第2.2.3节、表3 |
| 紫薯花青素的提取及稳定性比较研究;韩成云，等;《食品科技》;20161231;第41卷(第1期);第166页第1.1节、第1.3节 |
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