CN107573317A - A kind of extracting method of blueberry anthocyanin - Google Patents
A kind of extracting method of blueberry anthocyanin Download PDFInfo
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- CN107573317A CN107573317A CN201710933586.0A CN201710933586A CN107573317A CN 107573317 A CN107573317 A CN 107573317A CN 201710933586 A CN201710933586 A CN 201710933586A CN 107573317 A CN107573317 A CN 107573317A
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- blueberry
- rice
- anthocyanidin
- extracting method
- dry powder
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Abstract
The present invention discloses a kind of extracting method of the multiple anthocyanidin of blueberry, rice extract is fermented as extraction auxiliary agent by the use of aspergillus oryzae, and assisted microwave synthesis processing is logical, the extraction of peracetic acid ethyl ester and D101 macroporous resin purifications, ethanol elution is finally utilized, blueberry anthocyanin powder is prepared in freeze-drying.The blueberry anthocyanin powder anthocyanidin content being prepared using the present invention is higher than traditional handicraft by 10% ~ 14%, and technical foundation is provided for the production and processing of anthocyanidin.
Description
Technical field
The invention belongs to the preparation method of natural biologic material, more particularly to a kind of extracting method of blueberry anthocyanin.
Background technology
Containing abundant nutritional ingredient in Blueberry, having prevents cranial nerve aging, protection eyesight, cardiac stimulant, anticancer, soft
It is high to change function, the nutritional ingredients such as blood vessel, enhancing human organism be immune.The anthocyanidin contained in blueberry, it is other fruit such as apple, Portugal
Even tens times of several times of grape, total amino acid content 0.254% is also higher than hawthorn.Blueberry anthocyanin inoxidizability is very strong, to eye
Section and cardiovascular and cerebrovascular disease have the effect of preferable, can play the multiple efficacies such as beauty and health care.But blueberry is spent in the prior art
The recovery rate of blue or green element is still very low.
Such as number of patent application CN201210487338.5, a kind of extracting method of the good blueberry anthocyanin of stability, first will
Raw material is ground into 20-60 targeted fine powders；Again with 60% ethanol water extraction three times, Extracting temperature is 50 DEG C, and extraction time is respectively
2h、2h、1h；Then will be concentrated in vacuo recovery ethanol after by concentrate add pure water precipitation impurity elimination after by supernatant after UF membrane again
Secondary vacuum concentration；Supercritical CO again2Extract and separate, and extraction temperature is 35 DEG C, pressure 25MPa；It is true after final refining impurity elimination
Sky is dried, and dry cream is pulverized and sieved and adds inspection after auxiliary material is well mixed, pack, storage；The blueberry anthocyanin carries
Method is taken to obtain high-quality blueberry using the cryogenic separation such as membrane separation technique and supercritical fluid extraction and fractionation technology technology is extractable and carry
Thing powder is taken, it is not easy to change, and stability is good.Number of patent application CN201510847783.1, the extracting method of blueberry anthocyanin,
Extracting method is as follows：First, in flash extracter, by blueberry and the broken extraction of extract solution, extract solution is filtered to obtain；2nd, will extraction
Liquid and oil phase hybrid extraction, separate to obtain oil phase and aqueous phase；3rd, oil phase is mixed into back extraction with citric acid extraction liquid, obtains aqueous phase extracted；
4th, after mixing aqueous phase and aqueous phase extracted, anthocyanidin filtrate is separated to obtain using membrane separation process, then anthocyanidin filtrate is concentrated, be dry
Dry acquisition anthocyanidin.Blueberry is efficiently effectively crushed in a short time using flash extracter, while in high-speed stirred
Under, the contact and collision of increase extract solution and broken blueberry material, reduce extraction time.There is provided the citric acid water of step 3 simultaneously
The strip stage of solution, using anthocyanidin property more stable in citric acid solution, by the anthocyanidin in oil phase be stripped to
Aqueous citric acid solution.Therefore, the impurity content in anthocyanidin extract solution is few, and the purity of the anthocyanidin obtained through UF membrane is high.
And for example number of patent application CN201010246735.4, a kind of a kind of extracting method of blueberry anthocyanin, there is provided blueberry
The extracting method of anthocyanidin, specifically comprises the following steps：(1) pretreatment of raw material；(2) extraction of blueberry anthocyanin, by feed liquid
Volume ratio adds extract solution extraction, obtains leaching liquor；It is collected by centrifugation, merges the supernatant of 2 extraction centrifugations of clarification；Centrifuge, subtract
Pressure is concentrated to give blueberry anthocyanin crude extract；(3) blueberry anthocyanin is refined, and blueberry anthocyanin crude extract is by macroreticular resin
Absorption, elution, eluent is concentrated under reduced pressure, blueberry anthocyanin concentrate is freeze-dried or is spray-dried obtain blueberry anthocyanin into
Product.The present invention solves blueberries Seasonal Harvest and is not easy to store by force, unsalable blueberries economic damage huge caused by rotting
The problem of mistake；Present invention process is simple, and operation is controllable, and cost is low, pollution-free, particularly suitable for scale extraction blueberry anthocyanin
Method.
The content of the invention
It is an object of the invention to provide a kind of method is simple, cost is low, be easy to industrialized production, there is higher blueberry
The method of anthocyanidin recovery rate.
The aspergillus oryzae that the present invention uses isA.orgzae SP-01。
Specifically, technical scheme is as follows：
A kind of extracting method of blueberry anthocyanin, is comprised the steps of：
（1）60 ~ 80 parts of high quality white rice is taken, clear water is cleaned, and is added water enchroachment (invasion) to steep to rice and is reached no hard core, will be invaded the rice that soaks and is put into
Boil ripe without viscous to rice in electric cooker, then cooked rice is dispensed to container, inoculation aspergillus oryzae and simultaneously mixed, is placed in 35
DEG C, ferment 4 ~ 6 days under more than 90% damp condition；The aspergillus oryzae inoculum concentration is 2 ~ 4%；
（2）Take the rice after fermentation 4 ~ 6 days to be put into container, add the phosphate buffer of its quality 10 ~ 20%, after homogeneous 3min,
5min is centrifuged under 4200r/min, takes supernatant standby；The phosphate buffer pH is 6.5 ~ 7.5；
Preferably, the rice after fermenting 4 days is taken to be extracted.
（3）Blueberry fresh fruit is cleaned, fast frozen is carried out to blueberry fresh fruit with liquid nitrogen, quickly blueberry is smashed to pieces, then added
The step of its quality 5 ~ 10%（2）Gained supernatant, it is well mixed, it is dry in -80 DEG C of freezings with freeze drier after 10 ~ 30min
It is dry, blueberry dry powder is made；Moisture in the blueberry dry powder should be less than 5%；The liquid nitrogen temperature be -30 ~ -50 DEG C, flow be 4 ~
5m/s；
（4）Blueberry dry powder is taken, according to 1g：Blueberry dry powder and acetum are well mixed by 10 ~ 30ml solid-liquid ratio, use citric acid
PH to 2 ~ 4 is adjusted, at 40 ~ 60 DEG C, 420w power microwaves processing 20s, 60 ~ 130min is extracted, obtains anthocyanidin crude extract；Institute
It is 3 ~ 4mol/L to state acetate concentration；
（5）Anthocyanidin crude extract is taken, adds the citric acid of its volume 5 ~ 8%, the step of adding its volume 5 ~ 8%（2）Gained supernatant
Liquid, be extracted with ethyl acetate 3 times, non-ester layer is added in D101 macroporous resin columns, first cleaned with ultra-pure water it is de-, then with ethanol-
Aqueous systems elute, and collect 50% ethanol eluate, are concentrated under reduced pressure, and are freeze-dried, and obtain refined anthocyanidin powder.The citric acid
PH is 3 ~ 5, and concentration is 0.3 ~ 0.5g/ml.
As a further improvement on the present invention, in the extraction of the blueberry anthocyanin, addition aspergillus oryzae fermentation rice extraction
Thing, suppress polyphenol oxidase using its active material, so as to improve the recovery rate of anthocyanidin.
Rice contains vanillic acid, syringic acid, forulic acid, coumaric acid and the styrene acid of free state, while also contains
Syringic acid, forulic acid, coumaric acid and the styrene acid of reference state, wherein the forulic acid of free state and reference state is major phenolic
Material, aldehydes matter have very strong antioxidation, can neutralize the free radical in human body, have to health and protect well
Shield acts on.
Utilize aspergillus oryzaeA.orgzaeSP-01 fermentation rice, then extracts the aldehydes matter in fermentation rice, its is main
Aldehydes matter is kojic acid and forulic acid, compared to the kojic acid and forulic acid of same concentration, is obtained in fermenting rice extract from aspergillus
The forulic acid of kojic acid there is stronger antioxidation.Suppress polyphenol oxidase using the material, blueberry anthocyanin can be improved
Recovery rate.
The beneficial effects of the invention are as follows：
1st, kojic acid and forulic acid are mainly contained in aspergillus oryzae fermentation rice product, can effectively suppresses polyphenol oxidase enzyme activity in blueberry
Property, handled using liquid nitrogen and crush blueberries, significantly reduced the activity for aoxidizing more phenolase, improve the extraction of follow-up anthocyanidin
Rate；
2nd, raw material of the invention is all from natural products, meets requirement of the social people to food " matter " now, has good
Development prospect.
3rd, technology of the invention is simple, easily operated, and technical foundation is provided for large-scale industrial production.
Embodiment
With reference to specific embodiment, the present invention is further described, and not as limitation of the present invention.
Embodiment 1
（1）60 parts of high quality white rice is taken, clear water is cleaned, and is added water enchroachment (invasion) to steep to rice and is reached no hard core, will be invaded the rice that soaks and is put into electricity
Boil ripe without viscous to rice in pot for cooking rice, then cooked rice dispensed to container, inoculation aspergillus oryzae and simultaneously mixed, be placed in 35 DEG C,
Fermented 4 days under more than 90% damp condition；The aspergillus oryzae inoculum concentration is 2%；
（2）Take the rice after fermentation 4 days to be put into container, add the phosphate buffer of its quality 10%, after homogeneous 3min,
5min is centrifuged under 4200r/min, takes supernatant standby；The phosphate buffer pH is 6.5；
（3）Blueberry fresh fruit is cleaned, fast frozen is carried out to blueberry fresh fruit with liquid nitrogen, quickly blueberry is smashed to pieces, then adds its matter
The step of measuring 5%（2）Gained supernatant, it is well mixed, with freeze drier in -80 DEG C of freeze-dryings, obtained blueberry after 10min
Dry powder；Moisture in the blueberry dry powder should be less than 5%；The liquid nitrogen temperature is -50 DEG C, flow 4m/s；
（4）Blueberry dry powder is taken, according to 1g：Blueberry dry powder and acetum are well mixed by 10ml solid-liquid ratio, are adjusted with citric acid
PH to 4 is saved, at 40 DEG C, 420w power microwaves processing 20s, 60min is extracted, obtains anthocyanidin crude extract；The acetate concentration
For 3mol/L；
（5）Anthocyanidin crude extract is taken, adds the citric acid of its volume 5%, the step of adding its volume 5%（2）Gained supernatant, use
Ethyl acetate is extracted 3 times, and non-ester layer is added in D101 macroporous resin columns, is first cleaned and taken off with ultra-pure water, then uses ethanol-water system
Elution, 50% ethanol eluate is collected, is concentrated under reduced pressure, be freeze-dried, obtain refined anthocyanidin powder.The citric acid pH is 3,
Concentration is 0.3g/ml.
In the present embodiment, blueberry anthocyanin recovery rate is 340mg/100g blueberries.
Embodiment 2
（1）80 parts of high quality white rice is taken, clear water is cleaned, and is added water enchroachment (invasion) to steep to rice and is reached no hard core, will be invaded the rice that soaks and is put into electricity
Boil ripe without viscous to rice in pot for cooking rice, then cooked rice dispensed to container, inoculation aspergillus oryzae and simultaneously mixed, be placed in 35 DEG C,
Fermented 6 days under more than 90% damp condition；The aspergillus oryzae inoculum concentration is 4%；
（2）Take the rice after fermentation 6 days to be put into container, add the phosphate buffer of its quality 10 ~ 20%, after homogeneous 3min,
5min is centrifuged under 4200r/min, takes supernatant standby；The phosphate buffer pH is 7.5；
（3）Blueberry fresh fruit is cleaned, fast frozen is carried out to blueberry fresh fruit with liquid nitrogen, quickly blueberry is smashed to pieces, then adds its matter
The step of amount 5 ~ 10%（2）Gained supernatant, it is well mixed, with freeze drier in -80 DEG C of freeze-dryings, obtained indigo plant after 30min
Certain kind of berries dry powder；Moisture in the blueberry dry powder should be less than 5%；The liquid nitrogen temperature is -50 DEG C, flow 5m/s；
（4）Blueberry dry powder is taken, according to 1g：Blueberry dry powder and acetum are well mixed by 10 ~ 30ml solid-liquid ratio, use citric acid
PH to 4 is adjusted, at 60 DEG C, 420w power microwaves processing 20s, 60 ~ 130min is extracted, obtains anthocyanidin crude extract；The vinegar
Acid concentration is 4mol/L.
（5）Anthocyanidin crude extract is taken, adds the citric acid of its volume 8%, the step of adding its volume 8%（2）Gained supernatant
Liquid, be extracted with ethyl acetate 3 times, non-ester layer is added in D101 macroporous resin columns, first cleaned with ultra-pure water it is de-, then with ethanol-
Aqueous systems elute, and collect 50% ethanol eluate, are concentrated under reduced pressure, and are freeze-dried, and obtain refined anthocyanidin powder.The citric acid
PH is 5, concentration 0.5g/ml.
In the present embodiment, blueberry anthocyanin recovery rate is 327mg/100g blueberries.
Embodiment 3
（1）70 parts of high quality white rice is taken, clear water is cleaned, and is added water enchroachment (invasion) to steep to rice and is reached no hard core, will be invaded the rice that soaks and is put into electricity
Boil ripe without viscous to rice in pot for cooking rice, then cooked rice dispensed to container, inoculation aspergillus oryzae and simultaneously mixed, be placed in 35 DEG C,
Fermented 4 days under more than 90% damp condition；The aspergillus oryzae inoculum concentration is 3%；
（2）Take the rice after fermentation 4 days to be put into container, add the phosphate buffer of its quality 10 ~ 20%, after homogeneous 3min,
5min is centrifuged under 4200r/min, takes supernatant standby；The phosphate buffer pH is 7；
（3）Blueberry fresh fruit is cleaned, fast frozen is carried out to blueberry fresh fruit with liquid nitrogen, quickly blueberry is smashed to pieces, then adds its matter
The step of measuring 8%（2）Gained supernatant, it is well mixed, with freeze drier in -80 DEG C of freeze-dryings, obtained blueberry after 20min
Dry powder；Moisture in the blueberry dry powder should be less than 5%；The liquid nitrogen temperature is -40 DEG C, flow 4m/s；
（4）Blueberry dry powder is taken, according to 1g：Blueberry dry powder and acetum are well mixed by 20ml solid-liquid ratio, are adjusted with citric acid
PH to 3 is saved, at 50 DEG C, 420w power microwaves processing 20s, 70min is extracted, obtains anthocyanidin crude extract；The acetate concentration
For 3mol/L；
（5）Anthocyanidin crude extract is taken, adds the citric acid of its volume 6%, the step of adding its volume 6%（2）Gained supernatant, use
Ethyl acetate is extracted 3 times, and non-ester layer is added in D101 macroporous resin columns, is first cleaned and taken off with ultra-pure water, then uses ethanol-water system
Elution, 50% ethanol eluate is collected, is concentrated under reduced pressure, be freeze-dried, obtain refined anthocyanidin powder.The citric acid pH is 4,
Concentration is 0.4g/ml.
In the present embodiment, blueberry anthocyanin recovery rate is 343mg/100g blueberries.
Embodiment 4
The present embodiment is comparative example.
The extracting method of blueberry anthocyanin, realized by following steps：
Step 1: 1kg blueberries and 10L extract solutions are put into the extraction vessel of flash extracter, extract solution temperature is risen to 90
At a temperature of DEG C, flash extracter is opened, broken extraction 2min is carried out, is then quenched to less than 60 DEG C, continue broken extraction
10min, obtain broken extract solution；Broken extract solution is filtered into obtain extract solution and filter residue；The extract solution is to include mass concentration to be
The mixed solution of 60% ethanol and 0.2% citric acid.
Step 2: adding isopropyl palmitate oil phase into the extract solution of step 1, stir and evenly mix, it is scattered to obtain extract solution
Phase, the emulsion that oil phase is continuous phase, stand, layering, separate to obtain oil phase and aqueous phase；The body of the extract solution and grease type oil phase
Product ratio is 1 ﹕ 2；It is different that the organic impurity such as colloid, starch, carbohydrate, fat, organic acids and base in extract solution are extracted into palmitic acid
In propyl ester oil phase, wherein, the anthocyanidin of fraction can be also extracted into isopropyl palmitate oil phase.
Step 3: adding extract in the oil phase obtained into step 2, stir, then stand, be layered, separating to extract
Aqueous phase and raffinate oil phase；Wherein, the extract uses mass concentration as 0.2% aqueous citric acid solution, oil phase and extract
Volume ratio be 1 ﹕ 5；
Step 4: the aqueous phase extracted of the aqueous phase of step 2 and step 3 is mixed, anthocyanidin extract solution is obtained；By anthocyanidin extract solution
Use retention relative molecular weight to carry out membrane separation process for 200,000 organic film and separate to obtain anthocyanidin filtrate, then anthocyanidin filtrate is added
Enter in downward film evaporator, concentrated under vacuum, discharge ethanol, obtain concentrate；Then using lyophilized technique to dense
Processing is dried in contracting liquid, obtains 30g anthocyanidin.
The recovery rate of the extracting method of the blueberry anthocyanin of the present embodiment 1 is 300mg/100g.
Each embodiment measures anthocyanidin extracted amount parameter such as table 1.
Blueberry anthocyanin extracted amount in 1 each embodiment of table
| Embodiment | 1 | 2 | 3 | 4 |
| Blueberry anthocyanidin content（mg/100g） | 340 | 327 | 343 | 300 |
The above embodiment of the present invention scheme is only the description of the invention and can not limit the present invention, will with the right of the present invention
Any change in book suitable implication and scope is asked, is all considered to be and is included within the scope of the claims.
Claims (5)
1. a kind of extracting method of blueberry anthocyanin, it is characterised in that comprise the following steps：
（1）60 ~ 80 parts of high quality white rice is taken, clear water is cleaned, and is added water enchroachment (invasion) to steep to rice and is reached no hard core, will be invaded the rice that soaks and is put into
Boil ripe without viscous to rice in electric cooker, then cooked rice is dispensed to container, inoculation aspergillus oryzae and simultaneously mixed, is placed in 35
DEG C, ferment 4 ~ 6 days under more than 90% damp condition；
（2）Take the rice after fermentation 4 ~ 6 days to be put into container, add the phosphate buffer of its quality 10 ~ 20%, after homogeneous 3min,
5min is centrifuged under 4200r/min, takes supernatant standby；
（3）Blueberry fresh fruit is cleaned, fast frozen is carried out to blueberry fresh fruit with liquid nitrogen, quickly blueberry is smashed to pieces, then adds its matter
The step of amount 5 ~ 10%（2）Gained supernatant, it is well mixed, with freeze drier in -80 DEG C of freeze-dryings, system after 10 ~ 30min
Obtain blueberry dry powder；
（4）Blueberry dry powder is taken, according to 1g：Blueberry dry powder and acetum are well mixed by 10 ~ 30ml solid-liquid ratio, use citric acid
PH to 2 ~ 4 is adjusted, at 40 ~ 60 DEG C, 420w power microwaves processing 20s, 60 ~ 130min is extracted, obtains anthocyanidin crude extract；
（5）Anthocyanidin crude extract is taken, adds the citric acid of its volume 5 ~ 8%, the step of adding its volume 5 ~ 8%（2）Gained supernatant
Liquid, be extracted with ethyl acetate 3 times, non-ester layer is added in D101 macroporous resin columns, first cleaned with ultra-pure water it is de-, then with ethanol-
Aqueous systems elute, and collect 50% ethanol eluate, are concentrated under reduced pressure, and are freeze-dried, and obtain refined anthocyanidin powder.
2. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that the aspergillus oryzae inoculum concentration be 2 ~
4%。
3. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that the phosphate buffer pH is
6.5 ~ 7.5, the acetate concentration is 3 ~ 4mol/L.
4. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that the moisture in the blueberry dry powder
5% should be less than；The liquid nitrogen temperature is -30 ~ -50 DEG C, and flow is 4 ~ 5m/s.
5. the extracting method of blueberry anthocyanin according to claim 1, it is characterised in that the citric acid pH is 3 ~ 5, dense
Spend for 0.3 ~ 0.5g/ml.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108530412A (en) * | 2018-06-07 | 2018-09-14 | 盛林蓝莓集团股份有限公司 | A kind of extracting method of blueberry anthocyanin |
| CN108531356A (en) * | 2018-05-15 | 2018-09-14 | 刘兰民 | Jet rice vinegar and the method for extracting jet anthocyanin |
| CN110272405A (en) * | 2019-07-18 | 2019-09-24 | 长春市紫秘笈文化传播有限公司 | A kind of extracting method of anthocyanidin |
| CN110372659A (en) * | 2019-08-07 | 2019-10-25 | 太仓新亚逊生物科技有限公司 | The extraction process of blueberry anthocyanin |
| CN112544420A (en) * | 2020-12-08 | 2021-03-26 | 武汉昱辰信息技术有限责任公司 | Selenium-rich extract prepared from selenium-rich plants, and its preparation method and application |
-
2017
- 2017-10-10 CN CN201710933586.0A patent/CN107573317A/en active Pending
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108531356A (en) * | 2018-05-15 | 2018-09-14 | 刘兰民 | Jet rice vinegar and the method for extracting jet anthocyanin |
| CN108530412A (en) * | 2018-06-07 | 2018-09-14 | 盛林蓝莓集团股份有限公司 | A kind of extracting method of blueberry anthocyanin |
| CN110272405A (en) * | 2019-07-18 | 2019-09-24 | 长春市紫秘笈文化传播有限公司 | A kind of extracting method of anthocyanidin |
| CN110372659A (en) * | 2019-08-07 | 2019-10-25 | 太仓新亚逊生物科技有限公司 | The extraction process of blueberry anthocyanin |
| CN112544420A (en) * | 2020-12-08 | 2021-03-26 | 武汉昱辰信息技术有限责任公司 | Selenium-rich extract prepared from selenium-rich plants, and its preparation method and application |
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Application publication date: 20180112 |