CN103435588A - Novel method for preparing blueberry anthocyanidin - Google Patents
Novel method for preparing blueberry anthocyanidin Download PDFInfo
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- CN103435588A CN103435588A CN2013104127651A CN201310412765A CN103435588A CN 103435588 A CN103435588 A CN 103435588A CN 2013104127651 A CN2013104127651 A CN 2013104127651A CN 201310412765 A CN201310412765 A CN 201310412765A CN 103435588 A CN103435588 A CN 103435588A
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Abstract
The invention relates to a novel method for preparing blueberry anthocyanidin and in particular relates to a method combining enzymolysis with microwave. The novel method for preparing the blueberry anthocyanidin is characterized by comprising the following steps: a, smashing blueberry fruits by adopting a plant tissue destroying and extracting method; b, carrying out enzymolysis on the smashed blueberry; c, carrying out microwave extraction; and d, adsorbing and purifying anthocyanidin in an extracting solution by adopting macroporous adsorption resin, and then carrying out reduced pressure concentration and freeze drying, thus the anthocyanidin is obtained. When the novel method for preparing the blueberry anthocyanidin is adopted for treating the anthocyanidin, operation is easy, less pollution is produced, extraction time is short, extraction ratio is high, and purity of the anthocyanidin product is high, so that the novel method for preparing the blueberry anthocyanidin is applicable to industrial production of blueberry anthocyanidin.
Description
Technical field
The present invention relates to a kind of separation purification method of effective components in plants, particularly relate to a kind of novel method for preparing vaccinium oxycoccus pigment.
Background technology
Blueberry, formal name used at school cowberry, Ericaceae Vaccinium plant, perennial fallen leaves or evergreen shrubs.Blueberry mostly is mazarine, and subcircular is one of rare blue food.Fruits nutrition is abundant, contains the various active compositions such as VITAMIN, protein, anthocyanidin and flavones, and wherein anthocyanidin content occupies first of all fruit, vegetables.In the every hectogram fresh fruit of wild species blueberry, anthocyanidin content, up to 0.33 ~ 3.38g, is generally 0.1 ~ 0.2g in the every hectogram fresh fruit of cultivar.Anthocyanidin claims again cyanidin(e), is that a class extensively is present in the water-soluble natural pigment in plant, belongs to flavonoid compound, and the form existence mainly with glucosides, also claim anthocyanogen.The different physiological roles such as that cyanidin(e) has is anti-oxidant, antitumor, protection liver, vision enhancing, have huge application prospect at aspects such as food, cosmetic, medicine.
The research of the current extraction to anthocyanidin mainly contains water extraction or organic solvent extraction method, supercritical fluid extraction etc.There are the structure that can destroy anthocyanidin due to excess Temperature in traditional water extraction or solvent-extraction process, affect the problems such as its biological activity and productive rate reduction; Although modern supercritical extraction extraction yield is high, because of apparatus expensive, is not suitable for suitability for industrialized production.And the mode that plant tissue broken extracts, enzymolysis-microwave extraction combines both can be relatively mild that plant tissue is broken, decompose, improve by a relatively large margin yield, simultaneously the three-dimensional arrangement of survivable composition also.
Summary of the invention
Technical problem to be solved by this invention is: for the deficiencies in the prior art, provide a kind of method for preparing vaccinium oxycoccus pigment of efficient, low cost, high yield, high purity, applicable suitability for industrialized production.
Technical scheme of the present invention is carried out according to the following step:
1. pulverize blue berry with the plant tissue Smashing extraction method, wherein add 30 ~ 50% ethanolic soln of 0.5 ~ 2 times of weight ratio of blueberry, plant tissue smashing extractor rotating speed is 1000 ~ 3000r/min, extraction time 0.5 ~ 1.0min;
2. to the cellulase that adds blueberry weight 1 ~ 3% in above-mentioned extracting solution, hydrolysis temperature is 60 ~ 80 ℃, and regulating the extracting solution pH value is 2 ~ 4, and enzymolysis time is 50 ~ 70min, and concentrating under reduced pressure, obtain enriched material;
3. enriched material is added to 40 ~ 60% ethanol, Gu material is placed in microwave to be extracted than being 1:15 ~ 20, microwave condition is: power 100 ~ 200W, and extraction time is 1.5 ~ 2min, centrifugal removal of impurities afterwards obtains supernatant liquor;
4. supernatant liquor is joined to macroporous adsorptive resins, first use the distilled water wash-out of 2 ~ 3 times of sample liquid, then use 60 ~ 80% ethanolic soln wash-out, effluent volume is 15 ~ 20 times of sample liquid, collect elutriant, finally by rotary evaporation, lyophilize obtains the vaccinium oxycoccus pigment powder.
Macroreticular resin described in step 4 is NKA-9, D-101, AB-8 etc.
Compared with prior art, the present invention adopts the plant tissue Smashing extraction method to process raw material, and whole process only completes in to tens of seconds in the several seconds, simultaneously owing to having removed heating from, thereby can effectively avoid the destruction of Anthocyanins.Enzymolysis-microwave extraction method is extracted anthocyanidin, and low to the loss of vaccinium oxycoccus pigment composition, extraction yield is large, and the purity of product is high.The inventive method is simple, easily implements, and result of use is good.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
embodiment:
Embodiment 1: take blueberry fresh fruit 100g, with the plant tissue Smashing extraction method, pulverize blue berry, add 30% ethanolic soln of 0.5 times of weight ratio of blueberry, plant tissue smashing extractor rotating speed is 1500r/min, extraction time 1.0min; To the cellulase that adds blueberry weight 1% in above-mentioned extracting solution, hydrolysis temperature is 60 ℃, and regulating the extracting solution pH value is 2, and enzymolysis time is 50min, and concentrating under reduced pressure, obtain enriched material; To the ethanol that adds 40% in concentrated solution, Gu material than being 1:15, the microwave that is placed in power 100W is extracted, extraction time is 1.5min, centrifugal removal of impurities afterwards obtains supernatant liquor; Above-mentioned supernatant liquor is joined to the AB-8 macroporous adsorptive resins, first use the distilled water wash-out of 2 times of sample liquid, use again 60% ethanolic soln wash-out, effluent volume is 15 times of sample liquid, collect elutriant, finally by rotary evaporation, lyophilize obtains vaccinium oxycoccus pigment powder 254.2mg, through HPLC, detect, its purity is 54.3%.
Embodiment 2: take blueberry fresh fruit 100g, with the plant tissue Smashing extraction method, pulverize blue berry, add 50% ethanolic soln of 1 times of weight ratio of blueberry, plant tissue smashing extractor rotating speed is 2000r/min, extraction time 0.8min; To the cellulase that adds blueberry weight 2% in above-mentioned extracting solution, hydrolysis temperature is 70 ℃, and regulating the extracting solution pH value is 3.5, and enzymolysis time is 60min, and concentrating under reduced pressure, obtain enriched material; To the ethanol that adds 50% in concentrated solution, Gu material than being 1:18, the microwave that is placed in power 150W is extracted, extraction time is 1.8min, centrifugal removal of impurities afterwards obtains supernatant liquor; Above-mentioned supernatant liquor is joined to the NKA-9 macroporous adsorptive resins, first use the distilled water wash-out of 3 times of sample liquid, use again 70% ethanolic soln wash-out, effluent volume is 20 times of sample liquid, collect elutriant, finally by rotary evaporation, lyophilize obtains vaccinium oxycoccus pigment powder 256.8mg, through HPLC, detect, its purity is 56.9%.
Embodiment 3: take blueberry fresh fruit 100g, with the plant tissue Smashing extraction method, pulverize blue berry, add 40% ethanolic soln of 1.5 times of weight ratios of blueberry, plant tissue smashing extractor rotating speed is 3000r/min, extraction time 0.5min; To the cellulase that adds blueberry weight 3% in above-mentioned extracting solution, hydrolysis temperature is 80 ℃, and regulating the extracting solution pH value is 4, and enzymolysis time is 70min, and concentrating under reduced pressure, obtain enriched material; To the ethanol that adds 60% in concentrated solution, Gu material than being 1:20, the microwave that is placed in power 200W is extracted, extraction time is 2.0min, centrifugal removal of impurities afterwards obtains supernatant liquor; Above-mentioned supernatant liquor is joined to the D-101 macroporous adsorptive resins, first use the distilled water wash-out of 2.5 times of sample liquid, use again 80% ethanolic soln wash-out, effluent volume is 18 times of sample liquid, collect elutriant, finally by rotary evaporation, lyophilize obtains vaccinium oxycoccus pigment powder 255.8mg, through HPLC, detect, its purity is 53.5%.
Claims (3)
1. a novel method for preparing vaccinium oxycoccus pigment comprises the following steps:
A, with the plant tissue Smashing extraction method, pulverize blueberry fresh fruit, wherein add 30 ~ 50% ethanolic soln of 0.5 ~ 2 times of weight ratio of blueberry, plant tissue smashing extractor rotating speed is 1000 ~ 3000r/min, extraction time 0.5 ~ 1.0min;
B, to the cellulase that adds blueberry weight 1 ~ 3% in above-mentioned extracting solution, hydrolysis temperature is 60 ~ 80 ℃, regulating the extracting solution pH value is 2 ~ 4, enzymolysis time is 50 ~ 70min, concentrating under reduced pressure, obtain enriched material;
C, enriched material is added to 40 ~ 60% ethanol, Gu material is placed in microwave to be extracted than being 1:15 ~ 20, microwave condition is: power 100 ~ 200W, and extraction time is 1.5 ~ 2min, centrifugal removal of impurities afterwards obtains supernatant liquor;
D, supernatant liquor is joined to macroporous adsorptive resins, first use the distilled water wash-out of 2 ~ 3 times of sample liquid, then use 60 ~ 80% ethanolic soln wash-out, effluent volume is 15 ~ 20 times of sample liquid, collect elutriant, finally by rotary evaporation, lyophilize obtains the vaccinium oxycoccus pigment powder.
2. the novel method for preparing vaccinium oxycoccus pigment according to claim 1, is characterized in that, the acid of the adjusting pH value described in step b is the mineral acids such as hydrochloric acid, sulfuric acid.
3. the novel method for preparing vaccinium oxycoccus pigment according to claim 1, is characterized in that, the macroreticular resin described in steps d is NKA-9, D-101, AB-8 etc.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992300A (en) * | 2014-05-30 | 2014-08-20 | 云南朱提苦荞生物科技开发有限公司 | Method for extracting procyanidine from tartary buckwheat bran |
| CN104725341A (en) * | 2015-02-12 | 2015-06-24 | 贵州省生物研究所 | Efficient extraction method for blueberry anthocyanin |
| CN104817527A (en) * | 2015-03-31 | 2015-08-05 | 广西大学 | Method for extracting anthocyanidin from pitaya peel |
| CN104974548A (en) * | 2015-06-13 | 2015-10-14 | 常州大学 | Extraction method of a natural vegetable dye capable of changing along with change of environment |
| CN106046079A (en) * | 2016-05-27 | 2016-10-26 | 合肥工业大学 | Method for rapidly separating and preparing peonidin-3-caffeoyl sophoroside-5-glucoside from purple sweet potatoes |
| CN106083796A (en) * | 2016-06-20 | 2016-11-09 | 仇颖莹 | A kind of extracting method of vaccinium oxycoccus pigment |
| CN106349205A (en) * | 2016-08-26 | 2017-01-25 | 浙江奇异鸟生物科技有限公司 | Extraction method of blueberry anthocyanins |
| CN106442701A (en) * | 2016-11-28 | 2017-02-22 | 山东省分析测试中心 | Mass spectrometry method based on single-pixel solid-phase extraction technology and application thereof |
| CN107828238A (en) * | 2017-10-30 | 2018-03-23 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins process for refining |
| CN107841157A (en) * | 2017-10-30 | 2018-03-27 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins extraction process |
| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
| CN110256393A (en) * | 2019-06-17 | 2019-09-20 | 上海交通大学 | A method of threeleaf akebia anthocyanidin is extracted using RF assistance biological complex enzyme |
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2013
- 2013-09-12 CN CN2013104127651A patent/CN103435588A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103992300A (en) * | 2014-05-30 | 2014-08-20 | 云南朱提苦荞生物科技开发有限公司 | Method for extracting procyanidine from tartary buckwheat bran |
| CN104725341A (en) * | 2015-02-12 | 2015-06-24 | 贵州省生物研究所 | Efficient extraction method for blueberry anthocyanin |
| CN104817527A (en) * | 2015-03-31 | 2015-08-05 | 广西大学 | Method for extracting anthocyanidin from pitaya peel |
| CN104974548A (en) * | 2015-06-13 | 2015-10-14 | 常州大学 | Extraction method of a natural vegetable dye capable of changing along with change of environment |
| CN106046079B (en) * | 2016-05-27 | 2018-07-13 | 合肥工业大学 | A method of quick separating prepares paeonidin -3- caffeoyl sophoroside -5- glucosides from purple sweet potato |
| CN106046079A (en) * | 2016-05-27 | 2016-10-26 | 合肥工业大学 | Method for rapidly separating and preparing peonidin-3-caffeoyl sophoroside-5-glucoside from purple sweet potatoes |
| CN106083796A (en) * | 2016-06-20 | 2016-11-09 | 仇颖莹 | A kind of extracting method of vaccinium oxycoccus pigment |
| CN106349205A (en) * | 2016-08-26 | 2017-01-25 | 浙江奇异鸟生物科技有限公司 | Extraction method of blueberry anthocyanins |
| CN106442701A (en) * | 2016-11-28 | 2017-02-22 | 山东省分析测试中心 | Mass spectrometry method based on single-pixel solid-phase extraction technology and application thereof |
| CN106442701B (en) * | 2016-11-28 | 2023-07-21 | 山东省分析测试中心 | Mass spectrum imaging analysis method based on single-pixel solid-phase extraction technology and application thereof |
| CN107828238A (en) * | 2017-10-30 | 2018-03-23 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins process for refining |
| CN107841157A (en) * | 2017-10-30 | 2018-03-27 | 潍坊友容实业有限公司 | A kind of Suaeda salsa Betacyanins extraction process |
| CN109082911A (en) * | 2018-07-05 | 2018-12-25 | 佛山市衣香蒂丝服装设计有限公司 | A kind of colouring method of dye yam extracting solution to silk fabric |
| CN110256393A (en) * | 2019-06-17 | 2019-09-20 | 上海交通大学 | A method of threeleaf akebia anthocyanidin is extracted using RF assistance biological complex enzyme |
| CN110256393B (en) * | 2019-06-17 | 2022-12-27 | 上海交通大学 | Method for extracting akebia trifoliata anthocyanin by using radio frequency-assisted biological complex enzyme |
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Application publication date: 20131211 |