CN101434972A - Process for preparing Lonicera edulis anthocyanin by solid state biological reaction - Google Patents
Process for preparing Lonicera edulis anthocyanin by solid state biological reaction Download PDFInfo
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- CN101434972A CN101434972A CNA2008102096696A CN200810209669A CN101434972A CN 101434972 A CN101434972 A CN 101434972A CN A2008102096696 A CNA2008102096696 A CN A2008102096696A CN 200810209669 A CN200810209669 A CN 200810209669A CN 101434972 A CN101434972 A CN 101434972A
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Abstract
A process which uses a solid-state biological reaction method for preparing loniceraedulis anthocyanin relates to a preparation method of natural anthocyanin. The invention solves the problems that when the natural anthocyanin is extracted by the existing chemical method, the extraction rate is low, the purity is not high, and the production process is complicated. The process which uses the solid-state biological reaction method for preparing the loniceraedulis anthocyanin comprises the following steps: firstly an immobilized biological reaction method is used for extracting the loniceraedulis anthocyanin, later purification is carried out with the macroporous resin, then a vacuum scraper type thin film is used for concentrating the purified liquid, and finally loniceraedulis anthocyanin powder is obtained by vacuum drying crush. The loniceraedulis anthocyanin prepared by the invention consists of a plant loniceraedulis extract which can be used as pharmaceutical and food material, causes no side effects to the human body, has good internal antibody oxidation effect, is provided with anti-aging and anti-radiation effects, and can be applied to the fields such as food, health products, cosmetics, medicine, bio-chemical industry, etc.
Description
Technical field
The present invention relates to a kind of Lonicera edulis anthocyanin preparation method.
Background technology
Anthocyanogen is widespread in nature, people are to existing more than the 30 year history of its research, particularly since the eighties in 20th century, the whole world is increasingly extensive and deep to the research of anthocyanogen, and the researchist of states such as moral, method, meaning, U.S., Japan and Korea S. studies at the anthocyanogen of plant.The Heilongjiang Province is the anthocyanogen plant production base of China's maximum, mainly contains kinds such as linberry, Vaccinium uliginosum, indigo fruit, black currant, Vitis Amurensis, tree plum, has profuse anthocyanogen food dye resource.This class pigment is the natural components of food, does not only have safety issue, and has important physical functions such as the lipopenicillinase of flavonoid material, anti-ageing, beauty treatment, beauty treatment, fat-reducing, can be applicable to fields such as food, medicine, makeup.
Indigo really is one of the valuable source in Heilungkiang, and also is the main source of natural anthocyanogen.Though it is at present a lot of to the research of Lonicera edulis anthocyanin, but the extracting method of Lonicera edulis anthocyanin is mainly based on chemical extraction method, chemistry-physics extraction method, extraction yield is all on the low side, the extraction yield of chemical method has only about 40～50%, the extraction yield of chemistry-physics extraction method is the highest also to be no more than 60%, makes the production of Lonicera edulis anthocyanin and utilization all not bring into play its due value.
Summary of the invention
Low in order to solve the Lonicera edulis anthocyanin extraction yield, the problem that purity is not high the invention provides a kind of technology of preparing Lonicera edulis anthocyanin by solid state biological reaction, can effectively improve the extraction yield and the product purity of Lonicera edulis anthocyanin.Among the present invention, the step of the technology of preparing Lonicera edulis anthocyanin by solid state biological reaction is as follows: one, the extraction of Lonicera edulis anthocyanin: earlier with the screening of indigo fruit pomace, remove and rot and impurity, with liquid nitrogen and agitation beads polishing indigo fruit residue is ground into 40 order powder, by mass percentage 91～95% indigos fruits powder and 5～9% water are mixed and make solid-state biological respinse substrate, the viride that adds solid state reaction substrate mass percent 1.0～1.5% then carries out solid state fermentation, the ratio adding mass concentration that with the solid-liquid ratio is 1g:20mL～1g:40mL again is 70% aqueous ethanolic solution, with ultrasonic extraction 25～35 minutes, obtain indigo fruit-aqueous ethanolic solution, use whizzer with the centrifugal indigo fruit-aqueous ethanolic solution of the speed of 3000～5000r/min 5～10min at last, pour out the upper strata extracting solution, the ratio that with the solid-liquid ratio is 1g:20mL～1g:40mL is that 70% aqueous ethanolic solution joins and proceeds supersound extraction and centrifugation in the lower sediment with mass concentration, extract 3 times continuously, remove lower sediment, merging the upper strata extracting solution and being concentrated into anthocyanogen concentration is 8～10g/L, obtains the Lonicera edulis anthocyanin concentrated solution; Two, the purifying of Lonicera edulis anthocyanin: with X-5 macroporous resin chromatography column the Lonicera edulis anthocyanin concentrated solution is adsorbed, obtain the Lonicera edulis anthocyanin extracting solution of purifying then with the stripping liquid desorb; Three, concentrate: the Lonicera edulis anthocyanin extracting solution of purifying is adopted vacuum scraper-type thin film concentration, and concentrated condition is 30～40 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains the Lonicera edulis anthocyanin viscous fluid; Four, dry and pulverize: with the vacuum-freeze-dry machine under 0.4～0.7mbar, temperature-40～50 ℃ condition with Lonicera edulis anthocyanin viscous fluid vacuum-freeze-dry 24 hours and be ground into 60 order powder, promptly get the Lonicera edulis anthocyanin powder.
Among the present invention, the raw material that is adopted is an indigo fruit processing waste---indigo fruit pomace, indigo fruit pomace is utilized again, and both reduce production cost, created high value added product, prevent its pollution again to environment.In the Lonicera edulis anthocyanin extracting method, adopt solid-state biological respinse-ultrasonic wave economic benefits and social benefits extraction anthocyanogen technology, handle cooperation agitation beads Ginding process with nitrogen ultra low temperature indigo fruit residue is carried out micronizing, by solid-state biological respinse indigo fruit fruit powder is degraded again, then by the ultrasonic wave auxiliary extraction, make anthocyanogen be able to abundant release, make the extraction yield of Lonicera edulis anthocyanin can reach 70～80%, than the extraction yield of chemical extraction method or chemistry-physics extraction method high respectively 40～100% and 15～30%.Adopt X-5 macroporous resin chromatography column that Lonicera edulis anthocyanin is carried out purifying, make that anthocyanin content reaches 40～50% in the Lonicera edulis anthocyanin, than the content height of anthocyanogen in the chemical extraction method 50%, improved the added economic value of Lonicera edulis anthocyanin greatly.Adopt vacuum freeze drying technology among the present invention simultaneously, operation is operation at low temperatures, has kept the effective active composition in the indigo fruit greatly, has better kept Lonicera edulis anthocyanin structure and biological activity.Technology of the present invention is simple, extraction yield height, 11 promotion and application.The Lonicera edulis anthocyanin look valency height of the present invention's preparation, the purity height can be used as natural edible red pigment, Antialcoholic liver-protecting drink, the preparation that makes eye bright, radioprotective preparation and beauty treatment Oral preparation.
Embodiment
Embodiment one: in this embodiment, a kind of step of technology of preparing Lonicera edulis anthocyanin by solid state biological reaction is as follows: one, the extraction of Lonicera edulis anthocyanin: earlier with the screening of indigo fruit pomace, remove and rot and impurity, with liquid nitrogen and agitation beads polishing indigo fruit residue is ground into 40 order powder, by mass percentage 91～95% indigos fruits powder and 5～9% water are mixed and make solid-state biological respinse substrate, the viride that adds solid state reaction substrate mass percent 1.0～1.5% then carries out solid state fermentation, the ratio adding mass concentration that with the solid-liquid ratio is 1g:20mL～1g:40mL again is 70% aqueous ethanolic solution, with ultrasonic extraction 25～35 minutes, obtain indigo fruit-aqueous ethanolic solution, use whizzer with the centrifugal indigo fruit-aqueous ethanolic solution of the speed of 3000～5000r/min 5～10min at last, pour out the upper strata extracting solution, the ratio that with the solid-liquid ratio is 1g:20mL～1g:40mL is that 70% aqueous ethanolic solution joins and proceeds supersound extraction and centrifugation in the lower sediment with mass concentration, extract 3 times continuously, remove lower sediment, merging the upper strata extracting solution and being concentrated into anthocyanogen concentration is 8～10g/L, obtains the Lonicera edulis anthocyanin concentrated solution; Two, the purifying of Lonicera edulis anthocyanin: with X-5 macroporous resin chromatography column the Lonicera edulis anthocyanin concentrated solution is adsorbed, obtain the Lonicera edulis anthocyanin extracting solution of purifying then with the stripping liquid desorb; Three, concentrate: the Lonicera edulis anthocyanin extracting solution behind the purifying is adopted vacuum scraper-type thin film concentration, and concentrated condition is 30～40 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains the Lonicera edulis anthocyanin viscous fluid; Four, dry and pulverize: with the vacuum-freeze-dry machine under 0.4～0.7mbar, temperature-40～50 ℃ condition with Lonicera edulis anthocyanin viscous fluid vacuum-freeze-dry 24 hours and be ground into 60 order powder, promptly get the Lonicera edulis anthocyanin powder.
Embodiment two: what this embodiment and embodiment one were different is: the processing condition of solid state fermentation are in the step 1: the pH value of solid-state biological respinse substrate is 5.0～6.5, temperature is 28～35 ℃, fermentation time is 24～48 hours, aeration time was 20～30 seconds in per 10～15 minutes, venting pressure 1.0～1.5Mpa.Other is identical with embodiment one.
Embodiment three: what this embodiment and embodiment one were different is: hyperacoustic power is 300～400W in the step 1.Other is identical with embodiment one.
Embodiment four: what this embodiment and embodiment one were different is: the flow velocity of anthocyanogen concentrated solution is 1.0ml/min in the step 2, and the stripping liquid flow velocity is 1.0～2.0ml/min.Other is identical with embodiment one.
Embodiment five: what this embodiment and embodiment one were different is: stripping liquid is that mass percent concentration is 60%～80% aqueous ethanolic solution in the step 2.Other is identical with embodiment one.
Embodiment six: in this embodiment, the step of the technology of preparing Lonicera edulis anthocyanin by solid state biological reaction is as follows: one, the extraction of Lonicera edulis anthocyanin: earlier with the screening of indigo fruit pomace, remove and rot and impurity, with liquid nitrogen and agitation beads polishing indigo fruit residue is ground into 40 order powder, by mass percentage 91～95% indigos fruits powder and 5～9% water are mixed and make solid-state biological respinse substrate, add the viride of solid state reaction substrate mass percent 1.0～1.5% then, in the pH of solid-state biological respinse substrate value is 5.0～6.5, temperature is 28～35 ℃, fermentation time is 24～48 hours, aeration time was 20～30 seconds in per 10～15 minutes, carry out solid state fermentation under the condition of venting pressure 1.0～1.5Mpa, the ratio adding mass concentration that with the solid-liquid ratio is 1g:20mL～1g:40mL again is 70% aqueous ethanolic solution, with the ultrasonic extraction of power 300～400W 25～35 minutes, obtain indigo fruit-aqueous ethanolic solution, use whizzer with the centrifugal indigo fruit-aqueous ethanolic solution of the speed of 3000～5000r/min 5～10min at last, pour out the upper strata extracting solution, the ratio that with the solid-liquid ratio is 1g:20mL～1g:40mL is that 70% aqueous ethanolic solution joins and proceeds supersound extraction and centrifugation in the lower sediment with mass concentration, extract 3 times continuously, remove lower sediment, merging the upper strata extracting solution and being concentrated into anthocyanogen concentration is 8～10g/L, obtains the Lonicera edulis anthocyanin concentrated solution; Two, the purifying of Lonicera edulis anthocyanin: the Lonicera edulis anthocyanin concentrated solution is adsorbed with X-5 macroporous resin chromatography column, the Lonicera edulis anthocyanin extracting solution that obtains purifying with the stripping liquid desorb wherein then, the flow velocity of anthocyanogen concentrated solution is 1.0ml/min, the stripping liquid flow velocity is 1.0～2.0ml/min, and stripping liquid is that mass percent concentration is 60%～80% aqueous ethanolic solution; Three, concentrate: the Lonicera edulis anthocyanin extracting solution of purifying is adopted vacuum scraper-type thin film concentration, and concentrated condition is 30～40 ℃ of temperature, and vacuum tightness is 0.1～0.15
Mbar obtains the Lonicera edulis anthocyanin viscous fluid; Four, dry and pulverize: with the vacuum-freeze-dry machine under 0.4～0.7mbar, temperature-40～50 ℃ condition with Lonicera edulis anthocyanin viscous fluid vacuum-freeze-dry 24 hours and be ground into 60 order powder, promptly get the Lonicera edulis anthocyanin powder.
The extraction yield of Lonicera edulis anthocyanin is 70～80% in this embodiment, and the content of anthocyanogen is 40～50% in the Lonicera edulis anthocyanin.The look valency height of gained Lonicera edulis anthocyanin powder, quality better.
Embodiment seven: what this embodiment and embodiment six were different is: hyperacoustic power is 350W in the step 1, and ultrasonic time is 30 minutes.Other is identical with embodiment six.
The extraction yield of Lonicera edulis anthocyanin is 70～80% in this embodiment, and the content of anthocyanogen is 40～50% in the Lonicera edulis anthocyanin.The look valency height of gained Lonicera edulis anthocyanin powder, quality better.
Embodiment eight: what this embodiment and embodiment six were different is: the processing condition of solid state fermentation are in the step 1: the pH value of solid-state biological respinse substrate is 6.0, temperature is 30 ℃, fermentation time is 36 hours, aeration time was 30 seconds in per 15 minutes, venting pressure 1.0～1.5Mpa.Other is identical with embodiment six.
The extraction yield of Lonicera edulis anthocyanin is 70～80% in this embodiment, and the content of anthocyanogen is 40～50% in the Lonicera edulis anthocyanin.The look valency height of gained Lonicera edulis anthocyanin powder, quality better.
Claims (5)
1, a kind of technology of preparing Lonicera edulis anthocyanin by solid state biological reaction, the step of technology that it is characterized in that preparing Lonicera edulis anthocyanin by solid state biological reaction is as follows: one, the extraction of Lonicera edulis anthocyanin: earlier with the screening of indigo fruit pomace, remove and rot and impurity, with liquid nitrogen and agitation beads polishing indigo fruit residue is ground into 40 order powder, by mass percentage 91～95% indigos fruits powder and 5～9% water are mixed and make solid-state biological respinse substrate, the viride that adds solid state reaction substrate mass percent 1.0～1.5% then carries out solid state fermentation, the ratio adding mass concentration that with the solid-liquid ratio is 1g:20mL～1g:40mL again is 70% aqueous ethanolic solution, with ultrasonic extraction 25～35 minutes, obtain indigo fruit-aqueous ethanolic solution, use whizzer with the centrifugal indigo fruit-aqueous ethanolic solution of the speed of 3000～5000r/min 5～10min at last, pour out the upper strata extracting solution, the ratio that with the solid-liquid ratio is 1g:20mL～1g:40mL is that 70% aqueous ethanolic solution joins and proceeds supersound extraction and centrifugation in the lower sediment with mass concentration, extract 3 times continuously, remove lower sediment, merging the upper strata extracting solution and being concentrated into anthocyanogen concentration is 8～10g/L, obtains the Lonicera edulis anthocyanin concentrated solution; Two, the purifying of Lonicera edulis anthocyanin: with X-5 macroporous resin chromatography column the Lonicera edulis anthocyanin concentrated solution is adsorbed, obtain the Lonicera edulis anthocyanin extracting solution of purifying then with the stripping liquid desorb; Three, concentrate: the Lonicera edulis anthocyanin extracting solution behind the purifying is adopted vacuum scraper-type thin film concentration, and concentrated condition is 30～40 ℃ of temperature, and vacuum tightness is 0.1～0.15mbar, obtains the Lonicera edulis anthocyanin viscous fluid; Four, dry and pulverize: with the vacuum-freeze-dry machine under 0.4～0.7mbar, temperature-40～50 ℃ condition with Lonicera edulis anthocyanin viscous fluid vacuum-freeze-dry 24 hours and be ground into 60 order powder, promptly get the Lonicera edulis anthocyanin powder.
2, the technology of a kind of preparing Lonicera edulis anthocyanin by solid state biological reaction according to claim 1, the processing condition that it is characterized in that solid state fermentation in the step 1 are: the pH value of solid-state biological respinse substrate is 5.0～6.5, temperature is 28～35 ℃, fermentation time is 24～48 hours, aeration time was 20～30 seconds in per 10～15 minutes, venting pressure 1.0～1.5Mpa.
3, the technology of a kind of preparing Lonicera edulis anthocyanin by solid state biological reaction according to claim 1 is characterized in that hyperacoustic power is 300～400W in the step 1.
4, the technology of a kind of preparing Lonicera edulis anthocyanin by solid state biological reaction according to claim 1, the flow velocity that it is characterized in that anthocyanogen concentrated solution in the step 2 is 1.0ml/min, the stripping liquid flow velocity is 1.0～2.0ml/min.
5, the technology of a kind of preparing Lonicera edulis anthocyanin by solid state biological reaction according to claim 1 is characterized in that stripping liquid is that mass percent concentration is 60%～80% aqueous ethanolic solution in the step 2.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532219A (en) * | 2010-12-20 | 2012-07-04 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying anthocyanin in lonicera caerulea |
| CN102659870A (en) * | 2012-04-24 | 2012-09-12 | 哈尔滨工业大学 | Extracting method of lonicera caerulea anthocyanidin |
| CN103130762A (en) * | 2013-01-31 | 2013-06-05 | 宁波中药制药有限公司 | Method for extracting anthocyanin from indigo indicum |
| CN105125646A (en) * | 2014-09-15 | 2015-12-09 | 广东省农业科学院动物卫生研究所 | Application of trichoderma viride in improving of extraction rate of quercetin in daphniphyllum calycinum and ciderage composition medicinal material |
| CN105294632A (en) * | 2015-11-13 | 2016-02-03 | 大兴安岭林格贝寒带生物科技股份有限公司 | Industrial method for preparing lonicera caerulea fruit anthocyanidin from lonicera caerulea fruits |
| CN109748897A (en) * | 2018-12-26 | 2019-05-14 | 桃源县兴隆米业科技开发有限公司 | It is a kind of purple paddy in extract anthocyanidin method |
-
2008
- 2008-12-12 CN CNA2008102096696A patent/CN101434972A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102532219A (en) * | 2010-12-20 | 2012-07-04 | 大兴安岭林格贝有机食品有限责任公司 | Method for enriching and purifying anthocyanin in lonicera caerulea |
| CN102659870A (en) * | 2012-04-24 | 2012-09-12 | 哈尔滨工业大学 | Extracting method of lonicera caerulea anthocyanidin |
| CN103130762A (en) * | 2013-01-31 | 2013-06-05 | 宁波中药制药有限公司 | Method for extracting anthocyanin from indigo indicum |
| CN103130762B (en) * | 2013-01-31 | 2016-08-03 | 宁波中药制药股份有限公司 | A kind of method extracting anthocyanidin from indigo fruit |
| CN105125646A (en) * | 2014-09-15 | 2015-12-09 | 广东省农业科学院动物卫生研究所 | Application of trichoderma viride in improving of extraction rate of quercetin in daphniphyllum calycinum and ciderage composition medicinal material |
| CN105125646B (en) * | 2014-09-15 | 2018-08-10 | 广东省农业科学院动物卫生研究所 | A kind of application of Trichoderma viride in improving maple knotweed prescription medicinal material in Quercetin recovery rate |
| CN105294632A (en) * | 2015-11-13 | 2016-02-03 | 大兴安岭林格贝寒带生物科技股份有限公司 | Industrial method for preparing lonicera caerulea fruit anthocyanidin from lonicera caerulea fruits |
| CN105294632B (en) * | 2015-11-13 | 2018-08-28 | 大兴安岭林格贝寒带生物科技股份有限公司 | A kind of industrial method preparing indigo fruit anthocyanidin from indigo fruit |
| CN109748897A (en) * | 2018-12-26 | 2019-05-14 | 桃源县兴隆米业科技开发有限公司 | It is a kind of purple paddy in extract anthocyanidin method |
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