CN109206528A - A kind of fructus lycii functional component high-performance bio extracting method - Google Patents
A kind of fructus lycii functional component high-performance bio extracting method Download PDFInfo
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- CN109206528A CN109206528A CN201810880955.9A CN201810880955A CN109206528A CN 109206528 A CN109206528 A CN 109206528A CN 201810880955 A CN201810880955 A CN 201810880955A CN 109206528 A CN109206528 A CN 109206528A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
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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
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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
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0096—Purification; Precipitation; Filtration
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Abstract
The present invention relates to a kind of fructus lycii functional component high-performance bio extracting methods.Detailed process includes that cleaning, rehydration, broken, cryogenic vacuum extract, centrifuge separation, extract from extraction crude protein and polysaccharides in extracting solution and from fructus lycii pulp thick pigment.Technological merit of the invention is that polysaccharides, crude protein and thick pigment can be successively extracted from fructus lycii, and extraction conditions are mild, and recovery rate is high, and retains the bioactivity of fructus lycii functional component to the greatest extent, and technological operation is simple.
Description
Technical field
The invention belongs to bioactive ingredients extractive technique fields, and in particular to a kind of fructus lycii functional component high-performance bio mentions
Take method.
Background technique
Studies have shown that main active has the pigments such as polysaccharides, thick protein and carotenoid, fructus lycii in fructus lycii
Polysaccharide is a kind of water-soluble polysaccharide, it, which has, promotes immune, anti-aging, antitumor, removing free radical, antifatigue, reducing blood lipid, drop
Blood glucose adjusts the effects of immune, anti-radiation, liver protection, reproductive function protection and improvement.As people are to the weight of fructus lycii medicine price cheating value
Diopter increases, and the extracting method of polysaccharides and application become research hotspot.Some researches show that the contents of thick protein in fructus lycii
Up to 14%, during extracting polysaccharide, the extraction of crude protein does not cause the enough attention of people, causes great wave
Take.In addition to this, fructus lycii also contains the pigments such as a large amount of carotenoid, wherein the zeaxanthin contained, has significant improving eyesight to make
With.The existing extraction to efficacy active component in fructus lycii is mostly the extraction to polysaccharides, and technique is mostly traditional hot water extraction
Hot water extraction after method or organic solvent degreasing, solvent usage is big in these conventional methods, time-consuming and recovery rate is low.With skill
The raising of art level, in recent years, the methods of enzymolysis and extraction, Microwave Extraction and film filtering extraction are used, according to current research
The intervention of microwave equipment is likely to decrease the activity of polysaccharides；The yield of polysaccharide can be improved using enzymatic isolation method, but due to needing
High temperature enzyme deactivation is carried out to the material after enzymatic hydrolysis, to eliminate the activity of enzyme, the temperature of enzyme deactivation is generally at 100 DEG C or so, in enzyme deactivation
In the process, it also will be greatly reduced the activity of polysaccharides；The extraction conditions of film filtering are more mild, have centainly to the activity of polysaccharide
Protective effect, but since material composition is complicated in extracting solution, molecular size is different, need the film of different pore size by multiple
Filtering, equipment input cost is big, complex process.
One kind how is provided to can effectively protect functional component activity and can sufficiently extract polysaccharides, crude protein and thick pigment
Production technology, become the direction of very valuable research.
Summary of the invention
It is living the purpose of the present invention is disclosing a kind of polysaccharides, crude protein and thick pigment etc. of capable of successively extracting from fructus lycii
Property ingredient extraction process, so that the utilization rate of fructus lycii is reached maximum.
Following technical scheme is used to achieve the purpose of the present invention.
A kind of fructus lycii functional component high-performance bio extracting method, comprising the following steps:
(1) dry wolfberry is taken, impurity elimination is sorted, after cleaning, the pure water of 6-10 times of fructus lycii weight is added, feed liquid is squeezed into crushing together
Equipment is crushed；
(2) to the fructus lycii of step (1) crush liquid in activated cellulase and pectase is added, with sodium bicarbonate adjust pH to
Crushing liquid is squeezed into vacuum extraction tank and is extracted 2-4 hours by 8-9；
(3) said extracted liquid is centrifugated, collects the fructus lycii pulp of supernatant and lower layer respectively；
(4) after filtering the supernatant of step (3) by diatomite, filtrate is extracted, is separated, is freeze-dried and obtains fructus lycii
Polysaccharide and protein；
(5) after draining fructus lycii pulp isolated in step (3), put into vacuum back-flow tower, with ethyl alcohol be extractant into
Row refluxing extraction obtains thick pigment after separation, drying.
The dosage of cellulase described in step (2) and pectase is respectively 10-30mg/L, 30-60mg/L.
For the vacuum degree control of vacuum extraction in-90kPa-- 80kPa, temperature is maintained at 40-60 DEG C in step (2).
Extraction process described in step (4) is that relative molecular weight is added into filtrate in the polyethylene glycol of 1000-4000
(PEG) and potassium citrate, formed PEG and potassium citrate mass fraction be respectively 15-20%, 20%-25% extraction system after shake
Swing extraction.
The extraction system adjusts pH 6.5-7.5 with buffer.
The volume fraction of extractant ethyl alcohol is 70-90% in step (5).
For the vacuum degree control of step (5) vacuum back-flow in-80kPa-- 60kPa, temperature is maintained at 50-60 DEG C.
Present invention determine that extraction stage most effective solid-liquid ratio, vacuum degree and Extracting temperature, utmostly ensure that Chinese holly
The recovery rate and bioactivity of Qi polysaccharide and crude protein；PH, the substance of extraction crude protein and polysaccharides extracting system has been determined
Composition, mass fraction, the crude protein being obtained by extraction and polysaccharides are with high purity, activity stabilized；It is thick to be determined that vacuum back-flow extracts
The best solid-liquid ratio of pigment, vacuum degree and Extracting temperature, the yield height of thick pigment and not easy in inactivation.
Technological merit of the invention is that polysaccharides, crude protein and thick pigment can be successively extracted from fructus lycii, extracts item
Part is mild, and recovery rate is high, and retains the bioactivity of fructus lycii functional component to the greatest extent, and technological operation is simple.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described.
Embodiment 1:
(1) dry wolfberry sorts impurity elimination and drains after pure water spray cleaning, spare；
(2) 6 times of fructus lycii weight of pure water is added, is uniformly mixed, feed liquid is squeezed into beater crushing together.It stands, will float on
The fructus lycii seed of liquid level removes；
(3) 10mg/L cellulase and 30mg/L pectase through overactivation are added in crushing liquid, while will with sodium bicarbonate
The pH for crushing liquid is transferred to 8；
(4) liquid will be crushed after processing to squeeze into vacuum extraction tank, by vacuum degree control in -90kPa--80kPa, temperature is maintained at
It 40 DEG C, extracts 2 hours；
(5) extracting solution is squeezed into seperator and is centrifuged, collected supernatant for extracting polysaccharides and crude protein, sink
The fructus lycii to form sediment is meat in the thick pigment of extraction；
(6) after filtering the supernatant of step (5) by diatomite, filtrate is obtained.Relative molecular weight 1000 is added into filtrate
Polyethylene glycol (PEG) and potassium citrate, make in filtrate the mass fraction of PEG and potassium citrate be respectively 15% and 20%, simultaneously
Be 6.5 with buffer adjustment pH, will adjustment treated that filtrate squeezes into oscillation device vibrates 1 hour；
(7) filtrate after above-mentioned oscillation treatment is squeezed into centrifuge to be centrifuged, filtrate is divided into two layers after centrifugation, crude protein distribution
In the PEG solution on upper layer, polysaccharides is distributed in the potassium citrate solution of lower layer；
(8) potassium citrate is added again into above-mentioned steps (7) at the middle and upper levels PEG solution, vibrates, centrifugation is distributed in crude protein
In the potassium citrate solution of lower layer.Lower layer's potassium citrate solution is passed through into ion exchange column, after removing potassium citrate, vacuum refrigeration
It is dry to obtain crude protein.Upper layer PEG solution recycles.
(9) lower layer's potassium citrate solution passes through ion exchange column in above-mentioned steps (7), after removing potassium citrate, vacuum
Freeze-drying obtains polysaccharides；
(10) fructus lycii pulp obtained in above-mentioned steps (5) is drained, is placed in vacuum back-flow device, fructus lycii meat quality is added
The ethyl alcohol that 4 times of volume fraction is 70%, the vacuum degree control of reflux is in -80kpa, and temperature is maintained at 50 DEG C, and refluxing extraction 1 is small
When.
(11) above-mentioned reflux extracting liquid is taken, vacuum dehydrating at lower temperature obtains thick pigment, ethyl alcohol recycling.
Embodiment 2:
(1) dry wolfberry sorts impurity elimination and drains after pure water spray cleaning, spare；
(2) 10 times of fructus lycii weight of pure water is added, is uniformly mixed, feed liquid is squeezed into beater crushing together.It stands, will float on
The fructus lycii seed of liquid level removes；
(3) 30mg/L cellulase and 60mg/L pectase through overactivation are added in crushing liquid, while will with sodium bicarbonate
The PH for crushing liquid is transferred to 9；
(4) liquid will be crushed after processing to squeeze into vacuum extraction tank, by vacuum degree control in -80kpa, temperature is maintained at 60 DEG C, leaching
It mentions 4 hours；
(5) extracting solution is squeezed into seperator and is centrifuged, collected supernatant for extracting polysaccharides and crude protein, sink
The fructus lycii to form sediment is meat in the thick pigment of extraction；
(6) after filtering the supernatant of step (5) by diatomite, filtrate is obtained.Relative molecular weight 4000 is added into filtrate
Polyethylene glycol (PEG) and potassium citrate, make in filtrate the mass fraction of PEG and potassium citrate be respectively 20% and 25%, simultaneously
Be 7.5 with buffer adjustment pH, will adjustment treated that filtrate squeezes into oscillation device vibrates 2 hours；
(7) filtrate after above-mentioned oscillation treatment is squeezed into centrifuge to be centrifuged, filtrate is divided into two layers after centrifugation, crude protein distribution
In the PEG solution on upper layer, polysaccharides is distributed in the potassium citrate solution of lower layer；
(8) potassium citrate is added again into above-mentioned steps (7) at the middle and upper levels PEG solution, vibrates, centrifugation is distributed in crude protein
In the potassium citrate solution of lower layer.Lower layer's potassium citrate solution is passed through into ion exchange column, after removing potassium citrate, vacuum refrigeration
It is dry to obtain crude protein.Upper layer PEG solution recycles.
(9) lower layer's potassium citrate solution passes through ion exchange column in above-mentioned steps (7), after removing potassium citrate, vacuum
Freeze-drying obtains polysaccharides；
(10) fructus lycii pulp obtained in above-mentioned steps (5) is drained, is placed in vacuum back-flow device, fructus lycii meat quality is added
The ethyl alcohol that 6 times of volume fraction is 90%, the vacuum degree control of reflux is in -60kPa, and temperature is maintained at 60 DEG C, and refluxing extraction 2 is small
When.
(11) above-mentioned reflux extracting liquid is taken, vacuum dehydrating at lower temperature obtains thick pigment, ethyl alcohol recycling.
Claims (7)
1. a kind of fructus lycii functional component high-performance bio extracting method, comprising the following steps:
(1) dry wolfberry is taken, impurity elimination is sorted, after cleaning, the pure water of 6-10 times of fructus lycii weight is added, feed liquid is squeezed into crushing together
Equipment is crushed；
(2) to the fructus lycii of step (1) crush liquid in activated cellulase and pectase is added, with sodium bicarbonate adjust pH to
Crushing liquid is squeezed into vacuum extraction tank and is extracted 2-4 hours by 8-9；
(3) said extracted liquid is centrifugated, collects the fructus lycii pulp of supernatant and lower layer respectively；
(4) after filtering the supernatant of step (3) by diatomite, filtrate is extracted, is separated, is freeze-dried and obtains fructus lycii
Polysaccharide and protein；
(5) after draining fructus lycii pulp isolated in step (3), put into vacuum back-flow tower, with ethyl alcohol be extractant into
Row refluxing extraction obtains thick pigment after separation, drying.
2. a kind of fructus lycii functional component high-performance bio extracting method according to claim 1, it is characterised in that in step (2)
The dosage of the cellulase and pectase is respectively 10-30mg/L, 30-60mg/L.
3. a kind of fructus lycii functional component high-performance bio extracting method according to claim 1, it is characterised in that in step (2)
The vacuum degree control of vacuum extraction is maintained at 40-60 DEG C in-90kPa-- 80kPa, temperature.
4. a kind of fructus lycii functional component high-performance bio extracting method according to claim 1, it is characterised in that step (4) institute
The extraction process stated is that relative molecular weight is added into filtrate in the polyethylene glycol (PEG) and potassium citrate of 1000-4000, is formed
The mass fraction of PEG and potassium citrate be respectively 15-20%, 20%-25% extraction system after oscillation extraction.
5. a kind of fructus lycii functional component high-performance bio extracting method according to claim 4, it is characterised in that the extraction
System adjusts pH 6.5-7.5 with buffer.
6. a kind of fructus lycii functional component high-performance bio extracting method according to claim 1, it is characterised in that in step (5)
The volume fraction of extractant ethyl alcohol is 70-90%.
7. a kind of fructus lycii functional component high-performance bio extracting method according to claim 1, it is characterised in that step (5) is true
The vacuum degree control of backlash stream is maintained at 50-60 DEG C in-80kPa-- 60kPa, temperature.
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| CN201810880955.9A CN109206528A (en) | 2018-08-04 | 2018-08-04 | A kind of fructus lycii functional component high-performance bio extracting method |
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| CN201810880955.9A CN109206528A (en) | 2018-08-04 | 2018-08-04 | A kind of fructus lycii functional component high-performance bio extracting method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110092846A (en) * | 2019-05-30 | 2019-08-06 | 遵义医科大学 | A method of extracting Dendrobium officinale polysaccharide |
| CN110305231A (en) * | 2019-06-24 | 2019-10-08 | 温州广立生物医药科技有限公司 | A kind of the extraction preparation method and its extract equipment of lycium ruthenicum polysaccharide |
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| CN1743341A (en) * | 2005-09-16 | 2006-03-08 | 杨雪 | Method for preparing lycium barbarum polysaccharides |
| CN101134783A (en) * | 2007-10-19 | 2008-03-05 | 大连工业大学 | Method for preparing sea-tangle polysaccharide |
| CN104558229A (en) * | 2014-12-31 | 2015-04-29 | 江苏大学 | Separating and purifying method for Chinese wolfberry polyose |
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2018
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Patent Citations (3)
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| CN1743341A (en) * | 2005-09-16 | 2006-03-08 | 杨雪 | Method for preparing lycium barbarum polysaccharides |
| CN101134783A (en) * | 2007-10-19 | 2008-03-05 | 大连工业大学 | Method for preparing sea-tangle polysaccharide |
| CN104558229A (en) * | 2014-12-31 | 2015-04-29 | 江苏大学 | Separating and purifying method for Chinese wolfberry polyose |
Non-Patent Citations (2)
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| 卢艳敏: "聚合物或离子液体/柠檬酸钾双水相分离纯化蛋白质的研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110092846A (en) * | 2019-05-30 | 2019-08-06 | 遵义医科大学 | A method of extracting Dendrobium officinale polysaccharide |
| CN110305231A (en) * | 2019-06-24 | 2019-10-08 | 温州广立生物医药科技有限公司 | A kind of the extraction preparation method and its extract equipment of lycium ruthenicum polysaccharide |
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Application publication date: 20190115 |