CN101445529B - Process for simultaneously producing platycodon anthocyanin and polysaccharide single component - Google Patents
Process for simultaneously producing platycodon anthocyanin and polysaccharide single component Download PDFInfo
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- CN101445529B CN101445529B CN 200810249508 CN200810249508A CN101445529B CN 101445529 B CN101445529 B CN 101445529B CN 200810249508 CN200810249508 CN 200810249508 CN 200810249508 A CN200810249508 A CN 200810249508A CN 101445529 B CN101445529 B CN 101445529B
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- platycodon
- anthocyanin
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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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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The invention provides a process for simultaneously producing platycodon anthocyanin and polysaccharide single component, which is characterized in that the process comprises the following steps: (1) mixing Platycodon grandiflorum flowers and ethanol, placing into an ultrasonic extractor for extraction, filtering to obtain a filtrate, vacuum concentrating the filtrate, and recovering ethanol to obtain an ethanol-free concentrated solution; (2) extracting the ethanol-free concentrated solution with a mixed solution of n-butanol and water, collecting water-phase fraction, and vacuum concentrating to obtain a crude extract containing platycodon anthocyanin and total polysaccharides; (3) separating the crude extract with a macroporous resin HPD700 chromatography column, rinsing with distilled water to remove water-soluble sugar and other water-soluble impurities, and eluting with ethanol to obtain a mixed solution containing platycodon anthocyanin and polysaccharide; (4) separating the mixed solution with a DEAE-cellulose column, and eluting with distilled water to obtain a crude solution containing neutral polysaccharide single component and platycodon anthocyanin; and (5) separating the crude solution with the DEAE-cellulose column, and eluting with sodium chloride to obtain platycodon anthocyanin and acidic polysaccharide single component. The process has the advantages of high yield, short production period, and low cost.
Description
Technical field
The present invention relates to a kind of technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously, is to utilize coupling macroporous resin and DEAE-cellulose chromatography to prepare the technology of platycodon anthocyanin and polysaccharide single component simultaneously specifically.
Background technology
The Platycodon grandiflouorum campanulaceae, the flower bluish voilet is rich in anthocyanogen, and anthocyanogen is a water colo(u)r, and is bright in luster, and redness, red-purple, purple and blueness are arranged.Safe because of it, most countries (as China, Japan, the U.S., EU member country etc.) all allows it to be used for food color.Having developed many both at home and abroad at present is the anthocyanin class pigment of raw material with the plant resources, studies show that, anthocyanogen has many physiological active functionses, comprises that lipid content, resistance anti-oxidant and that eliminate in free radical, reduction serum and the liver are different and antitumor, prevents body endoperoxides effect etc.For human beings'health, substituting deleterious chemosynthesis food color additive with anthocyanogen is the target that we study, the anthocyanogen that has good stability is simultaneously used as color additive, can be used for the exploitation of some fine foods, and more wide application prospect is arranged.In addition, vegetable polysaccharides also belongs to natural active matter, has physiological actions such as antitumor, anti-ageing, lipopenicillinase, hypoglycemic and raising immunizing power, though its research is started late, the significant pharmacological effect effect of vegetable polysaccharides is paid attention to by people gradually.In addition, the method for traditional purifying active substance mainly adopts organic solvent extraction and ion complexation technology, and there is dissolvent residual rate height in it, and the rate of recovery is low, produces shortcomings such as utilizing difficulty.
Summary of the invention
The present invention aims to provide a kind ofly can overcome above-mentioned defective, yield height, the time is short, solvent consumption is few, simple to operate, cost is low, prepare the technology of platycodon anthocyanin and polysaccharide single component when environmental pollution is little.Its technical scheme is:
A kind of technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously, it is characterized in that adopting following steps: 1) being 75%～85% ethanol with the platycodon flower after bright or the oven dry and volumetric concentration mixes with 1: 15～20 solid-liquid ratio, wherein alcoholic acid pH value is 1～3, put into the ultrasonic extraction device and handle 30～35min down at 30～40 ℃, after the filtration filtrate vacuum concentration is removed alcohol, obtain pure concentrated solution; 2) will go pure concentrated solution with propyl carbinol and the volume ratio mixing solutions extraction of water with 1: 1, platycodon anthocyanin and polysaccharide single component just are dissolved in the water, and aqueous portion is taken out also vacuum concentration, obtain platycodon anthocyanin and total reducing sugar crude extract; 3) with macroporous resin HPD700 chromatography column on platycodon anthocyanin and the total reducing sugar crude extract, go out water-soluble sugar and other water-soluble impurity with distilled water, and then with the pH value be 1, volumetric concentration is the mixed solution that 40%～60% ethanol elution obtains platycodon anthocyanin and polysaccharide; 4), be that 1～3 distilled water wash-out obtains neutral polysaccharide single component and the thick liquid of platycodon anthocyanin by the pH value with DEAE-cellulose column on the mixed solution of platycodon anthocyanin and polysaccharide; 5), obtain platycodon anthocyanin single component and acidic polysaccharose single component by the NaCl wash-out that the pH value is 1～3, concentration is 0.2～0.4mol/L with DEAE-cellulose column on the thick liquid of platycodon anthocyanin.
The described technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously, in the step 1), extracting platycodon anthocyanin and the used method of polysaccharide is the auxiliary acidifying alcohol extracting of ultrasonic wave, temperature is controlled at 30～40 ℃ during vacuum concentration.
The described technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously, step 2) in, extract concentrated solution and before last macroporous resin HPD700 chromatography column, extract with the propyl carbinol water mixed liquid earlier, thereby remove contained saponin class impurity in the extracting solution.
The described technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously in the step 1), adopts HCl to regulate the pH value of ethanol extract, and used equipment is the flask that has the water of condensation circulation tube in the leaching process.
The present invention compared with prior art; adopt macroporous resin HPD700 and DEAE-Mierocrystalline cellulose coupling technique that platycodon anthocyanin and polysaccharide single component are carried out separation and purification; not only platycodon anthocyanin and polysaccharide single component can access simultaneously a plurality of; and active substance rate of recovery height; organic solvent residual is low; production cost is low, and the cycle is short, is easy to suitability for industrialized production.
Embodiment
Embodiment 1:
Step 1: with pH be 1, volumetric concentration is that 75% ethanol 300mL mixes with the dried platycodon flower of 20g, puts into the ultrasonic extraction device and handle 30min under 30 ℃ of temperature, after the filtration filtrate removed alcohol at 30 ℃ of following vacuum concentration, obtains pure concentrated solution;
Step 2: will go pure concentrated solution with propyl carbinol and water with 1: 1 volume ratio mixing solutions extraction 3 times, platycodon anthocyanin and polysaccharide single component just are dissolved in the water, and aqueous portion is taken out also vacuum concentration, obtain platycodon anthocyanin and total reducing sugar crude extract;
Step 3: platycodon anthocyanin and total reducing sugar crude extract 3mL are gone up macroporous resin HPD700 chromatography column, go out water-soluble sugar and other water-soluble impurity with distilled water, when the phenolsulfuric acid method detects no water-soluble sugar outflow, and then with the pH value be 1, volumetric concentration is the mixed solution that 40% ethanol elution obtains platycodon anthocyanin and polysaccharide;
Step 4: the mixed solution 1mL of platycodon anthocyanin and polysaccharide is gone up the DEAE-cellulose column, is that 1 distilled water wash-out obtains neutral polysaccharide single component and the thick liquid of platycodon anthocyanin by the pH value;
Step 5: the thick liquid 1mL of platycodon anthocyanin is gone up the DEAE-cellulose column, obtain platycodon anthocyanin single component and acidic polysaccharose single component by the NaCl wash-out that the pH value is 1, concentration is 0.2mol/L.
Embodiment 2:
Step 1: with pH be 3, volumetric concentration is that 85% ethanol 400mL mixes with the dried platycodon flower of 20g, puts into the ultrasonic extraction device and handle 35min under 40 ℃ of temperature, after the filtration filtrate removed alcohol at 40 ℃ of following vacuum concentration, obtains pure concentrated solution;
Step 2: will go pure concentrated solution with propyl carbinol and water with 1: 1 volume ratio mixing solutions extraction 3 times, platycodon anthocyanin and polysaccharide single component just are dissolved in the water, and aqueous portion is taken out also vacuum concentration, obtain platycodon anthocyanin and total reducing sugar crude extract;
Step 3: platycodon anthocyanin and total reducing sugar crude extract 3mL are gone up macroporous resin HPD700 chromatography column, go out water-soluble sugar and other water-soluble impurity with distilled water, when the phenolsulfuric acid method detects no water-soluble sugar outflow, and then with the pH value be 3, volumetric concentration is the mixed solution that 60% ethanol elution obtains platycodon anthocyanin and polysaccharide;
Step 4: the mixed solution 1mL of platycodon anthocyanin and polysaccharide is gone up the DEAE-cellulose column, is that 3 distilled water wash-out obtains neutral polysaccharide single component and the thick liquid of platycodon anthocyanin by the pH value;
Step 5: the thick liquid 1mL of platycodon anthocyanin is gone up the DEAE-cellulose column, obtain platycodon anthocyanin single component and acidic polysaccharose single component by the NaCl wash-out that the pH value is 3, concentration is 0.4mol/L.
Through UV spectrum and elution profile spectrum analysis, obtain component and be all polysaccharide or anthocyanogen single component, and polysaccharide and anthocyanogen separating effect are better.
Claims (4)
1. technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously, it is characterized in that adopting following steps: 1) being 75%～85% ethanol with the platycodon flower after bright or the oven dry and volumetric concentration mixes with 1: 15～20 solid-liquid ratio, wherein alcoholic acid pH value is 1～3, put into the ultrasonic extraction device and handle 30～35min down at 30～40 ℃, after the filtration filtrate vacuum concentration is removed alcohol, obtain pure concentrated solution; 2) will go pure concentrated solution with propyl carbinol and the volume ratio mixing solutions extraction of water with 1: 1, platycodon anthocyanin and polysaccharide single component just are dissolved in the water, and aqueous portion is taken out also vacuum concentration, obtain platycodon anthocyanin and total reducing sugar crude extract; 3) with macroporous resin HPD700 chromatography column on platycodon anthocyanin and the total reducing sugar crude extract, go out water-soluble sugar and other water-soluble impurity with distilled water, and then with the pH value be 1～3, volumetric concentration is the mixed solution that 40%～60% ethanol elution obtains platycodon anthocyanin and polysaccharide; 4), be that 1～3 distilled water wash-out obtains neutral polysaccharide single component and the thick liquid of platycodon anthocyanin by the pH value with DEAE-cellulose column on the mixed solution of platycodon anthocyanin and polysaccharide; 5), obtain platycodon anthocyanin single component and acidic polysaccharose single component by the NaCl wash-out that the pH value is 1～3, concentration is 0.2～0.4mol/L with DEAE-cellulose column on the thick liquid of platycodon anthocyanin.
2. the technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously as claimed in claim 1 is characterized in that: in the step 1), extracting platycodon anthocyanin and the used method of polysaccharide is the auxiliary acidifying alcohol extracting of ultrasonic wave, and temperature is controlled at 30～40 ℃ during vacuum concentration.
3. the technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously as claimed in claim 1; it is characterized in that: step 2) in; extract concentrated solution and before last macroporous resin HPD700 chromatography column, extract with the propyl carbinol water mixed liquid earlier, thereby remove contained saponin class impurity in the extracting solution.
4. the technology for preparing platycodon anthocyanin and polysaccharide single component simultaneously as claimed in claim 1 is characterized in that: in the step 1), adopt HCl to regulate the pH value of ethanol extract, used equipment is the flask that has the water of condensation circulation tube in the leaching process.
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| CN101445529A CN101445529A (en) | 2009-06-03 |
| CN101445529B true CN101445529B (en) | 2011-05-04 |
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| CN110180216B (en) * | 2019-06-11 | 2021-05-25 | 南京农业大学 | Method and device for extracting and purifying anthocyanin by ultrasonic-enhanced fluidized bed type resin adsorption-desorption |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101104645A (en) * | 2007-06-22 | 2008-01-16 | 山东理工大学 | Method for extracting balloonflower polysaccharide assisted by ultrasound wave |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101104645A (en) * | 2007-06-22 | 2008-01-16 | 山东理工大学 | Method for extracting balloonflower polysaccharide assisted by ultrasound wave |
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