CN108440480A - The extracting method of lycium ruthenicum procyanidins and obtained extract - Google Patents
The extracting method of lycium ruthenicum procyanidins and obtained extract Download PDFInfo
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- CN108440480A CN108440480A CN201810300292.9A CN201810300292A CN108440480A CN 108440480 A CN108440480 A CN 108440480A CN 201810300292 A CN201810300292 A CN 201810300292A CN 108440480 A CN108440480 A CN 108440480A
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- lycium ruthenicum
- ethanol water
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- 241000169546 Lycium ruthenicum Species 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000000284 extract Substances 0.000 title claims abstract description 16
- CWEZAWNPTYBADX-UHFFFAOYSA-N Procyanidin Natural products OC1C(OC2C(O)C(Oc3c2c(O)cc(O)c3C4C(O)C(Oc5cc(O)cc(O)c45)c6ccc(O)c(O)c6)c7ccc(O)c(O)c7)c8c(O)cc(O)cc8OC1c9ccc(O)c(O)c9 CWEZAWNPTYBADX-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 229920002414 procyanidin Polymers 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 147
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 55
- 238000010828 elution Methods 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 23
- 229920005989 resin Polymers 0.000 claims abstract description 23
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 11
- 238000002386 leaching Methods 0.000 claims abstract description 8
- 230000002745 absorbent Effects 0.000 claims abstract description 7
- 239000002250 absorbent Substances 0.000 claims abstract description 7
- 239000000945 filler Substances 0.000 claims abstract description 3
- 239000002904 solvent Substances 0.000 claims abstract description 3
- 235000019441 ethanol Nutrition 0.000 claims description 63
- 150000004676 glycans Chemical class 0.000 claims description 32
- 229920001282 polysaccharide Polymers 0.000 claims description 32
- 239000005017 polysaccharide Substances 0.000 claims description 32
- 108090000790 Enzymes Proteins 0.000 claims description 20
- 102000004190 Enzymes Human genes 0.000 claims description 20
- 229940088598 enzyme Drugs 0.000 claims description 20
- 238000000605 extraction Methods 0.000 claims description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 108010059892 Cellulase Proteins 0.000 claims description 12
- 229940106157 cellulase Drugs 0.000 claims description 12
- 229940059442 hemicellulase Drugs 0.000 claims description 8
- 108010002430 hemicellulase Proteins 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000001976 enzyme digestion Methods 0.000 claims description 2
- 238000012545 processing Methods 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- -1 pectase Proteins 0.000 claims 1
- 238000011161 development Methods 0.000 abstract description 3
- 239000003643 water by type Substances 0.000 abstract description 3
- 239000000706 filtrate Substances 0.000 description 36
- 239000000243 solution Substances 0.000 description 27
- 239000000463 material Substances 0.000 description 14
- 238000003756 stirring Methods 0.000 description 7
- 238000010792 warming Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 229920002488 Hemicellulose Polymers 0.000 description 3
- 244000241838 Lycium barbarum Species 0.000 description 3
- 235000015459 Lycium barbarum Nutrition 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 235000013399 edible fruits Nutrition 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- PFTAWBLQPZVEMU-DZGCQCFKSA-N (+)-catechin Chemical compound C1([C@H]2OC3=CC(O)=CC(O)=C3C[C@@H]2O)=CC=C(O)C(O)=C1 PFTAWBLQPZVEMU-DZGCQCFKSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- 235000002710 Ilex cornuta Nutrition 0.000 description 2
- 241001310146 Ilex cornuta Species 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 235000010326 Osmanthus heterophyllus Nutrition 0.000 description 2
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 2
- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 235000021014 blueberries Nutrition 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- ADRVNXBAWSRFAJ-UHFFFAOYSA-N catechin Natural products OC1Cc2cc(O)cc(O)c2OC1c3ccc(O)c(O)c3 ADRVNXBAWSRFAJ-UHFFFAOYSA-N 0.000 description 2
- 235000005487 catechin Nutrition 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 229950001002 cianidanol Drugs 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- XFZJEEAOWLFHDH-UHFFFAOYSA-N (2R,2'R,3R,3'R,4R)-3,3',4',5,7-Pentahydroxyflavan(48)-3,3',4',5,7-pentahydroxyflavan Natural products C=12OC(C=3C=C(O)C(O)=CC=3)C(O)CC2=C(O)C=C(O)C=1C(C1=C(O)C=C(O)C=C1O1)C(O)C1C1=CC=C(O)C(O)=C1 XFZJEEAOWLFHDH-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- MOJZMWJRUKIQGL-FWCKPOPSSA-N Procyanidin C2 Natural products O[C@@H]1[C@@H](c2cc(O)c(O)cc2)Oc2c([C@H]3[C@H](O)[C@@H](c4cc(O)c(O)cc4)Oc4c3c(O)cc(O)c4)c(O)cc(O)c2[C@@H]1c1c(O)cc(O)c2c1O[C@@H]([C@H](O)C2)c1cc(O)c(O)cc1 MOJZMWJRUKIQGL-FWCKPOPSSA-N 0.000 description 1
- 240000000851 Vaccinium corymbosum Species 0.000 description 1
- 244000077233 Vaccinium uliginosum Species 0.000 description 1
- 229930003268 Vitamin C Natural products 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 235000010208 anthocyanin Nutrition 0.000 description 1
- 229930002877 anthocyanin Natural products 0.000 description 1
- 239000004410 anthocyanin Substances 0.000 description 1
- 150000004636 anthocyanins Chemical class 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 229940093797 bioflavonoids Drugs 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000019990 fruit wine Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- FUKUFMFMCZIRNT-UHFFFAOYSA-N hydron;methanol;chloride Chemical compound Cl.OC FUKUFMFMCZIRNT-UHFFFAOYSA-N 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 229960003512 nicotinic acid Drugs 0.000 description 1
- 235000001968 nicotinic acid Nutrition 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 230000000050 nutritive effect Effects 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- HGVVOUNEGQIPMS-UHFFFAOYSA-N procyanidin Chemical compound O1C2=CC(O)=CC(O)=C2C(O)C(O)C1(C=1C=C(O)C(O)=CC=1)OC1CC2=C(O)C=C(O)C=C2OC1C1=CC=C(O)C(O)=C1 HGVVOUNEGQIPMS-UHFFFAOYSA-N 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 235000013343 vitamin Nutrition 0.000 description 1
- 239000011782 vitamin Substances 0.000 description 1
- 229940088594 vitamin Drugs 0.000 description 1
- 229930003231 vitamin Natural products 0.000 description 1
- 235000019154 vitamin C Nutrition 0.000 description 1
- 239000011718 vitamin C Substances 0.000 description 1
- 150000003722 vitamin derivatives Chemical class 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
-
- 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
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Nutrition Science (AREA)
- Food Science & Technology (AREA)
- Mycology (AREA)
- Molecular Biology (AREA)
- Botany (AREA)
- Sustainable Development (AREA)
- General Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention provides the extracting method of lycium ruthenicum procyanidins and obtained extracts.The extracting method of lycium ruthenicum procyanidins, includes the following steps：Using ethanol water as solvent, lycium ruthenicum is extracted, collects leaching liquor；Alcohol volume content in the leaching liquor is adjusted to 80~90%, precipitation, filtering and collecting filter liquid is precipitated；Using macroporous absorbent resin as filler, gradient elution is carried out with the ethanol water of 0% to 15~20% gradient, merges the fraction section that 15~20% ethanol waters elute, is dried to obtain solid-state procyanidine.The present invention can simply and efficiently extract the procyanidine of high-purity, and high income from lycium ruthenicum, utilized to the deep development of lycium ruthenicum and provide new way.
Description
Technical field
The present invention relates to field of food, extracting method more particularly, to lycium ruthenicum procyanidins and obtained extraction
Object.
Background technology
Lycium ruthenicum rich in protein, fat, carbohydrate, free amino acid, organic acid, minerals, trace element, alkaloid,
The various compositions such as vitamin C, B1, B2, calcium, magnesium, copper, zinc, manganese, iron, lead, nickel, cadmium, cobalt, chromium, potassium, sodium.It is detected through science,
Calcium, iron, niacin content are respectively that the 2.3 of red fruit matrimony vine, 4.6,16.7 times, especially procyanidine are more than blueberry (black fruit Chinese holly
Qi 3690mg/100g containing procyanidine；Blueberry 330~3380mg/100g containing procyanidine).This is to find former flower so far
The green highest wild fruit of cellulose content and most effective natural, effect is 20 times of VC, VE 50
Times, the nutrient composition contents such as vitamin, minerals are also very abundant, especially contain with the day for removing free radical, anti-oxidation function
Right anthocyanin element, medicinal, the significantly larger than common red matrimony vine of health value is known as " soft gold ".
Procyanidine, abbreviation OPC are a kind of bioflavonoids having special molecular structure, are to generally acknowledge in the world at present
The effective natural of removing people's interior free yl.
The prior art is also limited to food or extract oil to the utilization of lycium ruthenicum, for example, lycium ruthenicum jam, lycium ruthenicum fruit wine,
Lycium ruthenicum seed oil etc., there is no the procyanidine that deep development is rich in using it.
In view of this, special propose the present invention.
Invention content
The purpose of the present invention is to provide a kind of extracting method of lycium ruthenicum procyanidins, the extracting method can it is simple,
The procyanidine of high-purity, and high income are efficiently extracted from lycium ruthenicum, and offer is utilized to the deep development of lycium ruthenicum
New way.
In order to solve the above technical problems, the present invention provides following technical schemes：
The extracting method of lycium ruthenicum procyanidins, includes the following steps：
Using ethanol water as solvent, lycium ruthenicum is extracted, collects leaching liquor；
Alcohol volume content in the leaching liquor is adjusted to 80~90%, precipitation, filtering and collecting filter liquid is precipitated；
Using macroporous absorbent resin as filler, gradient elution is carried out with the ethanol water of 0% to 15~20% gradient, is merged
The fraction section that 15~20% ethanol waters elute, is dried to obtain solid-state procyanidine.
Since the ingredient type of alcohol-soluble in lycium ruthenicum is complicated, and there are compounds similar in many chemical constitutions, and
And lycium ruthenicum be rich in polysaccharides, to extract and separation there are severe jammings.Therefore, how to eliminate the interference of lycium ruthenicum polysaccharide with
And it is the key that extracting method that the procyanidine of high-purity how is isolated from alcohol extract.
In order to solve the above difficult point, the invention firstly uses the mixed liquors of ethyl alcohol and water to be extracted, by lycium ruthenicum polysaccharide
The equal Alcohol soluble compositions such as water soluble ingredients and procyanidine extract in leaching liquor；Then the spy for utilizing lycium ruthenicum polysaccharide non-alcohol molten
Point makes its precipitation, that is, improves the precipitation generated after ethanol content in leaching liquor, to eliminate its interference to detaching procyanidine,
And byproduct-lycium ruthenicum polysaccharide can also be obtained.Gradient elution is carried out in macroporous absorbent resin later, the gradient of mobile phase is
Ethanol content is continuously increased, and final procyanidine flows into the eluate of 15~20% ethanol waters, by drying, that is, obtains
The procyanidine of high-purity.
After testing, the purity of present invention acquisition procyanidine is 97% or more, and yield is 11.5% or more (relative to black Chinese holly
Qi raw material).
Above method can also be further improved, specific as follows to improve the comprehensive benefit of technique.
Preferably, the volume fraction of ethyl alcohol is 50-70% in the ethanol water when extraction.
The volume ratio of ethyl alcohol and water is most important for the dissolution rate of lycium ruthenicum polysaccharide and procyanidine when extraction, through experiment
It was found that when the volume fraction of ethyl alcohol is 50-70%, the two can be fully dissolved out, and can obtain higher yield.Specifically,
The volume fraction of ethyl alcohol can be 50%, 55%, 60%, 65%, 70% etc..
Preferably, when the gradient elution, the volume of mobile phase used in each gradient elution is 9~11 times of column volume；
The mobile phase of the gradient elution be followed successively by 0% ethanol water, 5% ethanol water, 10% ethanol water,
15% ethanol water, or it is followed successively by 0% ethanol water, 5% ethanol water, 10% ethanol water, 15% ethanol water
Solution, 20% ethanol water.
Each elution amount of gradient and the variable gradient of ethyl alcohol have a major impact separative efficiency and separating degree.Above two
In kind of gradient, the high income for the procyanidine that the gradient of the latter obtains.
In addition, in order to recycle resin, after collecting procyanidine, also needs to continue to elute, need to generally be eluted to ethyl alcohol and contain
Amount is 100%.
Preferably, when the gradient elution, the volume of mobile phase used in each gradient elution is 10~11 times of column volume.
Preferably, filter residue is also collected when the extraction, and the filter residue is subjected to following processing：
Water and complex enzyme are added into the filter residue, carries out enzyme digestion reaction；Then heat to 80-90 DEG C of extraction；Alcohol later
It is heavy to obtain lycium ruthenicum polysaccharide；
The complex enzyme is made of pectase, cellulase and hemicellulase.
Filter residue after extraction is also rich in polysaccharides, and the process by digesting and dissolving out can extract, and improves black
The utility value of matrimony vine also improves the economic benefit of extracting method of the present invention.
Due to being rich in pectin, cellulose and hemicellulose in the residue of lycium ruthenicum, corresponding enzyme reaction is needed.
Preferably, in the complex enzyme, the mass ratio of pectase, cellulase and hemicellulase is 1~3:0.5~
1.5:1, more preferable 1~2:0.5~1:1.
Preferably, the additive amount of the complex enzyme is 1 ‰~the 1% of the lycium ruthenicum.
Preferably, the method for the alcohol precipitation is：It first concentrates, the absolute ethyl alcohol of the 4-5 times of volume of the concentrated liquid is added later, be precipitated
Precipitation.
Preferably, the feed liquid mass ratio when extraction is 1:4~7.
Preferably, also the filtrate decompression is concentrated before the gradient elution, until without alcohol taste.
Preferably, the macroporous absorbent resin is D101 resins, HP-20 resins or HPD-100 resins, the equal energy of these resins
Higher yield is obtained, wherein being optimal with HPD-100 resins.
Procyanidine using the above method of the present invention extraction is in purple, and powder particle is uniform after drying.
To sum up, compared with prior art, invention achieves following technique effects：
(1) procyanidine and lycium ruthenicum polysaccharide for extracting high-purity respectively from lycium ruthenicum, realize to lycium ruthenicum
Deep exploitation and precision exploitation, avoid the food such as lycium ruthenicum jam/beverage that from cannot making full use of the nutritive value of lycium ruthenicum；
(2) it by the reaction condition of each step in optimize technique, improves the purity of procyanidine and lycium ruthenicum polysaccharide, receive
The production efficiency and operation ingredient etc. of rate and technique.
Specific implementation mode
Technical scheme of the present invention is clearly and completely described below in conjunction with specific implementation mode, but ability
Field technique personnel will be understood that following described embodiments are some of the embodiments of the present invention, instead of all the embodiments,
It is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.Based on the embodiments of the present invention, the common skill in this field
The every other embodiment that art personnel are obtained without making creative work belongs to the model that the present invention protects
It encloses.The person that is not specified actual conditions in embodiment, carries out according to conventional conditions or manufacturer's recommended conditions.Agents useful for same or instrument
Production firm person is not specified, is the conventional products that can be obtained by commercially available purchase.
Embodiment 1
The first step：Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 50% ethanol solution 500ml is added and extracts 1h, mistake in 50 DEG C
Filter residue after filter repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol tune is added into filtrate
Volume fraction of ethanol is saved to 80%, 8h is stood in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, 1h is concentrated under reduced pressure extremely in 35 DEG C of filtrate
Ethyl alcohol all volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, 20% ethanol water, the volume of mobile phase used in each gradient elution are
10 times of column volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 12.8g, it is pure
Degree is up to 98%, mode of appearance：It is uniform in purple, powder particle.
The detection method of procyanidine is：
A series of concentration are prepared by standard items of catechin, take 1mL standard solutions, 2.5mL, 1% vanillic aldehyde-is added
Methanol solution, is then added 2.5mL, 8% hydrochloric acid-methanol solution, and after mixing, absorbance is measured under 500nm, does standard song
Line replaces catechin with extracting solution, surveys absorbance, calculates procyanidin content w.
The purity of quality=final product procyanidine of the final gained lycium ruthenicum procyanidine of w/.
Third walks：Be added into obtained filter residue 5 times of water of material quality and 0.1g complex enzyme (pectase, cellulase,
Hemicellulase, mass ratio 2:1:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h is concentrated under reduced pressure into volume
The absolute ethyl alcohol of 5 times of volume of the concentrated liquid is added after half, alcohol precipitation obtains lycium ruthenicum polysaccharide, merges with above-mentioned part lycium ruthenicum polysaccharide,
Total weight accounts for about the 4.1% of material quality (i.e. lycium ruthenicum).
Embodiment 2
Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 70% ethanol solution 400ml is added and extracts 1h in 60 DEG C, is filtered after filtering
Slag repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol is added into filtrate and adjusts ethyl alcohol body
Fraction stands 12h to 90%, in 10 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, it is complete to ethyl alcohol that 1h is concentrated under reduced pressure in 40 DEG C of filtrate
Portion volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, 20% ethanol water, the volume of mobile phase used in each gradient elution are
9 times of column volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 13.0g, it is pure
Degree is up to 98.5%, mode of appearance：It is uniform in purple, powder particle.Detection method is the same as embodiment 1.
Complex enzyme (pectase, cellulase, hemicellulose of 7 times of water of material quality and 0.1g are added into obtained filter residue
Plain enzyme, mass ratio 2:1:1) after 35 DEG C of enzymolysis 2h, it is warming up to 85-90 DEG C, stirring extraction 1h, after being concentrated under reduced pressure into the half of volume
The absolute ethyl alcohol of 4 times of volume of the concentrated liquid is added, alcohol precipitation obtains lycium ruthenicum polysaccharide, merges with above-mentioned part lycium ruthenicum polysaccharide, total weight
Account for about the 4.5% of material quality (i.e. lycium ruthenicum).
Embodiment 3
Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 60% ethanol solution 500ml is added and extracts 1h in 50 DEG C, it is filtered
Filter residue repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol is added into filtrate and adjusts ethyl alcohol
Volume fraction stands 8h to 80%, in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, it is complete to ethyl alcohol that 1h is concentrated under reduced pressure in 35 DEG C of filtrate
Portion volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, 20% ethanol water, the volume of mobile phase used in each gradient elution are
10 times of column volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 12.5g, it is pure
Degree is up to 98.2%, mode of appearance：It is uniform in purple, powder particle.Detection method is the same as embodiment 1.
Complex enzyme (pectase, cellulase, hemicellulose of 5 times of water of material quality and 0.1g are added into obtained filter residue
Plain enzyme, mass ratio 2:1:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h, after being concentrated under reduced pressure into the half of volume
The absolute ethyl alcohol of 5 times of volume of the concentrated liquid is added, alcohol precipitation obtains lycium ruthenicum polysaccharide, merges with above-mentioned part lycium ruthenicum polysaccharide, total weight
Account for about the 4.2% of material quality (i.e. lycium ruthenicum).
Embodiment 4
Difference lies in the condition of gradient elution is different from embodiment 1：
The first step：Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 50% ethanol solution 500ml is added and extracts 1h, mistake in 50 DEG C
Filter residue after filter repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol tune is added into filtrate
Volume fraction of ethanol is saved to 80%, 8h is stood in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, 1h is concentrated under reduced pressure extremely in 35 DEG C of filtrate
Ethyl alcohol all volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, the volume of mobile phase used in each gradient elution are 11 times of column volume；It receives
Collect 15% ethanol solution eluate, spray drying is to get lycium ruthenicum procyanidine 12g, and purity is up to 98.4%, mode of appearance：It is in
Purple, powder particle are uniform.Detection method is the same as embodiment 1.
Third walks：Be added into obtained filter residue 5 times of water of material quality and 0.1g complex enzyme (pectase, cellulase,
Hemicellulase, mass ratio 2:1:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h is concentrated under reduced pressure into volume
The absolute ethyl alcohol of 5 times of volume of the concentrated liquid is added after half, alcohol precipitation obtains lycium ruthenicum polysaccharide, merges with above-mentioned part lycium ruthenicum polysaccharide,
Total weight accounts for about the 4.1% of material quality (i.e. lycium ruthenicum).
Embodiment 5
Difference lies in the composition of complex enzyme is different from embodiment 1：
The first step：Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 50% ethanol solution 500ml is added and extracts 1h, mistake in 50 DEG C
Filter residue after filter repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol tune is added into filtrate
Volume fraction of ethanol is saved to 80%, 8h is stood in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, 1h is concentrated under reduced pressure extremely in 35 DEG C of filtrate
Ethyl alcohol all volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, 20% ethanol water, the volume of mobile phase used in each gradient elution are
10 times of column volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 12.8g, it is pure
Degree is up to 98%, mode of appearance：It is uniform in purple, powder particle.With embodiment 1.
Third walks：Be added into obtained filter residue 5 times of water of material quality and 0.1g complex enzyme (pectase, cellulase,
Hemicellulase, mass ratio 3:0.5:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h is concentrated under reduced pressure into volume
Half after the absolute ethyl alcohols of 5 times of volume of the concentrated liquid is added, alcohol precipitation obtains lycium ruthenicum polysaccharide, is closed with above-mentioned part lycium ruthenicum polysaccharide
And total weight accounts for about the 3.5% of material quality (i.e. lycium ruthenicum).
Embodiment 6
Difference lies in the composition of complex enzyme is different from embodiment 1：
The first step：Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 50% ethanol solution 500ml is added and extracts 1h, mistake in 50 DEG C
Filter residue after filter repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol tune is added into filtrate
Volume fraction of ethanol is saved to 80%, 8h is stood in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, 1h is concentrated under reduced pressure extremely in 35 DEG C of filtrate
Ethyl alcohol all volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses HPD-100 resins, water-soluble by 0% ethanol water, 5% ethanol water, 10% ethyl alcohol
The stagewise gradient elution of liquid, 15% ethanol water, 20% ethanol water, the volume of mobile phase used in each gradient elution are
10 times of column volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 12.8g, it is pure
It spends up to 98%.With embodiment 1.
Third walks：Be added into obtained filter residue 5 times of water of material quality and 0.1g complex enzyme (pectase, cellulase,
Hemicellulase, mass ratio 1:1.5:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h is concentrated under reduced pressure into volume
Half after the absolute ethyl alcohols of 5 times of volume of the concentrated liquid is added, alcohol precipitation obtains lycium ruthenicum polysaccharide, is closed with above-mentioned part lycium ruthenicum polysaccharide
And total weight accounts for about the 3.7% of material quality (i.e. lycium ruthenicum).
Embodiment 7
That difference lies in macroporous absorbent resin types is different from embodiment 1：
Difference lies in the composition of complex enzyme is different from embodiment 1：
The first step：Lycium ruthenicum 100g is taken, No.1 sieve is crushed, 50% ethanol solution 500ml is added and extracts 1h, mistake in 50 DEG C
Filter residue after filter repeats above step 2 times, each 1h, and it is spare to collect filter residue for merging filtrate.Absolute ethyl alcohol tune is added into filtrate
Volume fraction of ethanol is saved to 80%, 8h is stood in 4 DEG C, part lycium ruthenicum polysaccharide is obtained by filtration, 1h is concentrated under reduced pressure extremely in 35 DEG C of filtrate
Ethyl alcohol all volatilizees, and the filtrate after concentration is diluted with water to solution clear.
Second step：Filtrate crosses D101 resins, by 0% ethanol water, 5% ethanol water, 10% ethanol water,
The volume of the stagewise gradient elution of 15% ethanol water, 20% ethanol water, mobile phase used in each gradient elution is column
10 times of volume；15% and 20% ethanol solution eluate is collected, is spray-dried to get lycium ruthenicum procyanidine 12.3g, purity
Up to 97.5%.With embodiment 1.
Third walks：Be added into obtained filter residue 5 times of water of material quality and 0.1g complex enzyme (pectase, cellulase,
Hemicellulase, mass ratio 2:1:1) after 50 DEG C of enzymolysis 2h, it is warming up to 80-85 DEG C, stirring extraction 2h is concentrated under reduced pressure into volume
The absolute ethyl alcohol of 5 times of volume of the concentrated liquid is added after half, alcohol precipitation obtains lycium ruthenicum polysaccharide, merges with above-mentioned part lycium ruthenicum polysaccharide,
Total weight accounts for about the 4.1% of material quality (i.e. lycium ruthenicum).
Finally it should be noted that：The above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, it will be understood by those of ordinary skill in the art that：Its according to
So can with technical scheme described in the above embodiments is modified, either to which part or all technical features into
Row equivalent replacement；And these modifications or replacements, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme.
Claims (10)
1. the extracting method of lycium ruthenicum procyanidins, which is characterized in that include the following steps：
Using ethanol water as solvent, lycium ruthenicum is extracted, collects leaching liquor；
Alcohol volume content in the leaching liquor is adjusted to 80~90%, precipitation, filtering and collecting filter liquid is precipitated；
Using macroporous absorbent resin as filler, gradient elution is carried out with the ethanol water of 0% to 15~20% gradient, merge 15~
The fraction section that 20% ethanol water elutes, is dried to obtain solid-state procyanidine.
2. extracting method according to claim 1, which is characterized in that the body of ethyl alcohol in the ethanol water when extraction
Fraction is 50-70%.
3. extracting method according to claim 1, which is characterized in that when the gradient elution, used in each gradient elution
The volume of mobile phase is 9~11 times of column volume；
The mobile phase of the gradient elution is followed successively by 0% ethanol water, 5% ethanol water, 10% ethanol water, 15%
Ethanol water, or be followed successively by 0% ethanol water, 5% ethanol water, 10% ethanol water, 15% ethanol water,
20% ethanol water.
4. extracting method according to claim 3, which is characterized in that when the gradient elution, used in each gradient elution
The volume of mobile phase is 10~11 times of column volume.
5. extracting method according to claim 1, which is characterized in that also collect filter residue when the extraction, and by the filter
Slag carries out following processing：
Water and complex enzyme are added into the filter residue, carries out enzyme digestion reaction；Then heat to 80-90 DEG C of extraction；Alcohol precipitation obtains later
To lycium ruthenicum polysaccharide；
The complex enzyme is made of pectase, cellulase and hemicellulase.
6. extracting method according to claim 5, which is characterized in that in the complex enzyme, pectase, cellulase and half
The mass ratio of cellulase is 1~3:0.5~1.5:1, preferably 1~2:0.5~1:1；
Preferably, the additive amount of the complex enzyme is 1 ‰~the 1% of the lycium ruthenicum.
7. extracting method according to claim 5, which is characterized in that the method for the alcohol precipitation is：It first concentrates, is added later
Precipitation is precipitated in the absolute ethyl alcohol of the 4-5 times of volume of the concentrated liquid.
8. extracting method according to claim 1, which is characterized in that the feed liquid mass ratio when extraction is 1:4~7.
9. extracting method according to claim 1, which is characterized in that the macroporous absorbent resin is D101 resins, HP-20
Resin or HPD-100 resins.
10. the extract in a kind of lycium ruthenicum, which is characterized in that for using claim 1-9 any one of them extracting methods
The obtained solid-state procyanidine.
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