CN108558733A - The method for extracting Canton love-pea vine abrine - Google Patents
The method for extracting Canton love-pea vine abrine Download PDFInfo
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- CN108558733A CN108558733A CN201711483358.4A CN201711483358A CN108558733A CN 108558733 A CN108558733 A CN 108558733A CN 201711483358 A CN201711483358 A CN 201711483358A CN 108558733 A CN108558733 A CN 108558733A
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- 241000718543 Ormosia krugii Species 0.000 title claims abstract description 75
- CZCIKBSVHDNIDH-NSHDSACASA-N N(alpha)-methyl-L-tryptophan Chemical compound C1=CC=C2C(C[C@H]([NH2+]C)C([O-])=O)=CNC2=C1 CZCIKBSVHDNIDH-NSHDSACASA-N 0.000 title claims abstract description 59
- CZCIKBSVHDNIDH-UHFFFAOYSA-N Nalpha-methyl-DL-tryptophan Natural products C1=CC=C2C(CC(NC)C(O)=O)=CNC2=C1 CZCIKBSVHDNIDH-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000000034 method Methods 0.000 title claims abstract description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 49
- 108091005804 Peptidases Proteins 0.000 claims abstract description 22
- 239000004365 Protease Substances 0.000 claims abstract description 22
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 238000001728 nano-filtration Methods 0.000 claims abstract description 16
- 229920001661 Chitosan Polymers 0.000 claims abstract description 15
- 239000012528 membrane Substances 0.000 claims abstract description 13
- 239000011347 resin Substances 0.000 claims abstract description 10
- 229920005989 resin Polymers 0.000 claims abstract description 10
- 102000004190 Enzymes Human genes 0.000 claims abstract description 4
- 108090000790 Enzymes Proteins 0.000 claims abstract description 4
- 239000001913 cellulose Substances 0.000 claims abstract description 3
- 229920002678 cellulose Polymers 0.000 claims abstract description 3
- 239000000706 filtrate Substances 0.000 claims description 23
- 235000019441 ethanol Nutrition 0.000 claims description 19
- 239000002253 acid Substances 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000000843 powder Substances 0.000 claims description 17
- 239000003480 eluent Substances 0.000 claims description 16
- 108010059892 Cellulase Proteins 0.000 claims description 14
- 229940106157 cellulase Drugs 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- 238000004042 decolorization Methods 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 13
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 13
- 238000010828 elution Methods 0.000 claims description 9
- 238000002425 crystallisation Methods 0.000 claims description 7
- 230000008025 crystallization Effects 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- 238000001179 sorption measurement Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 5
- 229940088598 enzyme Drugs 0.000 claims description 3
- 150000004676 glycans Chemical class 0.000 claims 1
- 239000000284 extract Substances 0.000 abstract description 21
- 239000000243 solution Substances 0.000 description 76
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 39
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 18
- 108010084185 Cellulases Proteins 0.000 description 6
- 102000005575 Cellulases Human genes 0.000 description 6
- 238000003763 carbonization Methods 0.000 description 6
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 206010023126 Jaundice Diseases 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 230000001476 alcoholic effect Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 2
- 229960001231 choline Drugs 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000287 crude extract Substances 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 230000036407 pain Effects 0.000 description 2
- 238000001953 recrystallisation Methods 0.000 description 2
- 238000001223 reverse osmosis Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 1
- 241000220436 Abrus Species 0.000 description 1
- 244000135727 Abrus pulchellus subsp cantoniensis Species 0.000 description 1
- 235000017112 Abrus pulchellus subsp cantoniensis Nutrition 0.000 description 1
- 241000143437 Aciculosporium take Species 0.000 description 1
- 206010008909 Chronic Hepatitis Diseases 0.000 description 1
- 241001465965 Holotrichia Species 0.000 description 1
- 208000004880 Polyuria Diseases 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 229930182558 Sterol Natural products 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 150000003838 adenosines Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000007516 brønsted-lowry acids Chemical class 0.000 description 1
- 150000007528 brønsted-lowry bases Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 239000003729 cation exchange resin Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 230000035619 diuresis Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 208000006454 hepatitis Diseases 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 208000004396 mastitis Diseases 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 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
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 235000021251 pulses Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 231100000004 severe toxicity Toxicity 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 150000003432 sterols Chemical class 0.000 description 1
- 235000003702 sterols Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229930182493 triterpene saponin Natural products 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
- C07D209/04—Indoles; Hydrogenated indoles
- C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
- C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
- C07D209/24—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals with an alkyl or cycloalkyl radical attached to the ring nitrogen atom
Abstract
The invention discloses a kind of methods of extraction Canton love-pea vine abrine, this method is first by Canton love-pea vine drying, crushing, then plus water cellulose this enzyme, protease, pectase are digested, it is used in acidity after adjusting pH, then it is clarified with chitosan, is then adsorbed with polar resin, then eluted with hydrochloric acid, it is dry after alcohol precipitation to be made through nanofiltration membrane.The use of this method 2kg Herba Abri extract contents is 2085 2351mg, purity is 96.1 98.5%.
Description
Technical field
The present invention relates to traditional Chinese medicine extraction processing technique fields, and in particular to a method of extraction Canton love-pea vine abrine.
Background technology
Canton love-pea vine is the drying complete stool of legume jequirity (Abrus cantoniensis), and Chinese medicine Canton love-pea vine is pulse family
The effect of Abrus plant, is used as medicine with complete stool, has removing dampness through diuresis and removing jaundice, clearing heat and detoxicating, dispersing the depressed liver-qi and alleviating pain, be clinical conventional Chinese medicine,
For jaundice, side of body rib is bad, epigastric distending pain, acute, chronic hepatitis, mastitis, is also one of China's product herbal variety.Herb
Containing abrine (Abrine, i.e. N-methyl-tryptophane), choline (choline), adenosine class, sterols, triterpene saponin, flavones
Class, amino acid, carbohydrate.
Abrine (abrine) is called abrine, N-methyl-tryptophane, crystallizes (water) for prism-shaped, decomposition point 295
DEG C ,+44 ° of optical activity (0.28g is dissolved in 10mL0.5mol/L hydrochloric acid).1g is dissolved in about 100mL methanol, is slightly soluble in water, does not dissolve in
Ether is dissolved in dilute bronsted lowry acids and bases bronsted lowry.Molecular formula C12H14N2O2, molecular weight 218.25.At present abrine is extracted about Canton love-pea vine
Method, but there are still some problems.
A kind of method for extracting abrine from Canton love-pea vine of Publication No. CN102432521A, extracts abrine
The step of be:A. take Holotrichia trichophora raw material segment, Plus acidic water soak extraction 2-3 times, extracting solution filtering that cation is added and exchanges
It is adsorbed in resin, deionized water is washed till neutrality, then is eluted with 40-90% ethanol solutions, and medicinal extract is concentrated under reduced pressure to obtain in eluent；B. on
It states medicinal extract to detach using high speed adverse current chromatogram, UV detector on-line monitoring collects target flow point, is dried under reduced pressure to obtain jequirity
Alkali.But this method abrine extraction content is relatively low, and using the chloroform of severe toxicity in separation process, and to human body god
It is dangerous and be harmful to health through harmful methanol.
A kind of method of extraction abrine of Publication No. CN102875443A, extraction step are as follows:Canton love-pea vine is former
The broken 20-80 mesh of feed powder puts into extraction kettle, is passed through liquid CO2And entrainer, in 40-55 DEG C of pressure 20-30MPa, temperature condition
Under, 30-60min is extracted, is parsed under the conditions of pressure 5-9MPa, 40-60 DEG C of temperature, obtains extract；Above-mentioned extract sour water
Dissolving, with nanofiltration membrane, filtrate is concentrated with reverse osmosis membrane again, and concentrate adjusts pH5-6 and adds ethanol solution alcohol precipitation, filters out heavy
Starch is with 70-99% methanol solutions dissolving-recrystallization 2-3 times to get abrine.This method uses CO2Extract under high pressure
It takes, manufacturing technique requirent is higher, and input cost is high.
Therefore, have not yet to see that a kind of safety and environmental protection, input be low, the efficient Canton love-pea vine abrine extracting method of extraction.
Invention content
In order to solve the above technical problems, the present invention provides a kind of methods of extraction Canton love-pea vine abrine.
The present invention is achieved by the following technical programs:
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying crushes, and adds water, sterilizes, cellulase, protease, pectin are added at a temperature of 28-35 DEG C
Enzyme is digested, and adds the adjusting of the acid solutions such as dilute hydrochloric acid or acetic acid to make pH value of solution in acidity, it is 1.0-3.5% to add mass concentration
Chitosan solution, stood after stirring evenly, filter to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 2-3 is repeated using acid solutions such as dilute hydrochloric acid or acetic acid
It is secondary, then pH4.3-6.5 is dissolved and adjusted with acid solutions such as dilute hydrochloric acid or acetic acid, by macroporous resin adsorption, hydrochloric acid solution is added
Elution elutes 1-2 times to obtain eluent, adjusts eluent pH and takes filtrate with nanofiltration membrane to neutrality, then is removed through activated carbon decolorizing
It is miscellaneous, ethanol solution is added and stirs well, filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 0.8-3.5% through vacuum freeze drying；Vacuum freeze drying
Vacuum degree be 150-300Pa.
Drying temperature is 45-60 DEG C, drying time 6-8h in the step S1, and Canton love-pea vine powder particle diameter is 40-80 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in the step S1:3-10.
The cellulase that is added in the step S1, protease, the 0.8-5.2% that pectase total amount is Canton love-pea vine weight.
The step S1 cellulases, protease, pectase weight ratio be 1:0.2-0.6:0.4-0.8.
Add acid-conditioning solution to pH4.2-6.5 in the step S1.
The 0.5-3.6% that chitosan solution volume is liquor capacity is added in the step S1.
Hydrochloric acid solution volume fraction is 10-50% in the step S2.
Nanofiltration retaining molecular weight is 240-300 in the step S2.
Ethanol solution concentration 85-100% in the step S2.
Macroreticular resin is one kind of AB-8, HPD-200A, HPD-100C in the step S2.
The beneficial effects of the present invention are:This method is had the following advantages using enzymatic isolation method extraction Canton love-pea vine abrine:
1, Canton love-pea vine is digested using enzyme, reaction condition is mild, can discharge the substance in Canton love-pea vine, improves carrying for abrine
Take rate；2, chitosan solution can decolourize to clean with clear solution, activated carbon；3, selectively molecular cut off is NF membrane
240-300 can remove effectively the ingredient of non-abrine, improve the abrine purity of extraction；4, ethyl alcohol polarity is opposite
Weak, solubility very little, easily formation precipitate abrine wherein, are conducive to the separation of abrine and other compositions.It uses
This method 2kg Herba Abri extract contents are 2085-2351mg, purity 96.1-98.5%.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiments, but claimed range is not limited to
In described.
Embodiment one
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 28 DEG C be added cellulase, protease, pectase into
Row enzymolysis adds dilute hydrochloric acid solution adjusting to make pH value of solution in acidity, adds the chitosan solution that mass concentration is 1.0%, stirring
It is stood after uniformly, filters to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 2 times is repeated using acid solutions such as dilute hydrochloric acid or acetic acid,
PH4.3 is dissolved and adjusted with acid solutions such as acetic acid again, by AB-8 macroporous resin adsorptions, hydrochloric acid solution elution is added, elutes 1 time
Eluent is obtained, eluent pH is adjusted and takes filtrate with nanofiltration membrane to neutrality, then through decolorization and impurity removal by active carbon, ethanol solution is added
It stirs well, filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 0.8% through vacuum freeze drying；Vacuum freeze drying it is true
Reciprocal of duty cycle is 150Pa.
Drying temperature is 45 DEG C, drying time 6h in step S1, and Canton love-pea vine powder particle diameter is 40 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in step S1:3.
The cellulase that is added in step S1, protease, 0.8% that pectase total amount is Canton love-pea vine weight.
Step S1 cellulases, protease, pectase weight ratio be 1:0.2:0.4.
Add acid-conditioning solution to pH4.2 in step S1.
0.5% that chitosan solution volume is liquor capacity is added in step S1.
Hydrochloric acid solution volume fraction is 10% in step S2.
Nanofiltration retaining molecular weight is 240 in step S2.
Ethanol solution concentration 85% in step S2.
Embodiment two
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 30 DEG C be added cellulase, protease, pectase into
Row enzymolysis adds dilute hydrochloric acid solution adjusting to make pH value of solution in acidity, adds the chitosan solution that mass concentration is 1.5%, stirring
It is stood after uniformly, filters to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 3 times is repeated using acid solutions such as dilute hydrochloric acid or acetic acid,
PH4.7 is dissolved and adjusted with dilute hydrochloric acid solution again, by HPD-100C macroporous resin adsorptions, hydrochloric acid solution elution, elution 2 is added
It is secondary that eluent, adjusting eluent pH to neutrality take filtrate with nanofiltration membrane, then through decolorization and impurity removal by active carbon, addition ethyl alcohol is molten
Liquid stirs well, and filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 1.3% through vacuum freeze drying；Vacuum freeze drying it is true
Reciprocal of duty cycle is 180Pa.
Drying temperature is 48 DEG C, drying time 6.5h in step S1, and Canton love-pea vine powder particle diameter is 50 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in step S1:5.
The cellulase that is added in step S1, protease, 2.1% that pectase total amount is Canton love-pea vine weight.
Step S1 cellulases, protease, pectase weight ratio be 1:0.3:0.5.
Add acid-conditioning solution to pH4.8 in step S1.
1.1% that chitosan solution volume is liquor capacity is added in step S1.
Hydrochloric acid solution volume fraction is 21% in step S2.
Nanofiltration retaining molecular weight is 245 in step S2.
Ethanol solution concentration 89% in step S2.
Embodiment three
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 31 DEG C be added cellulase, protease, pectase into
Row enzymolysis adds the adjusting of the acid solutions such as dilute hydrochloric acid or acetic acid to make pH value of solution in acidity, adds the chitosan that mass concentration is 2.2%
Solution stands after stirring evenly, filters to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 2 times is repeated using acid solutions such as dilute hydrochloric acid or acetic acid,
PH5.4 is dissolved and adjusted with acid solutions such as dilute hydrochloric acid or acetic acid again, by HPD-200A macroporous resin adsorptions, hydrochloric acid solution is added
Elution, elution 2 times eluent, adjust eluent pH and take filtrate with nanofiltration membrane to neutrality, then through decolorization and impurity removal by active carbon,
Ethanol solution is added to stir well, filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 2.3% through vacuum freeze drying；Vacuum freeze drying it is true
Reciprocal of duty cycle is 200Pa.
Drying temperature is 52 DEG C, drying time 7.2h in step S1, and Canton love-pea vine powder particle diameter is 62 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in step S1:7.3.
The cellulase that is added in step S1, protease, 3.9% that pectase total amount is Canton love-pea vine weight.
Step S1 cellulases, protease, pectase weight ratio be 1:0.5:0.7.
Add acid-conditioning solution to pH5.6 in step S1.
2.8% that chitosan solution volume is liquor capacity is added in step S1.
Hydrochloric acid solution volume fraction is 42% in step S2.
Nanofiltration retaining molecular weight is 266 in step S2.
Ethanol solution concentration 95% in step S2.
Example IV
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 35 DEG C be added cellulase, protease, pectase into
Row enzymolysis adds the adjusting of the acid solutions such as dilute hydrochloric acid to make pH value of solution in acidity, adds the chitosan solution that mass concentration is 3.5%,
It is stood after stirring evenly, filters to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 2 times is repeated using acid solutions such as dilute hydrochloric acid or acetic acid,
PH6.1 is dissolved and adjusted with acid solutions such as acetic acid again, by HPD-100C macroporous resin adsorptions, hydrochloric acid solution elution is added, washes
It is 1 time de- that eluent, adjusting eluent pH to neutrality take filtrate with nanofiltration membrane, then through decolorization and impurity removal by active carbon, addition second
Alcoholic solution stirs well, and filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 2.9% through vacuum freeze drying；Vacuum freeze drying it is true
Reciprocal of duty cycle is 240Pa.
Drying temperature is 58 DEG C, drying time 8h in step S1, and Canton love-pea vine powder particle diameter is 75 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in step S1:9.
The cellulase that is added in step S1, protease, 4.6% that pectase total amount is Canton love-pea vine weight.
Step S1 cellulases, protease, pectase weight ratio be 1:0.5:0.8.
Add acid-conditioning solution to pH5.5 in step S1.
3.2% that chitosan solution volume is liquor capacity is added in step S1.
Hydrochloric acid solution volume fraction is 45% in step S2.
Nanofiltration retaining molecular weight is 300 in step S2.
Ethanol solution concentration 100% in step S2.
Embodiment five
A method of extraction Canton love-pea vine abrine, this approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 35 DEG C be added cellulase, protease, pectase into
Row enzymolysis adds dilute hydrochloric acid solution adjusting to make pH value of solution in acidity, adds the chitosan solution that mass concentration is 3.5%, stirring
It is stood after uniformly, filters to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, and crystallization 3 times is repeated using acid solutions such as dilute hydrochloric acid or acetic acid,
PH6.5 is dissolved and adjusted with acid solutions such as acetic acid again, by HPD-200A macroporous resin adsorptions, hydrochloric acid solution elution is added, washes
It is 2 times de- that eluent, adjusting eluent pH to neutrality take filtrate with nanofiltration membrane, then through decolorization and impurity removal by active carbon, addition second
Alcoholic solution stirs well, and filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 3.5% through vacuum freeze drying；Vacuum freeze drying it is true
Reciprocal of duty cycle is 300Pa.
Drying temperature is 60 DEG C, drying time 8h in step S1, and Canton love-pea vine powder particle diameter is 80 mesh.
The mass ratio of Canton love-pea vine powder and water is 1 in step S1:10.
The cellulase that is added in step S1, protease, 5.2% that pectase total amount is Canton love-pea vine weight.
Step S1 cellulases, protease, pectase weight ratio be 1:0.6:0.4.
Add acid-conditioning solution to pH6.5 in step S1.
3.6% that chitosan solution volume is liquor capacity is added in step S1.
Hydrochloric acid solution volume fraction is 50% in step S2.
Nanofiltration retaining molecular weight is 240 in step S2.
Ethanol solution concentration 85% in step S2.
Experimental example one
A kind of method for extracting abrine from Canton love-pea vine of Publication No. CN102432521A, extracts abrine
The step of be:Canton love-pea vine segment, the aqueous hydrochloric acid solution soak at room temperature of 8 times of amount pH2 4 hours, are extracted 2 times every time, extracting solution filtering
After be added in 732 cation exchange resin columns and adsorb, deionized water is washed till neutrality, then 6BV60% ethanol solutions is taken to elute, and collects
12g crude extracts are concentrated under reduced pressure to obtain in eluent.Take chloroform, methanol, water by 5:4:2 mixing remove fully after layering and mutually fill high speed
Current chromatographic column, while opening and turning host 750rpm, it is pumped into phase and does mobile phase, after system balancing, flow velocity is adjusted to 3mL/
Min, while with phased soln crude extract is flowed, by sample introduction valve injection, target flow point is collected in UV detector monitoring, continuous to detach,
Merge flow point and is dried under reduced pressure to obtain white powder abrine.
Experimental example two
A kind of method of extraction abrine of Publication No. CN102875443A, extraction step are as follows:Canton love-pea vine powder
Broken 80 mesh, is passed through liquid CO2, pressure 27MPa, temperature 45 C are adjusted, reaches above-mentioned parameter, then be passed through 80% methanol solution, is extracted
50min is taken, extract is parsed under the conditions of pressure 5MPa, temperature 60 C.The gained extract aqueous sulfuric acid of pH2 dissolves,
With the hollow cellulose film nanofiltration of molecular cut off 500, filtrate is concentrated with reverse osmosis membrane again, and concentrate adjusts pH5 and adds ethyl alcohol molten
Liquid alcohol precipitation, filters out to obtain sediment 90% methanol solution dissolving-recrystallization 2 times, dry abrine.
Canton love-pea vine 14kg is taken, is divided into 7 parts, every part of 2kg, presses embodiment one, embodiment two, embodiment three, reality respectively
The method extraction abrine of example four, embodiment five, experimental example one, experimental example two is applied, and phase in extract is measured using HPLC
Think the content of sub- alkali, the results are shown in Table 1.
1 Canton love-pea vine abrine of table extracts result
| Project | Extract weight/mg | Abrine content/% in extract |
| Embodiment one | 2140 | 98.5 |
| Embodiment two | 2351 | 96.1 |
| Embodiment three | 2085 | 97.3 |
| Example IV | 2245 | 97.8 |
| Embodiment five | 2336 | 98.2 |
| Experimental example one | 1100 | 96.5 |
| Experimental example two | 1850 | 97.2 |
As can be known from the above table, 2kg Canton love-pea vines, extract weight 2085- are extracted at different conditions using this method
2351mg, abrine content is 96.1-98.5% in extract, is substantially above the extract weight of experimental example one
1100mg, abrine content is 96.5% in extract, the extract weight 1850mg of experimental example two.Therefore, using we
Compared with the prior art method, which extracts the abrine in Canton love-pea vine, has significant effect, there is larger application value.
Claims (10)
1. a kind of method of extraction Canton love-pea vine abrine, it is characterised in that:This approach includes the following steps:
S1:Canton love-pea vine drying, crush, add water, sterilize, at a temperature of 28-35 DEG C be added cellulase, protease, pectase into
Row enzymolysis, acid adding adjusting make pH value of solution in acidity, add the chitosan solution that mass concentration is 1.0-3.5%, stir evenly
After stand, filter to take filtrate；
S2:Filtrate is concentrated and dried through decolorization and impurity removal by active carbon, repeats crystallization 2-3 times using acid solution, then simultaneously with acid solution dissolving
PH4.3-6.5 is adjusted, by macroporous resin adsorption, hydrochloric acid solution elution is added, elutes 1-2 times to obtain eluent, adjusts eluent
PH takes filtrate to neutrality with nanofiltration membrane, then through decolorization and impurity removal by active carbon, ethanol solution is added and stirs well, filters to take precipitation；
S3:Precipitation obtains Canton love-pea vine abrine, moisture content 0.8-3.5% through vacuum freeze drying.
2. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Temperature is dried in the step S1
Degree is 45-60 DEG C, drying time 6-8h, and Canton love-pea vine powder particle diameter is 40-80 mesh.
3. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Canton love-pea vine in the step S1
The mass ratio of powder and water is 1:3-10.
4. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:It is added in the step S1
Cellulase, protease, the 0.8-5.2% that pectase total amount is Canton love-pea vine weight.
5. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Cellulose in the step S1
Enzyme, protease, pectase weight ratio be 1:0.2-0.6:0.4-0.8.
6. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Acid adding tune in the step S1
Solution is saved to pH4.2-6.5.
7. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Shell is added in the step S1
Glycan liquor capacity is the 0.5-3.6% of liquor capacity.
8. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Hydrochloric acid is molten in the step S2
Liquid fraction is 10-50%.
9. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:NF membrane in the step S2
Molecular cut off is 240-300.
10. the method for extracting Canton love-pea vine abrine according to claim 1, it is characterised in that:Ethyl alcohol in the step S2
Solution concentration 85-100%.
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Citations (3)
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| CA2020772A1 (en) * | 1990-01-11 | 1991-07-12 | A. Douglas Kinghorn | Natural intense sweeteners |
| CN102432521A (en) * | 2011-12-20 | 2012-05-02 | 苏州宝泽堂医药科技有限公司 | Method for extracting abrine from Abrus cantoniensis |
| CN102875443A (en) * | 2012-10-11 | 2013-01-16 | 南京泽朗医药科技有限公司 | Method for extracting abrine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2020772A1 (en) * | 1990-01-11 | 1991-07-12 | A. Douglas Kinghorn | Natural intense sweeteners |
| CN102432521A (en) * | 2011-12-20 | 2012-05-02 | 苏州宝泽堂医药科技有限公司 | Method for extracting abrine from Abrus cantoniensis |
| CN102875443A (en) * | 2012-10-11 | 2013-01-16 | 南京泽朗医药科技有限公司 | Method for extracting abrine |
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