CN104672246B - Method for extracting lycorine from Lycoris plants - Google Patents

Method for extracting lycorine from Lycoris plants Download PDF

Info

Publication number
CN104672246B
CN104672246B CN201510067699.8A CN201510067699A CN104672246B CN 104672246 B CN104672246 B CN 104672246B CN 201510067699 A CN201510067699 A CN 201510067699A CN 104672246 B CN104672246 B CN 104672246B
Authority
CN
China
Prior art keywords
lycoris
lycorine
enzyme
dried object
silica gel
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201510067699.8A
Other languages
Chinese (zh)
Other versions
CN104672246A (en
Inventor
田春莲
王鹏
覃基信
刘小攀
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jishou University
Original Assignee
Jishou University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Jishou University filed Critical Jishou University
Priority to CN201510067699.8A priority Critical patent/CN104672246B/en
Publication of CN104672246A publication Critical patent/CN104672246A/en
Application granted granted Critical
Publication of CN104672246B publication Critical patent/CN104672246B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D491/00Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00
    • C07D491/12Heterocyclic compounds containing in the condensed ring system both one or more rings having oxygen atoms as the only ring hetero atoms and one or more rings having nitrogen atoms as the only ring hetero atoms, not provided for by groups C07D451/00 - C07D459/00, C07D463/00, C07D477/00 or C07D489/00 in which the condensed system contains three hetero rings
    • C07D491/16Peri-condensed systems

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)

Abstract

The invention relates to a method for extracting lycorine from Lycoris plants, which comprises the following steps: 1. extraction: weighing Lycoris plant powder which is subjected to drying, pulverization and screening, adding water with the pH value of 1.5-7.5 according to the material-liquid ratio (g/mL) of 1:(5-25), adding an enzyme which accounts for 1-5 wt% of the Lycoris plant powder, carrying out enzymolysis at 40-80 DEG C for 0.5-2.5 hours, centrifuging for 20 minutes, filtering, and taking the supernate to obtain a lycorine extracting solution; 2. purification: (1) carrying out solvent extraction; (2) adsorbing with a cation exchange resin; (3) carrying out C18 reversed-phase silica gel column chromatography; (4) carrying out normal-phase silica gel column chromatography; and (5) recrystallization: dissolving the dried substance III obtained in the step (4) in ethanol, recrystallizing to obtain a lycorine crude product, filtering, and carrying out vacuum drying at 50-60 DEG C to obtain the lycorine. The method is simple to operate, and has the advantages of low production cost, no environment pollution, short reaction time and higher extraction yield (30.46% higher than other methods). The purification technique has the advantages of environment friendliness and high purity (up to 99.3%).

Description

A kind of method extracting lycorine from lycoris plants
Technical field
The present invention relates to a kind of extracting method of lycorine, extract lycorine from lycoris plants particularly to a kind of Method.
Background technology
Short-tube lycoris (Lycoris radiate.Herb) is the many of Amaryllidaceae (Amaryllidaceae) Lycoris (Lycoris) Year raw herbaceous plant, is mainly distributed on Asia, China has 17 kinds, and in China Hunan, Hubei, Jiangsu, Zhejiang, Fujian etc., province all has Distribution.Lycoris plants have higher ornamental value, are described as " Chinese tulip ", and short-tube lycoris bulb is rich in starch, such as by it Eluriated with a large amount of water after grinding, edible after detoxification, taste such as glutinous rice flour,《Herbal for Relief of Famines》Described in, can be fried, water logging Food.Short-tube lycoris nature and flavor are pungent, sweet, warm, have the effect of detumescence, desinsection, and contained by it, abundant alkaloid is also used widely, especially It is lycorine, lycorine has antitumor, antiviral curative effect, but content is all relatively low.
Mainly there is the side such as solvent extraction method, ultrasonic extraction, microwave loss mechanisms, supercritical fluid extraction in prior art Method, but there is the shortcomings of environmental pollution is serious, production cost is high.
Chinese patent 2006100512151 discloses a kind of method extracting lycorine from lycoris plants, extracts mesh Mark thing is lycorine;This patent focuses on lycorine and separates, complex process, complex operation, and ethyl acetate price is higher, needs repeatedly Extraction.By contrast, this method low production cost, operation is simpler.
Content of the invention
The technical problem to be solved, the drawbacks described above overcoming prior art to exist, provide a kind of recovery rate high, Become to produce the method extracting lycorine from short-tube lycoris of low cost.
The technical solution adopted for the present invention to solve the technical problems, a kind of side extracting lycorine from lycoris plants Method, comprises the following steps:
(1) extract:
Weigh first drying, pulverize, the lycoris plants powder of process of sieving, with solid-liquid ratio 1:5-25 (preferably 1:10- 1:25, more preferably 1:10), unit ratio is g/mL, adds pH to be adjusted to the water of 1.5-7.5 (preferably 3-6, more preferably 4.5), plus Enter the enzyme of lycoris plants powder quality 1%-5% (preferably 2-5%, more preferably 4%), 40-80 DEG C (preferably 35-65 DEG C, more Preferably 50 DEG C) enzymolysis 0.5-2.5h (preferably 1-2h, more preferably 1.5h), it is centrifuged 20min, filter, take supernatant, obtain final product lycorine Extract;
(2) purify
1. solvent extraction:The short-tube lycoris alkali extracting solution NaOH that step (1) is extracted adjusts pH to 10, and by volume 1:1 adds Enter extractant chloroform, shake up, stand overnight, take off a layer chloroform phase, HCl adjusts pH to 2, suction filtration, obtain lycorine extraction dense Contracting liquid;
2. cationic exchange resin adsorption:By step, 1. middle extraction concentrate adjusts pH to 1~6 (preferably pH is 2) through HCl With D-001 type cationic ion-exchange resin, with loading speed 1-3BV/h (preferably 3BV/h) loading to saturation, with containing 0.5- 40%-80% (preferably 70%) ethanol solution of 2.5mol/L (preferably 1.5mol/L) ammoniacal liquor is carried out with the elution rate of 3BV/h Wash-out, is dried, obtains dried object I;
③C18Reversed-phase silica gel column chromatography:C18Filler pre-treatment, by 20 times of quality in the C of step 2. middle dried object I18Filler It is loaded in chromatographic column, then with mobile phase (mobile phase:V (acetonitrile) V (phosphate) is 16 84) chromatography that separates out of dissolving layer Thing, loading, eluted by several times using methanol-water solution, collect eluent, concentrate, vacuum freeze drying, obtain dried object II;
4. normal-phase silica gel column chromatography:With pretreated 20 times of quality in the column chromatography silicon of step 3. gained dried object II With column diameter-pillar height wet method dress post, the ratio of described column diameter-pillar height is 1 to glue (200-300 mesh):10~30 (preferably 1:10), 3. gained dried object II and silica gel mix step, add eluant, eluent dissolving, described eluant, eluent is petroleum ether, ethyl acetate, chloroform, Two kinds of solvent mixing in acetone, methyl alcohol;Dry method loading after evaporation solvent, wash-out, collect eluent, concentrate, vacuum refrigeration is done Dry, obtain dried object III;
5. recrystallize:By step, 4. gained dried object III dissolves through ethanol, and recrystallization obtains lycorine crude product, filters, 50~60 DEG C of lycorines being vacuum dried.
Further, described step 4. in, eluant, eluent is petroleum ether and ethyl acetate, the body of described ethyl acetate and petroleum ether Long-pending ratio is 8.4:1.6.
Further, described enzyme is the mixed enzyme of cellulase and hemicellulase, the mixed enzyme of cellulase and pectase, Hemicellulase and the mixed enzyme of pectase, one of mixed enzyme of cellulase, hemicellulase and pectase.
Further, described enzyme is the mixed enzyme of cellulase and pectase, the mass ratio of described cellulase and pectase For 1:1.
Further, described lycoris plants are Lycoris aurea, Lycoris radiata, rose short-tube lycoris, straw short-tube lycoris or Lycoris (preferably Lycoris aurea)
Further, described lycoris plants powder is bulb or pollen end.
Compared with prior art, the present invention is simple to operate, low production cost, and the Extraction solvent because adopting is water, by feed liquid Ratio 1:10 calculating, if producing 1kg lycorine, more molten as extracting than methyl alcohol or absolute ethyl alcohol (industrial 7.5 yuan/kilogram) are used Agent, production cost just reduces by 42811 yuan;Environmentally safe, extraction yield is higher, extracts yield and improves 30.46%;Reaction Time is short, and compared with being extracted using ultrasonic assistant, the time shortens 1.5h, and compared with prior art leach extraction method, the time shortens 2.5h;The present invention only increases enzymolysis process on traditional extraction process by water, has certain using value, is easy for industrial metaplasia Produce;Purifying process environmental protection, and purity is high, up to 99.3%.
Brief description
Fig. 1 is the impact distribution map to lycorine yield for the pH value of the present invention;
Fig. 2 is the impact distribution map to lycorine yield for the enzyme dosage of the present invention;
Fig. 3 is the impact distribution map to lycorine yield for the enzymolysis time of the present invention;
Fig. 4 is the impact distribution map to lycorine yield for the hydrolysis temperature of the present invention;
Fig. 5 is the impact distribution map to lycorine yield for the solid-liquid ratio of the present invention.
Specific embodiment
Referring to the drawings and embodiment the present invention will be further described.
The present embodiment comprises the following steps:(1) extract:Weigh first drying, pulverize, the lycoris plants of process of sieving Powder 2.000g, with solid-liquid ratio 1:5-25, unit ratio is g/mL, is separately added into the water that pH is adjusted to 1.5-7.5, adds short-tube lycoris The enzyme of platymiscium powder quality 1%-5%, digests 0.5-2.5h at 40-80 DEG C, is centrifuged 20min, filters, takes supernatant, obtain final product Short-tube lycoris alkali extracting solution;
(2) purify
1. solvent extraction:The short-tube lycoris alkali extracting solution NaOH that step (1) is extracted adjusts pH to 10, and by volume 1:1 adds Enter extractant chloroform, shake up, stand overnight, take off a layer chloroform phase, HCl adjusts pH to 2, suction filtration, obtain lycorine extraction dense Contracting liquid;
2. cationic exchange resin adsorption:By step 1. middle extraction concentrate through HCl adjust pH to 2, with D-001 type sun from Sub-exchange resin, with loading speed 3BV/h loading to saturation, with 70% ethanol solution containing 1.5mol/L ammoniacal liquor with 3BV/h's Elution rate is eluted, and is dried, obtains dried object I;
③C18Reversed-phase silica gel column chromatography:C18Filler pre-treatment, by 20 times of quality in the C of step 2. middle dried object I18Filler It is loaded in chromatographic column, then with mobile phase (mobile phase:V (acetonitrile) V (phosphate) is 16 84) chromatography that separates out of dissolving layer Thing, loading, eluted by several times using methanol-water solution, collect eluent, concentrate, vacuum freeze drying, obtain dried object II;
4. normal-phase silica gel column chromatography:With pretreated 20 times of quality in the column chromatography silicon of step 3. gained dried object II With column diameter-pillar height wet method dress post, the ratio of described column diameter-pillar height is 1 to glue (200-300 mesh):10,3. gained is dried step Thing II is mixed with silica gel, adds eluant, eluent dissolving, and described eluant, eluent is petroleum ether, in ethyl acetate, chloroform, acetone, methyl alcohol Two kinds of solvent mixing;Dry method loading after evaporation solvent, wash-out, collect eluent, concentrate, vacuum freeze drying, obtain dried object III;
5. recrystallize:By step, 4. gained dried object III dissolves through ethanol, and recrystallization obtains lycorine crude product, filters, 50~60 DEG C be vacuum dried purity be 99.3% lycorine.
Described step 4. in, eluant, eluent is petroleum ether and ethyl acetate, and described ethyl acetate with the volume ratio of petroleum ether is 8.4:1.6.
Enzyme is the mixed enzyme of cellulase and hemicellulase, the mixed enzyme of cellulase and pectase, hemicellulase With the mixed enzyme of pectase, one of mixed enzyme of cellulase, hemicellulase and pectase.
Lycoris plants are Lycoris aurea, Lycoris radiata, rose short-tube lycoris, straw short-tube lycoris or Lycoris.
Lycoris plants powder is bulb or pollen end.
(1) screening of enzyme class
Weigh 2.000g short-tube lycoris bulb powder, with solid-liquid ratio 1:10(g:ML) it is separately added into the water that pH is adjusted to 4.5, respectively The cellulase of addition material quality 3%, hemicellulase, the mixed enzyme of pectase, cellulase and hemicellulase, fiber The mixed enzyme of mixed enzyme, hemicellulase and pectase of plain enzyme and pectase, cellulase and hemicellulase and pectase Mixed enzyme, 50 DEG C digest 2.0h, be centrifuged 20min, filter, take supernatant.Result of the test is shown in Table 1, using cellulase with The yield highest of lycorine during the mixed enzyme of pectase, and cellulase is 1 with the mass ratio of pectase:1.
Lycorine under the different enzyme effect of table 1 extracts result
Enzyme class Lycorine yield (%)
Cellulase 0.1474
Hemicellulase 0.1447
Pectase 0.1480
Cellulase and hemicellulase complex enzyme 0.1530
Cellulase and pectase complex enzyme 0.1575
Hemicellulase and pectase complex enzyme 0.1500
Cellulase and hemicellulase and pectase complex enzyme 0.1521
It is not added with enzyme 0.0902
(2) impact of pH
With reference to Fig. 1, weigh 2.000g short-tube lycoris bulb powder, be separately added into pH be 1.5,3.0,4.5,5.0,6.0,7.5 Water 20mL, adds cellulase and the pectase mixed enzyme of short-tube lycoris bulb powder quality 3%, the quality of cellulase and pectase Than for 1:Digest 2.0h under the conditions of 150 DEG C, be centrifuged 20min, filter, take supernatant.Investigate the impact to lycorine yield for the pH.Figure 1 shows, the yield highest of galanthamine and lycorine when Extractant pH is 4.5, this is because cellulase and pectase Optimal use pH is 4.5 about, when off-target uses pH, the inactivation of enzyme or part can be caused to inactivate, thus affecting to extract Yield, therefore selects pH to be tested for 4.5.
(3) impact of enzyme dosage
With reference to Fig. 2, weigh 2.000g short-tube lycoris bulb powder, the water 20mL adding pH to be 4.5, it is separately added into short-tube lycoris bulb powder The cellulase of last quality 0,1%, 2%, 3%, 4%, 5% and pectase mixed enzyme, digest 2.0h, centrifugation under the conditions of 50 DEG C 20min, filters, takes supernatant.When result enzyme dosage is excessive, concentration of substrate can not reach saturation to enzyme, leads to the effect of enzyme to be subject to Caused by suppression, therefore after enzyme dosage is more than 3%, lycorine yield has declined on the contrary with the increase of enzyme dosage.
(4) enzymolysis time
With reference to Fig. 3, weigh 2.000g short-tube lycoris bulb powder, by solid-liquid ratio 1:10(g:ML) add the water that pH is 4.5, add The cellulase of short-tube lycoris bulb powder quality 3% and pectase mixed enzyme, cellulase is 1 with the mass ratio of pectase:1;50 Digest 0.5 under the conditions of DEG C respectively, 1.0,1.5,2.0,2.5h, be centrifuged 20min, filter, take supernatant.Result in extraction time is In 0.5-1.5h, the yield of lycorine increases in time and raises.Reaction time is too short, and enzymolysis is insufficient, and works as enzyme concentration and reach During certain value, the prolongation of time of enzymatic reacting can not dramatically increase extraction effect, or even begins to decline.
(5) impact of hydrolysis temperature
With reference to Fig. 4, weigh 2.000g short-tube lycoris bulb powder, add the water 20mL that pH is 4.5, add short-tube lycoris bulb powder matter The cellulase of amount 3% and pectase mixed enzyme, cellulase is 1 with the mass ratio of pectase:1;Respectively 40,50,60, 70th, digest 2.0h under the conditions of 80 DEG C respectively, be centrifuged 20min, filter, take supernatant.Result lycorine yield is with extraction temperature Rising and increase, be gradually lowered after 50 DEG C.Too high or too low for temperature all it is unfavorable for the decomposition to cell membrane for the enzyme, thus can not be Limits play the effect of enzyme.
(6) impact of solid-liquid ratio
With reference to Fig. 5, weigh 2.000g short-tube lycoris bulb powder, press solid-liquid ratio 1 respectively:5、1:10、1:15、1:20、1:25 add Enter the water that pH is 4.5, add cellulase and pectase mixed enzyme, cellulase and the pectin of short-tube lycoris bulb powder quality 3% The mass ratio of enzyme is 1:1;Digest 2.0h at 50 DEG C, be centrifuged 20min, filter, take supernatant.Result lycorine yield is with feed liquid Rise than increasing, when solid-liquid ratio is 1:When 10, lycorine yield highest.
Orthogonal test
With the yield of lycorine as index, orthogonal test, and intuitively analyzed and be shown in Table 2 and table 3 with the results of analysis of variance.
Table 2 Orthogonal Experiment and Design and result
Table 3 variance analysis
Note:F0.10(2,2)=9.00;F0.05(2,2)=19.00;F0.01(2,2)=99.00
Intuitively analyzed by table 2 and understand that lycorine extracts optimised process and is combined as A2B3C3D2, i.e. 50 DEG C of hydrolysis temperature, enzyme The aqueous solution that solution time 2.0h, enzyme concentration 4%, extractant are 4.5 for pH, impact lycorine yield each factor primary and secondary order be Hydrolysis temperature > enzyme dosage > enzymolysis time > digests pH.By table 3 variance analysis, the impact to lycorine yield for the hydrolysis temperature shows Write (P < 0.05).
Repeatedly extracted for raw material with Lycoris aurea bulb powder under this Optimal technique process, detected during to the 3rd time Do not go out short-tube lycoris alkaloid substance, lycorine yield is 0.1750%.
HPLC method detects lycorine:Chromatographic column is Kromasil 100-5C18Reversed-phase column (250mm × 4.6mm, 5 μm);Stream Fast 1.0mL/min;Sampling volume is 20 μ L;Column temperature is 35 DEG C.Mobile phase is acetonitrile phosphate buffer 16 84 (V:V), its Middle phosphate buffer is dissolved in 100mL water for 2.72g potassium dihydrogen phosphate and adds 1.4mL triethylamine to be dissolved to 1L;Detection wavelength For 290nm.The equation of linear regression of lycorine is y=16007x+10676, and linear regression coeffficient r=0.9999, in 0.005- In 0.500mg/mL concentration range, linear relationship is good.

Claims (8)

1. a kind of method of lycorine of extracting from lycoris plants is it is characterised in that comprise the following steps:(1) extract:First Weigh drying, pulverize, the lycoris plants powder of process of sieving, with solid-liquid ratio 1:5-25, unit ratio is g/mL, adds pH It is adjusted to the water of 1.5-7.5, adds the enzyme of lycoris plants powder quality 1%-5%, digest 0.5-2.5h at 40-80 DEG C, from Heart 20min, filters, takes supernatant, obtain final product short-tube lycoris alkali extracting solution;
(2) purify
1. solvent extraction:The short-tube lycoris alkali extracting solution NaOH that step (1) is extracted adjusts pH to 10, and by volume 1:1 adds extraction Take agent chloroform, shake up, stand overnight, take off a layer chloroform phase, HCl adjusts pH to 2, suction filtration, obtain lycorine extraction concentrate;
2. cationic exchange resin adsorption:By step, 1. middle extraction concentrate adjusts pH to 1~6 D-001 type cation through HCl Exchanger resin, with loading speed 1-3BV/h loading to saturation, with the 40%-80% ethanol solution containing 0.5-2.5mol/L ammoniacal liquor Eluted with the elution rate of 3BV/h, be dried, obtain dried object I;
③C18Reversed-phase silica gel column chromatography:C18Filler pre-treatment, by 20 times of quality in the C of step 2. middle dried object I18Filler is loaded on In chromatographic column, the chromatography thing that then separated out with mobile phase dissolving layer, loading, eluted by several times using methanol-water solution, collection is washed De- liquid, concentrates, vacuum freeze drying, obtains dried object II;
4. normal-phase silica gel column chromatography:With pretreated 20 times of quality in step 3. gained dried object II column chromatography silica gel with Column diameter-pillar height wet method dress post, the ratio of described column diameter-pillar height is 1:10~30, step 3. gained dried object II and silica gel Mix, add eluant, eluent dissolving, described eluant, eluent is petroleum ether, ethyl acetate, chloroform, acetone, two kinds of solvents in methyl alcohol mix Close;Dry method loading after evaporation solvent, wash-out, collect eluent, concentrate, vacuum freeze drying, obtain dried object III;
5. recrystallize:By step, 4. gained dried object III dissolves through ethanol, and recrystallization obtains lycorine crude product, filters, 50~ 60 DEG C are vacuum dried to obtain lycorine;
Described enzyme is the mixed enzyme of cellulase and hemicellulase, the mixed enzyme of cellulase and pectase, hemicellulase With the mixed enzyme of pectase, one of mixed enzyme of cellulase, hemicellulase and pectase.
2. the method for lycorine of extracting from lycoris plants according to claim 1 is it is characterised in that described step (1) in, weigh first drying, pulverize, the lycoris plants powder of process of sieving, with solid-liquid ratio 1:10-25, unit ratio is G/mL, adds pH to be adjusted to the water of 3-6, adds the enzyme of lycoris plants powder quality 2-5%, digest 1-2h at 50-65 DEG C, from Heart 20min, filters, takes supernatant, obtain final product short-tube lycoris alkali extracting solution.
3. the method extracting lycorine from lycoris plants according to claim 2 is it is characterised in that walk below including Suddenly:(1) extract:Weigh first drying, pulverize, the lycoris plants powder of process of sieving, with solid-liquid ratio 1:10, unit ratio For g/mL, add pH to be adjusted to 4.5 water, add the enzyme of lycoris plants powder quality 4%, digest 1.5h, centrifugation at 50 DEG C 20min, filters, takes supernatant, obtain final product short-tube lycoris alkali extracting solution;
(2) purify:
1. solvent extraction:The short-tube lycoris alkali extracting solution NaOH that step (1) is extracted adjusts pH to 10, and by volume 1:1 adds extraction Take agent chloroform, shake up, stand overnight, take off a layer chloroform phase, HCl adjusts pH to 2, suction filtration, obtain lycorine extraction concentrate;
2. cationic exchange resin adsorption:By step, 1. middle extraction concentrate adjusts pH to 2 through HCl, is handed over D-001 type cation Change resin, with loading speed 3BV/h loading to saturation, with 70% ethanol solution containing 1.5mol/L ammoniacal liquor with the wash-out of 3BV/h Speed is eluted, and is dried, obtains dried object I;
③C18Reversed-phase silica gel column chromatography:C18Filler pre-treatment, by 20 times of quality in the C of step 2. middle dried object I18Filler is loaded on In chromatographic column, the chromatography thing that then separated out with mobile phase dissolving layer, loading, eluted by several times using methanol-water solution, collection is washed De- liquid, concentrates, vacuum freeze drying, obtains dried object II;
4. normal-phase silica gel column chromatography:With pretreated 20 times of quality in step 3. gained dried object II column chromatography silica gel with Column diameter-pillar height wet method dress post, the ratio of described column diameter-pillar height is 1:10,3. gained dried object II and silica gel mix step, Add eluant, eluent dissolving, described eluant, eluent is petroleum ether, ethyl acetate, chloroform, acetone, two kinds of solvents mixing in methyl alcohol;Steam Send out dry method loading after solvent, wash-out, collect eluent, concentrate, vacuum freeze drying, obtain dried object III;
5. recrystallize:By step, 4. gained dried object III dissolves through ethanol, and recrystallization obtains lycorine crude product, filters, 50~ 60 DEG C are vacuum dried to obtain lycorine.
4. the method for lycorine of extracting from lycoris plants according to claim 3 is it is characterised in that described cellulose Enzyme is 1 with the mass ratio of pectase:1.
5. according to claim 1 from lycoris plants extract lycorine method it is characterised in that described step 4. In, eluant, eluent is petroleum ether and ethyl acetate, and described ethyl acetate is 8.4 with the volume ratio of petroleum ether:1.6.
6. extract the method for lycorine from lycoris plants it is characterised in that institute according to any one of claim 1-3 Stating lycoris plants is Lycoris aurea, Lycoris radiata, rose short-tube lycoris, straw short-tube lycoris or Lycoris.
7. the method for lycorine of extracting from lycoris plants according to claim 6 is it is characterised in that described Lycoris Plant is Lycoris aurea.
8. the method for lycorine of extracting from lycoris plants according to claim 1 and 2 is it is characterised in that described stone Garlic platymiscium powder is bulb or pollen end.
CN201510067699.8A 2015-02-07 2015-02-07 Method for extracting lycorine from Lycoris plants Active CN104672246B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510067699.8A CN104672246B (en) 2015-02-07 2015-02-07 Method for extracting lycorine from Lycoris plants

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510067699.8A CN104672246B (en) 2015-02-07 2015-02-07 Method for extracting lycorine from Lycoris plants

Publications (2)

Publication Number Publication Date
CN104672246A CN104672246A (en) 2015-06-03
CN104672246B true CN104672246B (en) 2017-02-22

Family

ID=53307881

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510067699.8A Active CN104672246B (en) 2015-02-07 2015-02-07 Method for extracting lycorine from Lycoris plants

Country Status (1)

Country Link
CN (1) CN104672246B (en)

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4699912A (en) * 1984-07-16 1987-10-13 Behringwerke Aktiengesellschaft Use of Lycorine as an immunosuppressor
CN101157947A (en) * 2007-09-13 2008-04-09 华中科技大学 Method for extracting active alkaloid from lycoris herb
CN101250558A (en) * 2008-03-26 2008-08-27 贵州芊芊园艺新技术发展公司 Method for producing fuel ethanol by using lycoris plants
CN101602767A (en) * 2009-05-26 2009-12-16 苏州派腾生物医药科技有限公司 A kind of preparation method of lycoremine

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4699912A (en) * 1984-07-16 1987-10-13 Behringwerke Aktiengesellschaft Use of Lycorine as an immunosuppressor
CN101157947A (en) * 2007-09-13 2008-04-09 华中科技大学 Method for extracting active alkaloid from lycoris herb
CN101250558A (en) * 2008-03-26 2008-08-27 贵州芊芊园艺新技术发展公司 Method for producing fuel ethanol by using lycoris plants
CN101602767A (en) * 2009-05-26 2009-12-16 苏州派腾生物医药科技有限公司 A kind of preparation method of lycoremine

Also Published As

Publication number Publication date
CN104672246A (en) 2015-06-03

Similar Documents

Publication Publication Date Title
WO2008138243A1 (en) A preparation method of icaritin
CN104906153A (en) Technological method for efficiently extracting ginkgo flavone
CN103467551B (en) A kind of cordycepin and Cordyceps polysaccharide and preparation method thereof
CN104306428B (en) A method of the extraction purification gypenoside from gynostemma pentaphylla
CN102219824B (en) Method for producing glycyrrhizic acid through enzymolysis
CN102988440A (en) Method for extracting ginsenoside
CN101322758B (en) Method for producing spina date seed extract using complex enzyme
CN109053821B (en) Method for extracting tea polyphenol, total amino acids and flavone compounds from momordica grosvenori leaves
CN101289480B (en) Method for separating and preparing liquiritin
CN102180938A (en) Method for preparing capilliposide
CN102351863A (en) Method for extracting qingdainone from isatis tinctoria
CN103224491A (en) Method for extracting high-purity puerarin by using water as solvent
CN102935101B (en) A kind of extracting method of olive leaf polyphenol
CN105294542A (en) Preparation method of mulberry leaf extract containing 1-deoxynojirimycin
CN102432656B (en) Method for extracting and purifying cordycepin from Cordyceps militaris sporophore
CN104606288A (en) Novel method for preparing total flavonoid aglycone extract of scutellaria baicalensis georgi
CN104672246B (en) Method for extracting lycorine from Lycoris plants
CN107325139A (en) A kind of rapidly and efficiently method of extraction purification anthocyanin from indigo fruit
CN107213180B (en) Separation and extraction method of notoginseng flavone
CN104628736B (en) A kind of method extracting galantamine from lycoris plants
CN102670935B (en) Method for extracting total saponins from allium chinense
CN101618052A (en) Process for extracting total flavonoids from hippophae leaves
CN115010618A (en) Separation and purification method of aureoyl amide alcohol ester capable of reducing uric acid and application thereof
CN109553654B (en) The method of glycyrrhizin, licoflavone and licorice polysaccharide is extracted from Radix Glycyrrhizae
CN107353296B (en) A method of extracting activated protein and eurycomanone from Tongkat Ali

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
CB02 Change of applicant information

Address after: Key Laboratory of Hunan Province, Zhangjiajie City, Hunan Province, 427000 Jishou University chemical engineering of forest products

Applicant after: Jishou Univeristy

Address before: 427000 Key Laboratory of Hunan province Hunan province Xiangxi Tujia and Miao Autonomous Prefecture of Zhangjiajie city Jishou University of chemical engineering of forest products

Applicant before: Jishou Univeristy

COR Change of bibliographic data
C14 Grant of patent or utility model
GR01 Patent grant