CN107501282B - The preparation method of isoquinolone Alkaloid compound in a kind of short-tube lycoris - Google Patents
The preparation method of isoquinolone Alkaloid compound in a kind of short-tube lycoris Download PDFInfo
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Abstract
The invention belongs to the field of Chinese medicines, a kind of preparation method of isoquinolone Alkaloid compound in short-tube lycoris is disclosed.The method: (1) using ethanol solution heating and refluxing extraction short-tube lycoris coarse powder, and concentration is dissolved with water, using petroleum ether extraction, lower layer's water phase is extracted with ethyl acetate, then lower layer's water phase is used extracting n-butyl alcohol, obtains n-butanol phase；(2) n-butanol is mutually concentrated, is dried, silicagel column is crossed in methanol dissolution, is eluted with the chloroform-methanol that volume ratio is 9:1, is merged fraction more identical than analog values；Silicagel column is crossed, selects the chloroform-methanol that volume ratio is 4:1 to elute, merges the fraction more equal than analog values；Gel column is crossed, is eluted with the methanol-water that volume ratio is 1:1, merges the fraction more equal than analog values；ODS column is crossed, volume ratio is used to elute for the methanol-water of 7:3, merges the fraction more equal than analog values, drying obtains narciclasine.Narciclasine purity of the invention is up to 95%；Extracting method is simple, and yield is high.
Description
Technical field
The invention belongs to the technical fields of Chinese medicine, and in particular to one kind extracts isoquinolone Alkaloid chemical combination from short-tube lycoris
Object-narciclasine method.
Background technique
Alkaloid is a kind of nitrogenous alkalinity being present in nature (predominantly plant, but some exists in animal)
Organic compound has the property like alkali.Modern pharmacological studies have shown that alkaloid have a variety of physiological activity, such as have it is antitumor,
The various aspects pharmacological action such as anti-acetylcholinesterase (AchE), antibacterial, antiviral, anti-malarial, while the life separated from plant
Alkaloids also cause great concern in biomedicine, as alkaloid-galanthamine in short-tube lycoris be it is effective, have it is competitive and
Reversible acetylcholinesterase inhibitor, for treating light, moderate Alzheimer's disease senile dementia in clinic, and
Adverse reaction is few, has carried out active relevant research to over one hundred kind of plant alkaloid at present and has reported, short-tube lycoris be wherein study compared with
More one kind.
Short-tube lycoris is Amaryllidaceae (Amaryllidaceae) Lycoris (Lycoris Herb) herbaceos perennial.Research hair
Existing lycoris plants are rich in alkaloids chemical component, and many kinds of, various structures, pharmacological activity are extensive, have biggish
Development of resources and utility value.Its bulb is containing there are many alkaloids, such as lycorine, galanthamine, lycoramine；Lycorine tool
There is certain anticancer activity, and can anti-inflammatory, removing toxic substances, calmness and emetic；Contained galanthamine and lycoramine is good choline
Esterase inhibitor can be used for treating the diseases such as infantile paralysis and myasthenia gravis.In recent years, the alkaloid in short-tube lycoris is to cell toxicant
Journal of Sex Research has received widespread attention, but few to the separation identification research of the main noxious material of short-tube lycoris, and wherein narciclasine is exactly
The stronger substance of maryllidaceous alkaloid Poisoning reports that the research of its separation and Extraction is very few.
Narciclasine, also referred to as 7- hydroxyl isoquinolone derivatives were isolated from Narcissus Tazetta L. Var in 1967
First Alkaloid.For narciclasine as potential anticancer drug, mechanism is mainly that the flesh passed through in damage cancer cell moves egg
White skeleton organization reaches antitumaous effect, but the research report that narciclasine how is quickly and efficiently extracted from short-tube lycoris does not almost have
Have, easy to operate we have studied the method for the separation and Extraction narciclasine from short-tube lycoris more preferably to utilize plant resources, system
Make that the period is short, and extracted content purity is up to 95% or more.
Mainly there are solvent extraction method, ultrasonic extraction, microwave for plant total alkaloid extracting method in the prior art
Extraction method, the methods of supercritical fluid extraction and enzymolysis and extraction, but it is fresh individually for the extracting method of uniform monomer narciclasine
It has been reported that.
Summary of the invention
In order to make up for the deficiencies of the prior art and disadvantage, it a kind of is extracted from short-tube lycoris the primary purpose of the present invention is that providing
The method of isoquinolone Alkaloid compounds narciclasine.
The purpose of the present invention is realized by following proposal:
A method of it extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris, includes the following steps:
(1) short-tube lycoris dried, crushed, sieving processing, obtaining short-tube lycoris coarse powder；It is heated to reflux and is mentioned using ethanol water
Short-tube lycoris coarse powder is taken, extracting solution is obtained；
(2) extracting solution is concentrated under reduced pressure, obtains medicinal extract；Medicinal extract is dissolved using water, petroleum ether extraction is then used, obtains
Upper layer petroleum ether phase and lower layer water phase A；Lower layer water phase A is adopted and is extracted with ethyl acetate, ethyl acetate phase and lower layer's water phase are obtained
B；Lower layer's aqueous phase B is used into extracting n-butyl alcohol, obtains n-butanol phase and lower layer water phase C；
(3) n-butanol is mutually concentrated under reduced pressure, dries, obtains dry n-butanol phase；Using methanol by dry n-butanol
Then phased soln is mixed with 100~200 mesh silica gel mixed samples, drying obtains the n-butanol phase by mixing sample processing；
(4) 200~300 mesh silica gel are filled into column, then will be mutually used a dry method on a sample by the n-butanol for mixing sample processing, then adopt
With chloroform-methanol mixed solvent isocratic elution, the fraction of elution is evaporated, the fraction being evaporated；The volume of chloroform and methanol
Than for 9:1；
(5) fraction being evaporated is dissolved using methanol, puts silica gel plate, is unfolded in chromatography cylinder, solvent is that volume ratio is
The chloroform-methanol mixed solvent of 9:1 merges fraction more identical than analog values；Then fraction more identical than analog values is crossed into silicagel column, selected
The chloroform-methanol mixed solvent elution for being 4:1 with volume ratio, collects fraction, puts silica gel plate, is unfolded in chromatography cylinder, solvent
The chloroform-methanol mixed solvent for being 4:1 for volume ratio merges the fraction more equal than analog values, obtains the chloroform-that volume ratio is 4:1
The equal fraction of the ratio analog values of methanol mixed solvent elution；
(6) fraction more equal than analog values is crossed into gel column, is carried out with the Methanol+Water that volume ratio is 1:1 isocratic
Fraction is collected in elution, is put polyamide board, is unfolded in chromatography cylinder, and solvent is the Methanol+Water that volume ratio is 1:1,
The fraction more equal than analog values is merged, obtains that ratio analog values that the Methanol+Water that volume ratio is 1:1 elutes are equal to be evaporated
Point；
(7) the equal fraction of the ratio analog values that the Methanol+Water that volume ratio is 1:1 elutes is crossed into ODS column, using body
Product collects fraction than the Methanol+Water isocratic elution for being 7:3, puts polyamide board, is unfolded in chromatography cylinder, solvent
The Methanol+Water for being 7:3 for volume ratio merges the fraction more equal than analog values, drying, obtains isoquinolone class biology
Alkali cpd narciclasine.
It finally obtains fraction in step (7) to chromatograph the solvent of the methanol-water of multiple and different volume ratios, all than analog values phase
Deng primarily determining that the fraction that finally obtains is single substance；In order to further determine by liquid efficient on the fraction finally obtained
Phase uses volume ratio for the isocratic flushing of the methanol-water of 7:3, single peak shape occurs, the fraction finally obtained is determined as single object
Matter.
Fraction is finally obtained in step (7), Structural Identification is carried out by mass spectrum MS and NMR spectrum NMR etc., from atom
Structural analysis is determined as narciclasine.
The volume fraction of ethyl alcohol is 70%~85% in step (1) described ethanol water, the short-tube lycoris coarse powder and ethyl alcohol
The mass volume ratio of aqueous solution is 1g:10mL~1g:25mL, and the temperature being heated to reflux is 80 DEG C~100 DEG C, the extraction
Number be 2~4 times, the time extracted every time be 1~3 hour；
The condition of reduced pressure described in step (2) are as follows: pressure is 0.09~0.1MPa, and thickening temperature is 40 DEG C~60
DEG C, until no longer screwing out liquid；
The number of petroleum ether extraction described in step (2) is 3~5 times, is specifically referred to medicinal extract for petroleum ether extraction 3~5 times
It is dissolved using water, then uses petroleum ether extraction, obtain upper layer petroleum ether phase and lower layer's water phase, lower water is mutually continued using stone
Oily ether extraction, so repeatedly 3~5 times, lower layer's water phase of last time extraction is lower layer's water phase A, and upper layer petroleum ether is mutually merged,
Finally obtain petroleum ether phase and lower layer water phase A；
The dosage of petroleum ether are as follows: the volume ratio of petroleum ether and solution is (1~2): 1, solution is that medicinal extract is used water herein
Dissolve acquired solution；
The petroleum ether is mutually concentrated under reduced pressure, drying and processing, obtains short-tube lycoris petroleum ether phase；The temperature of the reduced pressure
It is 40 DEG C~50 DEG C, the temperature of the drying is 40 DEG C~50 DEG C；
The number of the extraction of ethyl acetate described in step (2) is 3~5 times, ethyl acetate extract specifically refer to for 3~5 times by
Lower layer water phase A, which is adopted, to be extracted with ethyl acetate, and upper layer ethyl acetate phase and lower layer's water phase are obtained, and lower water is mutually continued using acetic acid
Ethyl ester extraction, so repeatedly 3~5 times, lower layer's water phase of last time extraction is lower layer's aqueous phase B, and upper layer ethyl acetate is harmonious
And finally obtain ethyl acetate phase and lower layer's aqueous phase B；
The dosage of ethyl acetate are as follows: the volume ratio of ethyl acetate and lower layer's water phase A are (1~2): 1；
The ethyl acetate phase is concentrated under reduced pressure, drying and processing, obtains short-tube lycoris ethyl acetate phase；The reduced pressure
Temperature is 40 DEG C~50 DEG C, and the temperature of the drying is 40 DEG C~50 DEG C；
The number of extracting n-butyl alcohol described in step (2) is 3~5 times, is specifically referred to lower layer for extracting n-butyl alcohol 3~5 times
Aqueous phase B uses extracting n-butyl alcohol, obtains upper layer n-butanol phase and lower layer's water phase, lower water is mutually continued using extracting n-butyl alcohol,
It so repeats 3~5 times, lower layer's water phase of last time extraction is lower layer's water phase C, and upper layer n-butanol is mutually merged, is finally obtained
N-butanol phase and lower layer water phase C；
The dosage that n-butanol extracts every time are as follows: the volume ratio of n-butanol and lower layer's aqueous phase B is (1~2): 1；
The temperature of reduced pressure described in step (3) is 50 DEG C~60 DEG C, and the temperature of the drying is 40 DEG C~60 DEG C；
Dry n-butanol phase and 100~200 mesh silica gel quality ratio 1:1.5~1:3 described in step (3)；The drying
Condition be 40 DEG C~50 DEG C at drying to constant weight；
200~300 mesh silica gel described in step (4) and the mass ratio of n-butanol phase dry in step (3) be (30~
50): 1；
Dress column described in step (4) is wet method dress post, in particular to 200~300 mesh silica gel and initial liquid phase are abundant
Large pillar is packed into after mixing, bubble-free dress column is completed in silicagel column.
Described in step (4) after the n-butanol for mixing sample processing mutually uses a dry method on a sample, top end addition a small amount of 100~
200 mesh silica gel are as protective layer.
Chloroform-methanol mixed solvent isocratic elution described in step (4) refers to the chloroform-methanol punching using volume ratio 9:1
Multiple column volumes are washed, the temperature being evaporated is 40 DEG C~50 DEG C.
The principle of the present invention: the alkaloid of plant origin has antitumor, anti-acetylcholinesterase (AchE), antibacterial, resists
The various aspects pharmacological action such as virus, anti-malarial.Maryllidaceous alkaloid narciclasine especially can embody it by killing cancer cell
Pharmacological action.And it is up to by testing the short-tube lycoris isoquinolone Alkaloid compounds narciclasine purity that separation method obtains
95% or more, and it is easy to operate, fabrication cycle is short, and yield is higher.
The present invention has the following advantages and effects with respect to the prior art:
(1) method of the invention makes the purity of the narciclasine obtained in the short-tube lycoris be up to 95%；
(2) separating and extracting process of the present invention is easy to operate, and fabrication cycle is short, and yield is higher.
Detailed description of the invention
Fig. 1 is the maryllidaceous alkaloid narciclasine that embodiment 1 is prepared1H-NMR map；
Fig. 2 is the maryllidaceous alkaloid narciclasine that embodiment 1 is prepared13C-NMR map.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.In embodiment, short-tube lycoris calyx is purchased from the peaceful medicinal material market in Guangzhou, and the place of production is Zhejiang.
Embodiment 1 is extracted from short-tube lycoris and isolates alkaloid-narciclasine:
(1) short-tube lycoris is crushed into (each grinding time 10 seconds, continuous 5 times) and crosses 20 meshes afterwards, obtain short-tube lycoris coarse powder；It weighs small
It in the short-tube lycoris coarse powder 1Kg of 20 mesh, extracts in batches, each 500g is heated to reflux with the ethanol water of volume fraction 75% and is mentioned
It takes, wherein liquid-to-solid ratio 15mL:1g, refluxing extraction temperature are 80 DEG C, reflux extracting time 2h, refluxing extraction number 3 times；
It is then combined with extracting solution, (pressure 0.09MPa, thickening temperature is 50 DEG C, until no longer screwing out liquid) is concentrated under reduced pressure to cream
Shape obtains alcohol extracts；
(2) alcohol extracts are sufficiently dissolved using distilled water, obtains solution；With the petroleum ether (body of petroleum ether and solution
Product is than 1:1) extraction, 3 times are extracted until the lighter of upper layer, merges upper layer petroleum ether phase, obtain upper layer petroleum ether phase under
Layer water phase A；(40 DEG C) are mutually concentrated under reduced pressure in upper layer petroleum ether, and drying (45 DEG C) obtains petroleum ether phase extract afterwards；
(3) by lower layer water phase A ethyl acetate equal-volume extraction in step (2), extraction 3-5 times to upper layer lighter is
Only, merge upper layer ethyl acetate phase, obtain ethyl acetate phase and lower layer's aqueous phase B；After (45 DEG C) are concentrated under reduced pressure in ethyl acetate phase
Drying (45 DEG C) obtains ethyl acetate phase extract；
(4) by lower layer's aqueous phase B n-butanol equal-volume extraction in step (3), extraction 3-5 times to upper layer lighter is
Only, merge n-butanol phase, drying obtains n-butanol phase extract at 50 DEG C after reduced pressure (50 DEG C)；
(5) by the n-butanol phase extract weighing 30g in step (4), methanol is added sufficiently to dissolve, with the mesh of 60g100~200
Silica gel wet process is mixed sample and is mixed, and drying to constant weight at 50 DEG C；Weigh 200~300 mesh silica gel wet method dress post (Ф 8* of 1200g
120cm), 100~200 mesh silica gel of 60g is added as protective layer in top end；
(6) selecting volume ratio is the chloroform-methanol of 9:1, rinses 5 column volumes, receives every 1 fraction flowed up,
45 DEG C are spin-dried for, and are collected in test tube with methanol dissolution；
(7) above-mentioned fraction point silica gel plate is collected, is unfolded in chromatography cylinder, solvent is chloroform-first that volume ratio is 9:1
Alcohol merges identical fraction and obtains 2.8g fraction；It crosses silicagel column (φ 2.5*80cm), selecting volume ratio is the chloroform-methanol etc. of 4:1
Degree elution, collects fraction, puts silica gel plate, is unfolded in chromatography cylinder, and solvent is the chloroform-methanol that volume ratio is 4:1, collects and closes
And the fraction more equal than analog values, the 600mg fraction more equal than analog values is obtained, next step gel post separation is carried out；
(8) gel column (φ 3*90cm) on the above-mentioned 600mg fraction more equal than analog values, the methanol for being 1:1 with volume ratio: water
Isocratic elution is carried out, fraction is collected, polyamide board is put, is unfolded in chromatography cylinder, solvent is the methanol-water that volume ratio is 1:1
System collects and merges the fraction more equal than analog values, obtains the 500mg fraction more equal than analog values, carries out next step ODS post separation；
(9) fraction above-mentioned 500mg more equal than analog values crosses ODS column (φ 2.5*80cm), according to polarity size, selects volume
Than the methanol-water isocratic elution for 7:3, several fractions are collected, polyamide board is put, is unfolded in chromatography cylinder, solvent is volume
Than the methanol-water for 7:3, collects and merge the fraction more equal than analog values, obtain 400mg product (compound 1), primarily determine as list
One substance (the ratio analog values of fraction are equal)；
(10) by efficient liquid phase on 400mg product, there is simple spike in the isocratic flushing of methanol-water for the use of volume ratio being 7:3
Shape is determined as uniform substance again；
(11) Structural Identification is carried out using mass spectrum MS and NMR spectrum NMR etc. to monomeric compound: collects uniform object
Matter, drying weighing weigh 50mg 1ml deuterated methanol and dissolve, carry out structure mirror using mass spectrum MS and NMR spectrum NMR etc.
It is fixed, narciclasine is determined that it is from atomic structure analysis.
The purity for the narciclasine that the present embodiment extracts is 95% or more.
Embodiment 2 determines the structure of compound 1
The compound 1 (20mg) that embodiment 1 is prepared is dissolved with 1ml deuterated methanol and is placed in nuclear magnetic tube, is utilized
Bruker DRX-400 Nuclear Magnetic Resonance, using tetramethylsilane (TMS) as internal standard compound, measure its hydrogen spectrum (1H-NMR) (Fig. 1),
Full decoupled carbon spectrum (13C-NMR) (Fig. 2).Test result is as illustrated in fig. 1 and 2.Fig. 1 be hydrogen spectrogram (1H-NMR map), Fig. 2 is carbon
Spectrogram (13C-NMR map).
Compound 1 is white crystal, methanol and dimethyl sulfoxide is dissolved in, after silica gel plate expansion, in uv analyzer
The ultraviolet lower display purple dot of 365nm, shows yellow band in allusion quotation cylinder.Pass through13C-NM R (100MHz, DMSO-d6) and knot
It closes1H-NMR (300MHz, DMSO-d6), the molecular formula for calculating the compound is C14H13NO7, and calculating degree of unsaturation is 9.Knot
It closes13C-NMR spectrum is it is found that there are also the carbon signal δ C132.2 of δ C169.0 conjugation lactone carbon signal and monosubstituted double bond in this compound
With 124.8.In the visible three companies oxygen methine signals δ C72.4 of High-Field, the methine signals δ C of 68.8,69.2 and one azines
52.9.Illustrate High-Field part cyclization according to degree of unsaturation.The compound scaffold is similar with phenanthridine alkaloid.
13C-NMR(100MHz,DMSO-d6):152.4(C-2),144.8(C-3),133.5(C-4),132.2(C-5),
129.3(C-6),124.8(C-7),105.6(C-8),102.1(C-9),95.9(C-10),72.4(C-11),69.2(C-12),
68.8 (C-13), 52.9 (C-14) speculate that the compound is (+)-narciclasine.Document above data and bibliography data
(Pettit G.R.；Melody N.；Antineoplastic Agents.Synthesis of 7-Deoxynarcistatin,
7-Deoxy-trans-dihydronarcistatin,and trans-Dihydronarcistatin1.J.Nat.Prod[J]
.2005,68 (2): 207-211.) it is almost the same, interpretation of result is shown in Table 1, therefore identifies that the compound is (+)-narciclasine.
1 compound 1 of table13The C-NMR chemical shift table of comparisons
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris, it is characterised in that: including such as
Lower step:
(1) short-tube lycoris dried, crushed, sieving processing, obtaining short-tube lycoris coarse powder；Using ethanol water heating and refluxing extraction stone
Garlic coarse powder, obtains extracting solution；The volume fraction of ethyl alcohol is 70% ~ 85% in ethanol water described in step (1)；
(2) extracting solution is concentrated under reduced pressure, obtains medicinal extract；Medicinal extract is dissolved using water, petroleum ether extraction is then used, obtains upper layer
Petroleum ether phase and lower layer water phase A；Lower layer water phase A is adopted and is extracted with ethyl acetate, ethyl acetate phase and lower layer's aqueous phase B are obtained；It will
Lower layer's aqueous phase B uses extracting n-butyl alcohol, obtains n-butanol phase and lower layer water phase C；
(3) n-butanol is mutually concentrated under reduced pressure, dries, obtains dry n-butanol phase；Dry n-butanol is mixed using methanol
Then solution is mixed with 100 ~ 200 mesh silica gel mixed samples, drying obtains the n-butanol phase by mixing sample processing；
(4) 200 ~ 300 mesh silica gel are filled into column, then will be mutually used a dry method on a sample by the n-butanol for mixing sample processing, then use chlorine
Imitation-carbinol mixed solvent isocratic elution, the fraction of elution is evaporated, the fraction being evaporated；The volume ratio of chloroform and methanol is
9:1；
(5) fraction being evaporated is dissolved using methanol, puts silica gel plate, is unfolded in chromatography cylinder, solvent is that volume ratio is 9:1's
Chloroform-methanol mixed solvent merges fraction more identical than analog values；Then fraction more identical than analog values is crossed into silicagel column, selects body
Product is eluted than the chloroform-methanol mixed solvent for being 4:1, collects fraction, is put silica gel plate, is unfolded in chromatography cylinder, solvent is body
Product merges the fraction more equal than analog values than the chloroform-methanol mixed solvent for being 4:1, obtains the chloroform-methanol that volume ratio is 4:1
The equal fraction of the ratio analog values of mixed solvent elution；
(6) fraction more equal than analog values is crossed into gel column, carries out isocratic elution with the Methanol+Water that volume ratio is 1:1,
Fraction is collected, polyamide board is put, is unfolded in chromatography cylinder, solvent is the Methanol+Water that volume ratio is 1:1, will be compared
The equal fraction of analog values merges, and obtains the equal fraction of the ratio analog values for the Methanol+Water elution that volume ratio is 1:1；
(7) the equal fraction of the ratio analog values that the Methanol+Water that volume ratio is 1:1 elutes is crossed into ODS column, using volume ratio
For the Methanol+Water isocratic elution of 7:3, fraction is collected, polyamide board is put, is unfolded in chromatography cylinder, solvent is body
Product merges the fraction more equal than analog values than the Methanol+Water for being 7:3, and drying obtains isoquinolone Alkaloid
Close object narciclasine.
2. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 1, special
Sign is: the mass volume ratio of short-tube lycoris coarse powder described in step (1) and ethanol water is 1g:10mL ~ 1g:25mL, described to add
The temperature of heat reflux is 80 DEG C ~ 100 DEG C, and the number of the extraction is 2 ~ 4 times, and the time extracted every time is 1 ~ 3 hour.
3. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 1, special
Sign is: the number of petroleum ether extraction described in step (2) is 3 ~ 5 times, specifically refers to use medicinal extract for petroleum ether extraction 3 ~ 5 times
Water dissolution, then uses petroleum ether extraction, obtains upper layer petroleum ether phase and lower layer's water phase, and lower water is mutually continued using petroleum ether
Extraction, so repeatedly 3 ~ 5 times, lower layer's water phase of last time extraction is lower layer's water phase A, upper layer petroleum ether is mutually merged, finally
Obtain petroleum ether phase and lower layer water phase A.
4. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 3, special
Sign is: extraction every time, the dosage of petroleum ether are as follows: the volume ratio of petroleum ether and solution is (1 ~ 2): 1, solution is by medicinal extract herein
Acquired solution is dissolved using water；
The petroleum ether is mutually concentrated under reduced pressure, drying and processing, obtains short-tube lycoris petroleum ether phase；The temperature of the reduced pressure is 40
DEG C ~ 50 DEG C, the temperature of the drying is 40 DEG C ~ 50 DEG C.
5. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 1, special
Sign is: the number of the extraction of ethyl acetate described in step (2) is 3 ~ 5 times, and ethyl acetate is extracted 3 ~ 5 times and specifically referred to lower layer
Water phase A, which is adopted, to be extracted with ethyl acetate, and upper layer ethyl acetate phase and lower layer's water phase are obtained, and lower water is mutually continued using ethyl acetate
Extraction, so repeatedly 3 ~ 5 times, lower layer's water phase of last time extraction is lower layer's aqueous phase B, upper layer ethyl acetate phase is merged, most
After obtain ethyl acetate phase and lower layer's aqueous phase B.
6. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 5, special
Sign is: extraction every time, the dosage of ethyl acetate are as follows: the volume ratio of ethyl acetate and lower layer's water phase A are (1 ~ 2): 1；
The ethyl acetate phase is concentrated under reduced pressure, drying and processing, obtains short-tube lycoris ethyl acetate phase；The temperature of the reduced pressure
It is 40 DEG C ~ 50 DEG C, the temperature of the drying is 40 DEG C ~ 50 DEG C.
7. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 1, special
Sign is: the number of extracting n-butyl alcohol described in step (2) is 3 ~ 5 times, is specifically referred to lower layer's water phase for extracting n-butyl alcohol 3 ~ 5 times
B uses extracting n-butyl alcohol, obtains upper layer n-butanol phase and lower layer's water phase, and lower water is mutually continued using extracting n-butyl alcohol, so
It repeats 3 ~ 5 times, lower layer's water phase of last time extraction is lower layer's water phase C, and upper layer n-butanol is mutually merged, n-butanol is finally obtained
Phase and lower layer's water phase C.
8. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 7, special
Sign is: the dosage that n-butanol extracts every time are as follows: the volume ratio of n-butanol and lower layer's aqueous phase B is (1 ~ 2): 1.
9. the method for extracting isoquinolone Alkaloid compounds narciclasine from short-tube lycoris according to claim 1, special
Sign is: the condition of reduced pressure described in step (2) are as follows: pressure is 0.09 ~ 0.1MPa, and thickening temperature is 40 DEG C ~ 60 DEG C, until
Until no longer screwing out liquid；
The temperature of reduced pressure described in step (3) is 50 DEG C ~ 60 DEG C；During dry n-butanol is mutually prepared, the temperature of the drying
Degree is 40 DEG C ~ 60 DEG C；
Dry n-butanol phase and 100 ~ 200 mesh silica gel quality ratio 1:1.5 ~ 1:3 described in step (3)；By mixing sample processing
During n-butanol is mutually prepared, the condition of the drying is that drying to constant weight at 40 DEG C ~ 50 DEG C；
200 ~ 300 mesh silica gel described in step (4) and the mass ratio of n-butanol phase dry in step (3) are (30 ~ 50): 1.
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| CN101008023A (en) * | 2006-12-20 | 2007-08-01 | 贵州芊芊园艺新技术发展公司 | Technology for extracting dihydrogalanthamine from lycoris radiata genus plant |
| CN101102769A (en) * | 2005-01-14 | 2008-01-09 | 亚利桑那董事会，代表亚利桑那州立大学行事的亚利桑那州法人团体 | Synthesis of sodium narcistatin and related compounds |
| CN106543194A (en) * | 2015-09-22 | 2017-03-29 | 孙青* | Narciclasine derivative and its preparation and the application in antineoplastic is prepared |
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| US20090203646A1 (en) * | 2008-02-12 | 2009-08-13 | Sun Health Research Institute | Use of sodium narcistatin for reducing internal adhesions and fibrosis |
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| CN101102769A (en) * | 2005-01-14 | 2008-01-09 | 亚利桑那董事会，代表亚利桑那州立大学行事的亚利桑那州法人团体 | Synthesis of sodium narcistatin and related compounds |
| CN101008023A (en) * | 2006-12-20 | 2007-08-01 | 贵州芊芊园艺新技术发展公司 | Technology for extracting dihydrogalanthamine from lycoris radiata genus plant |
| CN106543194A (en) * | 2015-09-22 | 2017-03-29 | 孙青* | Narciclasine derivative and its preparation and the application in antineoplastic is prepared |
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