CN106916131B - The preparation method and its pharynx-clearing throat-benefiting effect of a kind of isobenzofuran class compound in pueraria lobata - Google Patents
The preparation method and its pharynx-clearing throat-benefiting effect of a kind of isobenzofuran class compound in pueraria lobata Download PDFInfo
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- CN106916131B CN106916131B CN201710078271.2A CN201710078271A CN106916131B CN 106916131 B CN106916131 B CN 106916131B CN 201710078271 A CN201710078271 A CN 201710078271A CN 106916131 B CN106916131 B CN 106916131B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
- C07D307/77—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D307/87—Benzo [c] furans; Hydrogenated benzo [c] furans
- C07D307/88—Benzo [c] furans; Hydrogenated benzo [c] furans with one oxygen atom directly attached in position 1 or 3
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/14—Use of materials for tobacco smoke filters of organic materials as additive
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/488—Pueraria (kudzu)
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- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a kind of isobenzofuran class compounds and its preparation method and application, the isobenzofuran class compound is isolated from traditional Chinese medicine pueraria lobata, name are as follows: 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene)-isobenzofuran -1 (3H) -one, English name are as follows: 6-hydroxy-5- (3-methyl-2-oxobut-3-enyl)-isobenzofuran-1 (3H)-one, molecular formula C13H12O4, there is following structural formula:(I) preparation method of the isobenzofuran class compound is to obtain using traditional Chinese medicine pueraria lobata as raw material through medicinal extract extraction, organic solvent extraction, MCI decoloration, silica gel column chromatography, high pressure liquid chromatography separating step.The compounds of this invention is added in cigarette filter, can reduce cigarette smoking throat irritation, has obvious pharynx-clearing throat-benefiting effect.
Description
Technical field
The invention belongs to technical field of phytochemistry, and in particular to it is a kind of extracted for the first time from Chinese medicine pueraria lobata it is different
Benzofuran compounds.Meanwhile the compounds of this invention is added in cigarette filter, can reduce the stimulation of cigarette smoking throat
Property, there is obvious pharynx-clearing throat-benefiting effect.
Background technique
Pueraria lobata is the dry root of legume pueraria lobata, practises and claims elegant jessamine.Autumn, the excavation of two season of winter, fresh-cut is taken advantage of into sheet or fritter；
It is dry.It is sweet, pungent, it is cool.There is expelling pathogenic factors from muscles and skin to bring down a fever, promoting eruption promotes the production of body fluid to quench thirst, the function of Shengyang Zhixie.It is usually used in exterior syndrome to generate heat, stiff nape and back,
Measles without adequate eruption, pyreticosis is thirsty, and the deficiency of Yin is quenched one's thirst, and heat is purged heat dysentery, splenasthenic diarrhea.Pueraria lobata is also a kind of important health food simultaneously,
Containing can increase the sweet sense in oral cavity, action and efficacy of promoting the production of body fluid ingredient, it is known as the good reputation of " asia ginseng ", kudzuvine root starch is referred to as " long-lived powder ",
" royal specially offered food " is known as in Japan.
Main chemical compositions in pueraria lobata are flavonoids, and main active is daidzein, daidzin, Puerarin, pueraria lobata
Element -7- xyloside etc., the compound also containing the other structures type such as terpene, lactone, sterol.Lactone refers in same molecule
The ester type compound of carboxyl and hydroxyl interaction dehydration and formation, such compound is generally existing in natural plants, in day
Also there is the document report for being widely present such compound in right plant, except with extensive pharmacological action, lactone or a kind of weight
The volatile compound wanted is naturally present in various fruit and spice berry, such compound be widely used in various beverages,
In the formula of the edible essences such as bakery product.
The present invention isolated a kind of benzo lactone compound, the compound from pueraria lobata are added to cigarette filter
In, cigarette smoking throat irritation can be reduced, there is obvious pharynx-clearing throat-benefiting effect, the suction comfort of cigarette can be improved.
Summary of the invention
The first object of the present invention is to provide a kind of isobenzofuran class compound；Second be designed to provide it is described different
The preparation method of benzofuran compounds；Third is designed to provide the isobenzofuran class compound as cigarette filter
The application of additive is used.
The first object of the present invention is achieved in that the isobenzofuran class compound is from traditional Chinese medicine Pueraria lobota
It is isolated in root, molecular formula C13H12O4, have a structure in which
The compound is light yellow gum object, name are as follows: 6- hydroxyl -5- (3- methyl -
2- oxo butyl- 3- alkene)-isobenzofuran -1 (3H) -one, English name are as follows: 6-hydroxy-5- (3-methyl-2-oxobut-3-
enyl)isobenzofuran- 1(3H)-one。
The second object of the present invention is achieved in that the preparation method of the isobenzofuran class compound, is with Pueraria lobota
Root block is raw material, is walked through medicinal extract extraction, organic solvent extraction, MCI decoloration, silica gel column chromatography, high performance liquid chromatography preparative separation
Suddenly, specifically:
A, medicinal extract extracts: the root block of pueraria lobata is crushed to 20 ~ 40 mesh, with organic solvent ultrasonic extraction 2 ~ 5 times, every time 30 ~
60 minutes, extracting solution was concentrated under reduced pressure in combined extract, filtering, stands, filters out sediment, be condensed into medicinal extract a；
B, organic solvent extracts: the water of 1 ~ 2 times of weight ratio amount is added in medicinal extract a, then with isometric organic of water
Solvent extraction 3 ~ 5 times, merge organic solvent extraction phase, is concentrated under reduced pressure into medicinal extract b；
C, MCI decolourizes: the methanol-water dissolution of 3 ~ 5 times of weight ratio amounts, upper MCI column, with 90%-95% methanol is added in medicinal extract b
Water elution merges organic phase, is concentrated under reduced pressure into medicinal extract c;
D, silica gel column chromatography: silica gel column chromatography on medicinal extract c, dress column silica gel be 160 ~ 200 mesh, dosage be medicinal extract c weight 6 ~
10 times of amounts；It is the chloroform and acetone mixed organic solvents gradient elution of 1:0 ~ 0:1 with volume proportion, collects gradient eluent, dense
Contracting, monitors through TLC, merges identical part；
E, high performance liquid chromatography separation: by the eluent for being afforded chloroform-acetone of 7:3 with volume content through efficient
Liquid chromatogram isolates and purifies to get the isobenzofuran class compound.
The structure for the isobenzofuran class compound being in the above way prepared is to identify to come by the following method:
The compounds of this invention is light yellow gum object；HRESI-MS shows that its quasi-molecular ion peak is 255.0630 [M+
Na]+(calculated value 255.0633), in conjunction with1H NMR and DEPT, which are composed, determines that its molecular formula is C13H12O4, degree of unsaturation 8.
Hydroxyl (3465 cm are shown in infrared spectroscopy-1), carbonyl (1749 and 1660 cm-1) and aromatic ring (1612,1546 and
1469 cm-1) resonance absorbing peak.And ultraviolet spectra has absorption maximum to also illustrate in compound in 210,272,308 nm
There may be aromatic ring structures.Compound1H and13C H NMR spectroscopy (table -1) shows that it contains 13 carbon and 12 hydrogen, including 11,
2,4,5- quaternary phenyl ring (C-4 ~ C-7, C-4a and C-7a, H-4 and H-7), a 3- methyl -2- oxo butyl- 3- alkene knot
Tile section (C-1' ~ C-5', H2-1'、H2- 4' and H3- 5), ester carbonyl group (δ C168.8 s), the methylene of an oxidation
(δ C74.1 t,δ H5.17 s) and phenolic hydroxyl group (δ H10.52 s).Its HMBC coherent signal is further analyzed, according to
H2- 3 and C-1, C-4, C-4a, C-7a, the HMBC phase of H-7 and C-1, C-4a, C-7a and H-4 and C-3, C-4a, C-7a
Closing (Fig. 3) can speculate that compound is benzofuran lactone structure.H-1' and C-4, C- can be observed in the HMBC spectrum of compound
5,C-6；And H-4 is long-range related to C-1''s, can speculate that 3- methyl -2- oxo butyl- 3- alkene structure fragment is substituted in compound
The position C-5.According to phenolic hydroxyl group signal (δ H10.52 s) have that HMBC is related to C-5, C-6 to C-7, can speculate that phenolic hydroxyl group is substituted in
C-6.So far, the structure of compound is determined, and is named as 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene)-different benzene
And furans -1 (3H) -one.
Infrared, the ultraviolet and mass spectrometric data of compound: UV (methanol),λ max (log ε) 308 (3.09)、272
(3.69),210 (4.01) nm；IR (pressing potassium bromide troche):ν max 3465、3021、2946、1749、1660、1612、1546、
1469、1370、1274、1153、1067、908、859 cm-1；1H and13C NMR data (500 and 125 MHz,
(CDCl3), it is shown in Table -1；Positive ion mode ESIMSm/z 255 [M+Na]+；Positive ion mode HRESIMSm/z 255.0630
[M+Na]+(calculated value C13H12NaO4, 255.0633).
- 1. the compounds of this invention of table1H NMR and13C NMR data (CDCl3)
The third object of the present invention is achieved in that the isobenzofuran class compound is added as cigarette filter
The application of agent.In view of triacetyl glycerine is that cigarette filter forms most common plasticizer, and the compounds of this invention is dissolved in
Triacetyl glycerine, in cigarette filter forming process, the compounds of this invention is added in filter tip by triacetyl glycerine.
Isobenzofuran class compound of the present invention is separated for the first time, passes through nuclear magnetic resonance and measuring method of mass spectrum
It is determined as isobenzofuran class compound, and characterizes its structure.The compounds of this invention is added to volume by triacetyl glycerine
In tobacco filters, the identical cigarette to be not added with the compound carries out sensory evaluation as control.Evaluation and analysis the result shows that: and it is right
Photograph is compared, and addition the compounds of this invention can reduce cigarette smoking throat irritation, has obvious pharynx-clearing throat-benefiting effect.The present invention
Compound is added in cigarette filter, easy to accomplish in technique, does not increase the additional step in production process, can be obviously improved volume
Cigarette suction quality has good application prospect.
Detailed description of the invention
Fig. 1 be isobenzofuran class compound of the present invention carbon-13 nmr spectra (13C NMR)；
Fig. 2 be isobenzofuran class compound of the present invention nuclear magnetic resonance spectroscopy (1H NMR)；
Fig. 3 is the crucial HMBC correlation figure of isobenzofuran class compound of the present invention.
Specific embodiment
The present invention will be further described below with reference to the drawings, but the present invention is limited in any way, base
In present invention teach that made any transformation or improvement, each fall within protection scope of the present invention.
Unless otherwise indicated, percentage of the present invention is mass percent.
Isobenzofuran class compound of the present invention is isolated from traditional Chinese medicine pueraria lobata, molecular formula
For C13H12O4, have a structure in which
The compound is light yellow gum object, name are as follows: 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene) different benzo
Furans -1 (3H) -one, English name are as follows: 6-hydroxy-5- (3-methyl-2-oxobut-3-enyl) isobenzofuran- 1
(3H)-one。
The preparation method of isobenzofuran class compound of the present invention is to mention using the root block of pueraria lobata as raw material through medicinal extract
It takes, organic solvent extraction, MCI decoloration, silica gel column chromatography, high performance liquid chromatography preparative separation step, specifically:
A, medicinal extract extracts: the root block of pueraria lobata is broken to 20 ~ 40 mesh, with organic solvent ultrasonic extraction 2 ~ 5 times, and every time 30 ~ 60
Minute, extracting solution is concentrated under reduced pressure in combined extract, filtering, stands, filters out sediment, be condensed into medicinal extract a；
B, organic solvent extracts: the water of 1 ~ 2 times of weight ratio amount is added in medicinal extract a, then with isometric organic of water
Solvent extraction 3 ~ 5 times, merge organic solvent extraction phase, is concentrated under reduced pressure into medicinal extract b；
C, MCI decolourizes: the methanol-water dissolution of 3 ~ 5 times of weight ratio amounts, upper MCI column, with 80%-90% methanol is added in medicinal extract b
Water elution merges organic phase, is concentrated under reduced pressure into medicinal extract c；
D, silica gel column chromatography: silica gel column chromatography on medicinal extract c, dress column silica gel be 160 ~ 200 mesh, dosage be medicinal extract c weight 6 ~
10 times of amounts；It is the chloroform and acetone mixed organic solvents gradient elution of 1:0 ~ 0:1 with volume proportion, collects gradient eluent, dense
Contracting, monitors through TLC, merges identical part；
E, high performance liquid chromatography separation: will be that the eluent for affording the chloroform-acetone of (7:3) is passed through with volume content
High performance liquid chromatography separation purifies to get the isobenzofuran class compound.
The organic solvent of the step A be 70 ~ 100% acetone, 90 ~ 100% ethyl alcohol or 90 ~ 100% methanol.
The organic solvent of the step B is methylene chloride, chloroform, ethyl acetate ether or petroleum ether.
Before through silica gel column chromatography, the acetone or methanol measured with 1.5 ~ 3 times of weight ratio dissolve medicinal extract c in the D step,
Then 0.8 ~ 1.2 times of 80 ~ 100 mesh silica gel mixed samples are weighed with medicinal extract.
The chloroform of the D step and the volume proportion of acetone mixed organic solvents are 20:1,9:1,8:2,7:3,6:4
And 1:1.
The high performance liquid chromatography separation purifying of the E step is 15 ~ 25 ml/ of flow velocity using the methanol of 35-46% as mobile phase
Min, with 21.2 × 250 mm, 5 μm of Zorbax PrepHT GF reverse phase preparative column is stationary phase, and UV detector detects wave
A length of 308 nm, each 10 ~ 100 μ L of sample introduction collect the chromatographic peak of 20 ~ 40 min, are evaporated after repeatedly adding up.
The compounds of this invention is added in cigarette filter, has preferable flavouring effect；And compare with control, add
Add the compounds of this invention that can reduce cigarette smoking throat irritation, there is obvious pharynx-clearing throat-benefiting effect.
Pueraria lobata of the present invention is not limited by area and kind, and the present invention may be implemented.
Embodiment 1
Dry 4.4 kg of pueraria lobata block is taken, coarse powder is broken to 30 mesh, with acetone ultrasonic extraction 4 times of 70%, 60 minutes every time,
Extracting solution merges；Extracting solution filtering, is concentrated under reduced pressure into the 1/4 of volume；It stands, filters out sediment, be condensed into the medicinal extract a of 120g；
250g water is added in medicinal extract a, is extracted 5 times with the isometric chloroform of water, merges extraction phase, be concentrated under reduced pressure into 80g medicinal extract b；
Medicinal extract b fills column with MCI, the 80% methanol-water dissolution of 240 g is added in medicinal extract b, then upper prop, is washed for 2 to 6 liters with 90% methanol-water
It is de-, eluent is collected, 62 g medicinal extract c are concentrated under reduced pressure to give；The acetone solution of 120g is added in medicinal extract c in medicinal extract c, is then added
100 mesh silica gel, 62 g mixes sample, after mixing sample, fills column with 200 mesh silica gel, 400 g；It is respectively 20:1,9:1,8:2 with volume ratio,
The chloroform of 7:3,6:4 and 1:1-acetone mixed organic solvents gradient elution are collected gradient eluent, concentration, are monitored through TLC,
Merge identical part, obtain 6 part A-F, wherein to 14 g of the part sample D (7:3) being collected into, then with 40% first
Alcohol is mobile phase, and flow velocity 20 ml/min, 21.2 × 250 mm, 5 μm of Zorbax PrepHT GF reverse phase preparative column is solid
Determine phase, UV detector Detection wavelength is 308 nm, each 50 μ L of sample introduction, the chromatographic peak of 33.9 min is collected, after repeatedly adding up
It is evaporated to get the isobenzofuran class compound.
Embodiment 2
Dry 10 kg of pueraria lobata block is taken, coarse powder is broken to 40 mesh, is extracted 4 times, 3 days every time, is extracted with 80% methanol cold soaking
Liquid merges；Extracting solution filtering, is concentrated under reduced pressure into the 1/4 of volume；It stands, filters out sediment, be condensed into 300 g medicinal extract a；In medicinal extract
350 g water are added in a, is extracted 5 times with the isometric ethyl acetate of water, merges extraction phase, be concentrated under reduced pressure into 210 g medicinal extract b；
Medicinal extract b fills column with MCI, the 80% methanol-water dissolution of 600 g is added in medicinal extract b, then upper prop, with 5 to 15 liters of 90% methanol-water
Elution collects eluent, is concentrated under reduced pressure to give 150 g medicinal extract c；The acetone solution of 300 g is added in medicinal extract c, is then added 100
150 g of mesh silica gel mixes sample, fills column with 200 mesh silica gel, 1 Kg, mixes upper prop after sample；It is respectively 20:1,9:1,8:2 with volume ratio,
The chloroform of 7:3,6:4 and 1:1-acetone mixed organic solvents gradient elution are collected gradient eluent, concentration, are monitored through TLC,
Merge identical part, obtain 6 part A-F, wherein to 25 g of the part sample D (7:3) being collected into, then with 40% first
Alcohol is mobile phase, and flow velocity 20 ml/min, 21.2 × 250 mm, 5 μm of Zorbax PrepHT GF reverse phase preparative column is to fix
Phase, UV detector Detection wavelength are 308 nm, each 80 μ L of sample introduction, collect the chromatographic peak of 33.9 min, steam after repeatedly adding up
It does to get the noval chemical compound.
Embodiment 3
Compound prepared by Example 1 is light yellow gum object；
Measuring method are as follows: use nuclear magnetic resonance, identify structure in conjunction with other spectroscopic techniques.
HRESI-MS shows that its quasi-molecular ion peak is 255.0630 [M+Na]+(calculated value 255.0633), in conjunction with1H
NMR and DEPT, which is composed, determines that its molecular formula is C13H12O4, degree of unsaturation 8.Hydroxyl (3465 cm are shown in infrared spectroscopy-1), carbonyl (1749 and 1660 cm-1) and aromatic ring (1612,1546 and 1469 cm-1) resonance absorbing peak.And ultraviolet light
Spectrum has absorption maximum to also illustrate that there may be aromatic ring structures in compound in 210,272,308 nm.Compound1H and13C
H NMR spectroscopy (table -1) shows that it contains 13 carbon and 12 hydrogen, including 11,2,4,5- quaternary phenyl ring (C-4 ~ C-7, C-4a
And C-7a, H-4 and H-7), 3- methyl -2- oxo butyl- 3- alkene structure fragment (C-1' ~ C-5', a H2-1'、H2- 4' and H3-
5), ester carbonyl group (δ C168.8 s), one oxidation methylene (δ C74.1 t,δ H5.17 s) and a phenol hydroxyl
Base (δ H10.52 s).Its HMBC coherent signal is further analyzed, according to H2- 3 and C-1, C-4, C-4a, C-7a, H-7 and C-
1, C-4a, C-7a and H-4 (Fig. 3) related to the HMBC of C-3, C-4a, C-7a can speculate that compound is benzofuran lactone
Structure.H-1' and C-4, C-5, C-6 can be observed in the HMBC spectrum of compound；And H-4 is long-range related to C-1''s, can push away
Survey the position C-5 that 3- methyl -2- oxo butyl- 3- alkene structure fragment is substituted in compound.According to phenolic hydroxyl group signal (δ H 10.52 s)
Have that HMBC is related to C-5, C-6 to C-7, can speculate that phenolic hydroxyl group is substituted in C-6.So far, the structure of compound is determined, and
It is named as 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene)-isobenzofuran -1 (3H) -one.
Embodiment 4
Compound prepared by Example 2 is light yellow gum object.Measuring method is same as Example 3, and confirmation implements 2
The compound of preparation is the isobenzofuran class compound --- 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene)-different benzene
And furans -1 (3H) -one.
Embodiment 5
The isobenzofuran compound of any preparation in Example 1-2 carries out the additive effect test of cigarette filter, examination
It is as follows to test situation:
For the cigarette " purple cloud " that addition cigarette is the Red River Hong Yun group, with triacetyl glycerine by above-mentioned isobenzofuran
The compound solution for being made into 0.1 mg/mL.It is uniformly sprayed on filter tow by the 8% of filter tow weight, filter is made
Then the filter stick is made cigarette by conventional cigarette cigarette, carries out sensory evaluation, and to be not added with the phase of the compound by stick
With cigarette as control.Evaluation and analysis the result shows that: compare with control, addition the compounds of this invention can reduce cigarette smoking throat pierce
Swash property, there is obvious pharynx-clearing throat-benefiting effect.
Embodiment 6
The isobenzofuran compound of any preparation in Example 1-4 carries out the additive effect test of cigarette filter,
For the cigarette " purple cloud " that addition cigarette is the Red River Hong Yun group, with triacetyl glycerine by above-mentioned isobenzofuran
The compound solution for being made into 0.2 mg/mL.It is uniformly sprayed on filter tow by the 5% of filter tow weight, filter is made
Then the filter stick is made cigarette by conventional cigarette cigarette, carries out sensory evaluation, and to be not added with the phase of the compound by stick
With cigarette as control.Evaluation and analysis the result shows that: compare with control, addition the compounds of this invention can reduce cigarette smoking throat pierce
Swash property, there is obvious pharynx-clearing throat-benefiting effect.
Claims (6)
1. a kind of isobenzofuran class compound, it is characterised in that the isobenzofuran class compound is from traditional Chinese medicine Pueraria lobota
It is isolated in root, name are as follows: 6- hydroxyl -5- (3- methyl -2- oxo butyl- 3- alkene)-isobenzofuran -1 (3H) -one, English
Name are as follows: 6-hydroxy-5- (3-methyl-2-oxobut-3-enyl)-isobenzofuran-1 (3H)-one, molecular formula
For C13H12O4, have a structure in which
。
2. the preparation method of isobenzofuran class compound described in a kind of claim 1, it is characterised in that using pueraria lobata block as raw material,
It is extracted through medicinal extract, organic solvent extraction, MCI decoloration, silica gel column chromatography, high performance liquid chromatography separation step, specifically:
A, medicinal extract extracts: pueraria lobata being crushed to 20 ~ 40 mesh, with organic solvent ultrasonic extraction 2 ~ 5 times, every time 30 ~ 60 minutes, is merged
Extracting solution is concentrated under reduced pressure in extracting solution, filtering, stands, filters out sediment, be condensed into medicinal extract a；
B, organic solvent extracts: the water of 1 ~ 2 times of weight ratio amount being added in medicinal extract a, then with the organic solvent isometric with water
Extraction 3 ~ 5 times merges organic solvent extraction phase, is concentrated under reduced pressure into medicinal extract b；
C, MCI decolourizes: the methanol-water dissolution of 3 ~ 5 times of weight ratio amounts is added in medicinal extract b, upper MCI column is washed with 90%-95% methanol
It is de-, merge organic phase, is concentrated under reduced pressure into medicinal extract c;
D, silica gel column chromatography: silica gel column chromatography on medicinal extract c, dress column silica gel are 160 ~ 200 mesh, and dosage is 6 ~ 10 times of medicinal extract c weight
Amount；It is the chloroform and acetone mixed organic solvents gradient elution of 1:0 ~ 0:1 with volume proportion, collects gradient eluent, concentration, warp
TLC monitoring, merges identical part；
E, high performance liquid chromatography separation: the eluent that chloroform-acetone of 7:3 is afforded is pure through high performance liquid chromatography separation
Change to get the isobenzofuran class compound.
3. the preparation method of isobenzofuran class compound according to claim 2, it is characterised in that the step A has
Solvent be 70 ~ 100% acetone, 90 ~ 100% ethyl alcohol or 90 ~ 100% methanol.
4. the preparation method of isobenzofuran class compound according to claim 2, it is characterised in that the step B has
Solvent is methylene chloride, chloroform, ethyl acetate, ether or petroleum ether.
5. the preparation method of isobenzofuran class compound according to claim 2, it is characterised in that soaked in the D step
Before through silica gel column chromatography, the acetone or methanol measured with 1.5 ~ 3 times of weight ratio dissolve cream c, then weigh 0.8 ~ 1.2 times with medicinal extract
80 ~ 100 mesh silica gel mixed samples.
6. the preparation method of isobenzofuran class compound according to claim 2, it is characterised in that the chlorine of the D step
Imitative and acetone mixed organic solvents volume proportions are 20:1,9:1,8:2,7:3,6:4 and 1:1.
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