CN102503918B - Separation and purification method for dehydrodiisoeugenol monomers - Google Patents
Separation and purification method for dehydrodiisoeugenol monomers Download PDFInfo
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- CN102503918B CN102503918B CN 201110420161 CN201110420161A CN102503918B CN 102503918 B CN102503918 B CN 102503918B CN 201110420161 CN201110420161 CN 201110420161 CN 201110420161 A CN201110420161 A CN 201110420161A CN 102503918 B CN102503918 B CN 102503918B
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- isoeugenol
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- 239000000178 monomer Substances 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000000926 separation method Methods 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims abstract description 8
- ITDOFWOJEDZPCF-AATRIKPKSA-N 2-methoxy-4-[7-methoxy-3-methyl-5-[(e)-prop-1-enyl]-2,3-dihydro-1-benzofuran-2-yl]phenol Chemical compound O1C=2C(OC)=CC(\C=C\C)=CC=2C(C)C1C1=CC=C(O)C(OC)=C1 ITDOFWOJEDZPCF-AATRIKPKSA-N 0.000 title abstract description 6
- ITDOFWOJEDZPCF-CWTRNNRKSA-N Dehydro-diisoeugenol Natural products COC1=CC(=CC=2[C@H]([C@@H](OC=21)C1=CC(=C(C=C1)O)OC)C)C=CC ITDOFWOJEDZPCF-CWTRNNRKSA-N 0.000 title abstract description 6
- ITDOFWOJEDZPCF-UHFFFAOYSA-N dl-Dehydrodiisoeugenol Natural products O1C=2C(OC)=CC(C=CC)=CC=2C(C)C1C1=CC=C(O)C(OC)=C1 ITDOFWOJEDZPCF-UHFFFAOYSA-N 0.000 title abstract description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 47
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000741 silica gel Substances 0.000 claims abstract description 25
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 25
- 239000003480 eluent Substances 0.000 claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 235000009421 Myristica fragrans Nutrition 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 238000006356 dehydrogenation reaction Methods 0.000 claims description 44
- BJIOGJUNALELMI-UHFFFAOYSA-N trans-isoeugenol Natural products COC1=CC(C=CC)=CC=C1O BJIOGJUNALELMI-UHFFFAOYSA-N 0.000 claims description 44
- BJIOGJUNALELMI-ONEGZZNKSA-N Isoeugenol Natural products COC1=CC(\C=C\C)=CC=C1O BJIOGJUNALELMI-ONEGZZNKSA-N 0.000 claims description 37
- BJIOGJUNALELMI-ARJAWSKDSA-N cis-isoeugenol Chemical compound COC1=CC(\C=C/C)=CC=C1O BJIOGJUNALELMI-ARJAWSKDSA-N 0.000 claims description 37
- 239000000284 extract Substances 0.000 claims description 24
- 239000000047 product Substances 0.000 claims description 24
- 229960001866 silicon dioxide Drugs 0.000 claims description 24
- 238000000605 extraction Methods 0.000 claims description 22
- 238000002360 preparation method Methods 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 17
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 15
- 210000000582 semen Anatomy 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 10
- 239000012071 phase Substances 0.000 claims description 10
- 238000004587 chromatography analysis Methods 0.000 claims description 8
- 239000007791 liquid phase Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 6
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- -1 extraction Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000012856 packing Methods 0.000 claims description 5
- 238000004262 preparative liquid chromatography Methods 0.000 claims description 5
- 238000000658 coextraction Methods 0.000 claims description 4
- 238000001514 detection method Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 238000003810 ethyl acetate extraction Methods 0.000 claims description 4
- 239000000945 filler Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 235000012054 meals Nutrition 0.000 claims description 4
- 238000012544 monitoring process Methods 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000004062 sedimentation Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 239000008346 aqueous phase Substances 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 241000498779 Myristica Species 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000001702 nutmeg Substances 0.000 claims description 2
- 238000010025 steaming Methods 0.000 claims description 2
- 239000006200 vaporizer Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 244000270834 Myristica fragrans Species 0.000 abstract description 3
- 239000004480 active ingredient Substances 0.000 abstract description 2
- 235000008216 herbs Nutrition 0.000 abstract description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract 2
- 239000003208 petroleum Substances 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 238000004811 liquid chromatography Methods 0.000 description 3
- YTJSFYQNRXLOIC-UHFFFAOYSA-N octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[SiH3] YTJSFYQNRXLOIC-UHFFFAOYSA-N 0.000 description 3
- 238000004007 reversed phase HPLC Methods 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 241001081833 Myristicaceae Species 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 208000001848 dysentery Diseases 0.000 description 1
- 230000004345 fruit ripening Effects 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 244000045947 parasite Species 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 230000008673 vomiting Effects 0.000 description 1
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- Treatment Of Liquids With Adsorbents In General (AREA)
Abstract
The invention relates to a method for extracting and separating dehydrodiisoeugenol monomers from myristica fragrans, which belongs to the technical field of separation and purification of active ingredients of Chinese herbs, and includes the steps of utilizing the myristica fragrans as raw materials for extracting ethanol and ethyl acetate; utilizing petroleum ether (60-90 DEG C)- ethyl acetate as eluent for silica gel column depravation; utilizing methyl alcohol and water as mobile phase for high-performance liquid chromatographic column separation, wherein the detected wavelength is 274nm;obtaining the dehydrodiisoeugenol monomers and the like. The method is simple and convenient in operation, short in production cycle, high in separation efficiency, stable in process, low in cost andcapable of preparing a great number of high-purity dehydrodiisoeugenol monomers by means of separation, the obtained dehydrodiisoeugenol monomers are high in purity and can be used as comparison products for content determination.
Description
Technical field
The present invention relates to a kind of preparation method of plant compound monomer, be specifically related to the method for extraction separation dehydrogenation two isoeugenol monomers from Semen Myristicae, belong to the separating and purifying technology field of active ingredient of Chinese herbs.
Background technology
Semen Myristicae, Myristicaceae nux moschata plant Semen Myristicae
Myristica fragransHoutt. drying kind benevolence.Main product is in Malaysia, Indonesia; Also there is cultivation in China Guangdong, Guangxi, Yunnan.This kind is famous spices and medicinal plant of the torrid zone.Winter, two season of spring gather during fruit maturation.Its kind benevolence is used as medicine, and can control void and rush down cold dysentery, coldness and pain in the epigastrium, vomiting etc.; External application can be made the parasite expellent, treatment rheumatalgia etc.Dehydrogenation two isoeugenols are characteristic constituents in the Semen Myristicae, its English name Dehydrodiisoeugenol, and molecular formula is C
20H
22O
4 +, molecular weight is 326.39, belongs to Lignanoids compounds, its structural formula is as follows:
Dehydrogenation two isoeugenols are characteristic constituents in the Semen Myristicae, and version Chinese Pharmacopoeia in 2010 is unique foundation of differentiating Semen Myristicae medicinal material standard with dehydrogenation two isoeugenols.
But the contriver finds to have only the document introduction to the conventional crystallization of dehydrogenation two isoeugenols at present by consulting lot of documents, but good separating high purity dehydrogenation two isoeugenols all.Therefore, up to now, still from Semen Myristicae, do not prepare the maturation process report of effective constituent dehydrogenation two isoeugenols.
Summary of the invention
The present invention is intended to overcome the defective of prior art, provide a kind of from Semen Myristicae the method for extraction separation dehydrogenation two isoeugenol monomers.This method is easy and simple to handle, the separation efficiency height, and process stabilizing, with low cost, can realize the industrial separation preparation of dehydrogenation two isoeugenol monomers, the dehydrogenation two isoeugenol monomer purity height that obtain can reach more than 99.5%.
In order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of separation purification method of dehydrogenation two isoeugenol monomers, it be with the Semen Myristicae be that raw material extracts, extraction, silicagel column separates and preparation is reclaimed and got, its concrete processing step is as follows:
A, extraction:
The ground nutmeg of drying is broken into meal, be that to add mass percent concentrations be 95% ethanolic soln for 1:8～10 by medicinal material weight and ethanol volume ratio, heating and refluxing extraction, extract altogether 3 times, each 2～3 hours, extracting liquid filtering merged filtered liquid, concentrate and reclaim ethanol, get concentrated extract and treat that next step carries out extraction treatment;
B, extraction:
Water (80 ℃) dilution that adds 1 times of volume in the volume of steps A gained concentrated extract, add again with dilution after the ethyl acetate extraction of 1 times of volume of the medicinal extract aqueous solution, coextraction 3 times, the combined ethyl acetate layer, be concentrated into into fluid extract for 55 ℃ with revolving the steaming vaporizer, the dry silicagel column that is equipped with of 60～80 order silica gel mixed samples that adds 5 times of gained medicinal extract weight separates;
C, silicagel column separate:
Mix all product weight according to step B gained, take by weighing 200～300 order silica gel of 10 times of weight, mix thoroughly in the glass chromatography column of packing into eluent, use the eluent sedimentation, till the constant flow rate; With dry good silica gel sample among the step B, in the glass chromatography column of packing into, use the eluent wash-out, detect according to TLC and collect dehydrogenation two isoeugenol product sections, reclaim eluent, get white cotton-shaped solid;
Described eluent is made up of by the 6:1 volume ratio sherwood oil (60-90 ℃) and ethyl acetate.
D, high performance liquid phase preparation separate:
Get the solid of step C gained, press the dissolving of 1g:10ml solution, filter with dimethyl formamide (DMF), the preparation of carrying out dehydrogenation two isoeugenol monomers separates, the UV-detector on-line monitoring, specific aim is collected the preparation cut solution of dehydrogenation two isoeugenol monomers, gets dehydrogenation two isoeugenol monomer solutions;
It is the chromatographic column of C18 that described high performance liquid phase separates the employing filler; Moving phase consists of: by volume, methyl alcohol: water=75:25, the detection wavelength is 274nm.
E, product reclaim:
Step D high performance preparative liquid chromatography is separated the dehydrogenation two isoeugenol monomer solution heating recovery methyl alcohol that obtain, dehydrogenation two isoeugenols can be separated out into cotton-shaped crystal in remaining liq, filter with funnel, the cotton-shaped crystal of gained places into that baking oven is drying to obtain dehydrogenation two isoeugenol monomer products for 55 ℃.
The invention has the advantages that:
1, step is few, and weak point consuming time can shorten the production cycle greatly, saves production cost.
2, solvent consumption is few, and the solvent in the preparative liquid chromatography separating step is recyclable recycling all.
3, the dehydrogenation two isoeugenol monomer purity height that make reach more than 99.5%, and the reference substance that can be used as assay uses.
4, good in economic efficiency, can carry out scale operation, and operation is easy, be easy to control, the separation efficiency height.
Description of drawings
Fig. 1 is the HPLC collection of illustrative plates of the embodiment of the invention 1 product
Fig. 2 prepares the liquid phase collection of illustrative plates for the embodiment of the invention 1 step D.
Embodiment
The present invention is described in further detail below in conjunction with embodiment.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment.
Among following each embodiment, the purity of finished product dehydrogenation two isoeugenol monomers is rechecked and is all adopted anti-phase analysis mode liquid chromatography (RP-HPLC) method, and chromatographic condition is as follows:
Be weighting agent with the octadecylsilane chemically bonded silica; With methyl alcohol: water (75:25) is moving phase; 30 ℃ of column temperatures; Flow velocity 1.0ml/min; Detecting wavelength is 274 nm.
Embodiment 1
A kind of separation purification method of dehydrogenation two isoeugenol monomers, it be with the Semen Myristicae be that raw material extracts, extraction, silicagel column separates and preparation is reclaimed and got, its concrete processing step is as follows:
A, extraction:
The Semen Myristicae 1kg of drying is ground into meal, pack in the extractor of volume 10L, the adding mass percent concentration is 95% ethanolic soln 8L, heating and refluxing extraction is extracted 3 times altogether, each 3 hours, extracting liquid filtering, merge filtered liquid, concentrate and reclaim ethanol, get concentrated extract and treat that next step carries out extraction treatment;
B, extraction:
The water (80 ℃) that adds 1 times of volume in the medicinal extract of steps A gained dilutes, altogether solution 1.6L, the ethyl acetate extraction that adds equivalent volumes, coextraction 3 times, merge and collect ethyl acetate layer, in 55 ℃ of rotatory evaporators, be recycled to the medicinal extract shape, add 60～80 order silica gel (50 gram) of 5 times of weight of gained medicinal extract, mix after the sample drying silica gel sample 60 grams;
C, silicagel column separate:
Take by weighing 600g 200～300 order silica gel, with sherwood oil (60-90 ℃): the eluent that ethyl acetate (6:1) is formed is mixed thoroughly, pack in the glass chromatography column of the high 70cm of diameter 10cm that gets ready, with sherwood oil (60-90 ℃): the eluent sedimentation that ethyl acetate (6:1) is formed, till the constant flow rate; With dry good silica gel sample 62 grams among the step B, pack in the chromatography column, use sherwood oil (60-90 ℃): the eluent wash-out that ethyl acetate (6:1) is formed, detect collection dehydrogenation two isoeugenol product sections according to TLC, reclaim eluent, get white shape solid 1.8 grams;
Described eluent is made up of by the 6:1 volume ratio sherwood oil (60-90 ℃) and ethyl acetate.
D, high performance liquid phase preparation:
The DMF that gets the 1.8g white solid adding 18mL of step C gained fully dissolves, remove by filter insoluble impurities, filtrate sample introduction, UV-detector on-line monitoring, specific aim is collected the preparation cut solution of dehydrogenation two isoeugenol monomers, gets dehydrogenation two isoeugenol monomer solutions;
It is the chromatographic column of octadecylsilane chemically bonded silica (C18) that described high performance liquid phase separates the employing filler, and the post specification is 50cm * 8cm; Moving phase consists of: methyl alcohol: water (volume ratio)=75:25; The detection wavelength is 274nm; Operate under the room temperature.
E, product reclaim:
Step D high performance preparative liquid chromatography is separated the dehydrogenation two isoeugenol monomer solutions that obtain be concentrated into no methyl alcohol for 55 ℃ with vacuum rotary steam, the white cotton-shaped crystal that dehydrogenation two isoeugenol monomers are separated out at the residue aqueous phase, filter collecting precipitation with funnel, dehydrogenation two isoeugenol products are placed into 55 ℃ of dryings in the baking oven, obtain dehydrogenation two isoeugenol monomer products 1.1 grams after the oven dry.
About 5 days of whole production flow process time spent.
Calculating product yield is (1.1/1000) * 100%=0.11%.
By changing the moving phase component, utilize anti-phase analysis mode liquid chromatography (RP-HPLC) to recheck product purity, recording the result is 99.56%.
Embodiment 2
A kind of separation purification method of dehydrogenation two isoeugenol monomers, it be with the Semen Myristicae be that raw material extracts, extraction, silicagel column separates and preparation is reclaimed and got, its concrete processing step is as follows:
A, extraction:
The Semen Myristicae 10kg of drying is ground into meal, pack in the extractor of volume 100L, the adding mass percent concentration is 95% ethanolic soln 80L, heating and refluxing extraction 3 times, each 3 hours, extracting liquid filtering merged filtered liquid, concentrate and reclaim ethanol, get pending next step extraction treatment of 10L concentrated extract;
B, extraction:
The water (80 ℃) that adds 10L in the medicinal extract of steps A gained dilutes, altogether solution 20L, the ethyl acetate extraction that adds equivalent volumes (20L), coextraction 3 times, merge and collect ethyl acetate layer, concentrate in 55 ℃ of rotatory evaporators and be recycled to the medicinal extract shape, the 60-80 order silica gel (775 gram) that adds 5 times of weight of medicinal extract is mixed dry silica gel sample 930 grams that get of sample;
C, silicagel column separate:
Take by weighing 9.3kg 200-300 order silica gel with sherwood oil (60-90 ℃): ethyl acetate (6:1) is mixed thoroughly, pack into 3 in the glass chromatography column of the high 120cm of diameter 15cm that gets ready, with sherwood oil (60-90 ℃): ethyl acetate (6:1) sedimentation, till the constant flow rate; With dry good silica gel sample 930 grams among the step B, divide in 3 batches of chromatography columns of evenly packing into, with sherwood oil (60-90 ℃): ethyl acetate (6:1) wash-out, detect collection dehydrogenation two isoeugenol product sections according to TLC, reclaim sherwood oil (60-90 ℃): ethyl acetate (6:1), get white shape solid 24 grams, treat next step preparation.
D, high performance liquid phase preparation:
Adopting filler is octadecylsilane chemically bonded silica (C
18) chromatographic column, the post specification is 50cm * 10cm;
Moving phase consists of: methyl alcohol: water (75:25).
The detection wavelength is 274nm; Operate under the room temperature.
The DMF that gets the 24g white solid adding 240ml of step C gained fully dissolves, remove by filter insoluble impurities, filtrate sample introduction, UV-detector on-line monitoring, specific aim is collected the preparation cut solution of dehydrogenation two isoeugenol monomers, gets dehydrogenation two isoeugenol monomer solutions.
E, product reclaim;
Step D high performance preparative liquid chromatography is separated the dehydrogenation two isoeugenol monomer solutions that obtain be concentrated into no methyl alcohol for 55 ℃ with the decompression rotatory evaporator, sample is separated out white cotton-shaped crystal at the residue aqueous phase, filter collecting precipitation with funnel, place 55 ℃ of dryings in the baking oven, namely obtain dehydrogenation two isoeugenol monomer products, obtain product 13.8 grams after the oven dry.
About 15 days of whole production flow process time spent.
Calculating product yield is (13.8/10000) * 100%=0.138%.
By changing the moving phase component, utilize anti-phase analysis mode liquid chromatography (RP-HPLC) to recheck product purity, recording the result is 99.68%.
Claims (2)
1. the separation purification method of dehydrogenation two isoeugenol monomers, it be with the Semen Myristicae be that raw material extracts, extraction, silicagel column separates and preparation is reclaimed and got, and it is characterized in that concrete processing step is as follows:
A, extraction:
The ground nutmeg of drying is broken into meal, be that to add mass percent concentrations be 95% ethanolic soln for 1:8～10 by medicinal material weight and ethanol volume ratio, heating and refluxing extraction, extract 3 times, each 2～3 hours, extracting liquid filtering merged filtered liquid, concentrate and reclaim ethanol, get concentrated extract and treat that next step carries out extraction treatment;
B, extraction:
Volume in the concentrated extract of steps A gained adds 80 ℃ of long-pending water dilutions of monoploid, add again with dilution after the long-pending ethyl acetate extraction of medicinal extract aqueous solution monoploid, coextraction 3 times, merge and collect ethyl acetate layer, be concentrated into fluid extract for 55 ℃ with revolving the steaming vaporizer, the dry silicagel column that is equipped with of 60～80 order silica gel mixed samples that adds 5 times of weight of gained fluid extract weight separates;
C, silicagel column separate:
Mix all product weight according to step B gained, take by weighing 200～300 order silica gel of 10 times of weight, mix thoroughly in the glass chromatography column of packing into eluent, use the eluent sedimentation, till the constant flow rate; With dry good silica gel sample among the step B, in the glass chromatography column of packing into, use the eluent wash-out, detect according to TLC and collect dehydrogenation two isoeugenol product sections, reclaim eluent, get white cotton-shaped solid;
D, high performance liquid phase preparation separate:
Get the solid of step C gained, press the dissolving of 1g:10ml solution, filter with dimethyl formamide, the preparation of carrying out dehydrogenation two isoeugenol monomers separates the UV-detector on-line monitoring, specific aim is collected the preparation cut solution of dehydrogenation two isoeugenol monomers, gets dehydrogenation two isoeugenol monomer solutions;
E, product reclaim:
Step D high performance preparative liquid chromatography is separated the dehydrogenation two isoeugenol monomer solutions that obtain, utilize rotatory evaporator to recycle methyl alcohol, the cotton-shaped crystal that dehydrogenation two isoeugenol products can be separated out at the residue aqueous phase, filter with funnel, filtering product places into that baking oven is drying to obtain dehydrogenation two isoeugenol monomer products for 55 ℃;
It is the chromatographic column of C18 that the described high performance liquid phase of step D separates the employing filler; Moving phase consists of: by volume, methyl alcohol: water=75:25, the detection wavelength is 274nm.
2. the separation purification method of dehydrogenation two isoeugenol monomers as claimed in claim 1, it is characterized in that: the described eluent of step C is made up of by the 6:1 volume ratio 60-90 ℃ sherwood oil and ethyl acetate.
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| CN111991387B (en) * | 2020-10-10 | 2022-05-10 | 上海中医药大学 | Application of dehydrodiisobutyrol in preparing medicine for preventing and treating ulcerative colitis |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101637484A (en) * | 2009-09-08 | 2010-02-03 | 青海大学 | Active extract for sanwei sandalwood as well as extraction method and medical application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101637484A (en) * | 2009-09-08 | 2010-02-03 | 青海大学 | Active extract for sanwei sandalwood as well as extraction method and medical application thereof |
Non-Patent Citations (2)
| Title |
|---|
| "肉豆蔻的化学成分";李秀芳等;《沈阳药科大学学报》;20061130;第23卷(第11期);698-701，734 * |
| 李秀芳等."肉豆蔻的化学成分".《沈阳药科大学学报》.2006,第23卷(第11期),698-701，734. |
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