CN105315118A - Integrated extracting and separating method for active ingredients of Chinese stellera roots - Google Patents

Integrated extracting and separating method for active ingredients of Chinese stellera roots Download PDF

Info

Publication number
CN105315118A
CN105315118A CN201510414030.1A CN201510414030A CN105315118A CN 105315118 A CN105315118 A CN 105315118A CN 201510414030 A CN201510414030 A CN 201510414030A CN 105315118 A CN105315118 A CN 105315118A
Authority
CN
China
Prior art keywords
extraction
stellera chamaejasme
ethyl acetate
extract
dry
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.)
Pending
Application number
CN201510414030.1A
Other languages
Chinese (zh)
Inventor
李玉山
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.)
Individual
Original Assignee
Individual
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 Individual filed Critical Individual
Priority to CN201510414030.1A priority Critical patent/CN105315118A/en
Publication of CN105315118A publication Critical patent/CN105315118A/en
Pending legal-status Critical Current

Links

Landscapes

  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)

Abstract

The invention relates to an integrated extracting and separating method for active ingredients of Chinese stellera roots. The method comprises the following steps that firstly, Chinese stellera roots are extracted, concentrated and added with water for dispersion; secondly, a concentrated solution is subjected to petroleum ether extraction, and chromatographic separation is carried out; thirdly, residual liquid obtained after petroleum ether extraction is subjected to diethyl ether extraction, and chromatographic separation is carried out; fourthly, residual liquid obtained after diethyl ether extraction is subjected to chloroform extraction, and chromatographic separation is carried out; fifthly, residual liquid obtained after chloroform extraction is subjected to ethyl acetate extraction, and chromatographic separation is carried out; sixthly, residual liquid obtained after ethyl acetate extraction is subjected to acetone extraction, and chromatographic separation is carried out. According to the method, one or more kinds of high-polarity mixed solvents are adopted for extracting and concentrating the active ingredients of Chinese stellera roots synchronously, extract of a mixture of all the ingredients is obtained, then the corresponding ingredients are extracted through solvents of different polarities according to the similarity and intermiscibility principle, and all monomer ingredients are obtained with the combination of different chromatographic separation methods. The technology is novel, unique and suitable for industrial production.

Description

The integrated extraction and separation method of Stellera chamaejasme L. effective constituent
Technical field
The present invention relates to the integrated extraction and separation method of Stellera chamaejasme L. effective constituent.
Background technology
Stellera chamaejasme L. (StellerachamaejasmeLimt), have another name called the root of langdu, Graceful Jessamine Herb, steamed bun flower etc., cover Da Lintugu by name, reach stupefied figure as, emerging, the hot first bar of few lattice, Re Zhage.It is the dry root of thymelaeceae (Thymelaeaceae) stellera (Stelleralinn) perennial herb poisonous plants.All have wild in China's most area, be distributed widely in meadow and the high mountain area without shade in northwest, the Inner Mongol, Heilungkiang, northeast, northwest, Qinghai, Tibet etc. area.This kind of plant about have recorded 50 genus in the whole world, about kind more than 500, all on the books in " Jingzhubencao ", Shennong's Herbal, " the positive allusion quotation of anaesthetic ", " Chinese medicine encyclopedia traditional Mongolian medicine ", " recognizing medicine Bai Jingjian ", " errorless anaesthetic mirror ", " anaesthetic ", " Inner Mongol anaesthetic material standard ".The traditional Chinese medical science is thought, its nature and flavor hardship is flat, and very toxic, having relieves oedema or abdominal distension through diuresis or purgation eliminates the phlegm, effect of broken long-pending desinsection.Have high rushing down, kill " gluing ", disappear " very breathe out ", only rotten, effect of detumescence, clinical in flesh, bone, arteries and veins " very Kazakhstan " disease, and erysipelas, acute mastitis, the cheek swell (parotitis), impetigo, variola.Its root is thick, cylindrical, the tough not frangibility of matter, section adularescent villus fiber, and this plant application is with a long history, is the certified products of Chinese medicine " root of langdu ".Stellera chamaejasme L. root system is flourishing, and Drought hardiness is strong, and reproduction speed is fast, not only reduce the seed output and quality on grassland, even cause grassland big area to degenerate in certain areas such as Qinghai, causing serious impact and threat to China's grassland ecosystem, is the grassland poisonous weeds that a kind of urgent need is prevented and kill off [1-8].
The chemical composition of Stellera chamaejasme L. has: 1. coumarins: Liu Gui virtue in 1996, Soviet Union scholar Tikhomirova in 1974, Mongolian scholar Narantuyaa in 1994, the former Russian scholar Modonova in 1985 is separated respectively and obtains sphondin (sphondin) (6-methoxyl group Sodium Ferulate), isobergapten, vakerine (pimpinelline), Isopimpinellin (isopimpinelline), coumarin glycoside, Umbelliferone-7-O-β-D-xylopyranosyl-β-D-glycopyranoside, umbelliferone, Daphnelin, new Daphnetin, different Fructus Citri Sarcodactylis propyl ester (isobergapten), Umbelliferone (umbelliferone umbelliferone), Raven's Test (daphnoritin), pimpinellin (pimpinllin), different pimpinellin (isopimpinllin), daphnetin (daphnetin), Scopoletin (scopoletin), daphnoretin (daphnoretin), daphnin (daphini), 5,7-dihydroxycoumarin, dephnin (daphnin) (5,7-dihydroxycoumarin), daphnoretin-7-O-glucoside (chamaejasmoside), Isodaphnoretin (isodaphnoretin), Isodaphnoretin B (isodaphnoretinB), 7-methoxyl group daphnoretin (7-methoxydaphnoretin).2. flavonoid: Yang Wei's literary composition in 1984, Japanese scholars MasatakeNiwa between 1984-1986, scholar Ikegawa, nineteen ninety-five Liu Gui virtue, Jin in 1999, Soviet Union scholar Rezanova in 1976, Jin Changdong etc. are separated to obtain 7-methoxyl group chamajasmin respectively, 7-methoxyl group root of langdu A (7-methoxychamaejasmin), Stellera chamaejasme L. element A ', B, 4 ', 4,5,5 ", 7,7 "-hexahydroxy--3,3 "-biflavones, chamajasmin (chamaejasmine) (A, B, C, D), methyl-derivatives (the A of chamajasmin, B, C), different chamajasmin (isochamejasmin), new stellerin (A, B) (neochamaeJasminAandB), wild goose skin element A, C (sikokianinA, C), different new stellerin A (isoneochamaejasminA), excellent chamajasmin (A, B, C) (euchamaejasmineA, B, C), different chamajasmin B (isochamaejasmineB), different wild goose skin element A (isosikokianinA), different chamajasmin and (+)-chamajasmin, winter daphne phenol, (-)-Biao loquat element-7-O-β-D-glucopyranoside, stelleranol, (+)-Biao loquat element, wikstromol (A, B), apiolin (apigenin), Quercetin (quercetin), violaguercitrin (rutin), Dihydrokaempferol (dihydrokaempferol), dihydro Daphnetin second (dihydrodaphnodorinB), Daphnetin second (daphnodorinB), 3 ', 14-dimethyl-4 ', 11-dimethoxy-5,7-dihydroxy-benzene a pair of horses going side by side flavanone, Stellera chamaejasme chromone (chamaechromone), mohsenone, chromone derivative I somohsenone, Dihydrokaempferol (dihydrokaempferol), Stellera chamaejasme L. A, B (ruixianglangduA, B), the new A of 7-methoxyl group wolf (7-methoxyneochamaejasmineA), 3 ', 14-dimethyl-4 ', 11-dimethoxy-5,7-dihydroxy-benzene a pair of horses going side by side dihydro Huang (3 ', 14-dimethyl-4 ', 11-dimethoxy-5,7-Dihydroxybenzoflavanone), (-)-Biao loquat element-7-O-β-D-glucopyranoside ((-)-epiafzelechin-7-O-β-dglucopyranoside), stelleranol, (+)-Biao loquat element ((+)-epiafzelechin), wikstromol A, B (wikstrolA, B).3. diterpenes: 1991-1992 Feng Wei is good for, 1993 and IkekawaTTetsuro in 1996, BudoYuichi in 1997 etc., Niwa etc., Yoshida etc., Ikegawa etc. are separated respectively and obtain huratoxin, Saab toxin A, simplexin, tool anti-leukocythemia liveness have simplexin (simplexin) pimeleafactorP2, the daphane diterpene of unsaturated fatty acids acylating acid, Diterpenoid epoxide class Buddhist nun morpholine (gnidimacrin) of tool anti-tumor activity, Stellera chamaejasme L. is appointed (stelleramacrin) (A, B), new auspicious plain neostellerin (A, B, C), diterpene-kind compound neostellin, 12-acetoxyl group He Lei toxin (subtoxinA), reddish brown thunder toxin (huratoxin), wherein the active Buddhist nun's morpholine of antitumour activity and anti HIV-1 virus the most significantly, its antitumour activity outline is higher than vincristine(VCR) and Zorubicin.4. lignanoids: Ikegawa in 1994, 1999 annuities are often eastern, Japanese scholars TatematsuHiroshi in 1985, IkegawaTetsuo in 1994 respectively sub-argument obtains greenhartin F, lariciresinol B (clemastaninB), Arctiin (arctiin), magnolenin C, lirioresinol B (lirioresinolB), rosin spirit (pinoresinol), Podocarpus macrophyllus resinol (matairesinol), kusunokinin, rosin spirit monomethyl ether, isohinokinin, ilemastaninB, pine resin diethylene glycol dimethyl ether (eudesmin), gumbolimbo fat element (bursehernin), pine tree lipidol, matairesinol (matairesino), the Eudesmin (eudesmin) of the anticancer anti HIV-1 virus effect of tool, coniferinoside, Radix Et Caulis Acanthopanacis Senticosi glucoside (syringin), syringinosidesinapylalc-1,3-diglucopyranoside, 4-(-β-D-glucopyranosyloxy-1-E-propenyl-2, 6-dimethoxyphenyl-6-O-β-D-glucopyranosyl-β-D-glucopyranoside and 4-(3-hydroxy-1-Z-propenyl)-2,6-dimethoxyphenyl-6-D-glucopyranosyl-β-D-GlucopYranoside, bursehernin, (-)-pinoresinolmonomethylether, kusunokinin, magnoleninC, (+)-matairesinol, (-)-eudesmin, greenhartin F (lappaolF), clemastaninB, there is the eudesmin of antivirus action.5. volatile oil: mainly contain octanal, phenylcarbinol, octanol, beta-myrcene, neral, vernol, 5-methyldecane, capraldehyde, 3,7,11-trimethylammonium 12 carbon α-trans-6,6-is along 10-enol, 3,7,11-trimethylammonium 12 carbon α-trans-6, O-is along three enols, NSC 77136, Palmitic acid methyl esters, Palmitic acid ethyl ester, Palmitic acid, 7,10-octadecadienoic acid methyl esters, 18 methyl carbonates, farnesol, 10,13-18 dienoic acid methyl ester, diazanyl formyl diphenylamine N-, methyl phenyl ketone, palmitinic acid, adjacent hydroxymethylbenzaldehyde, 9-methyl-8-pentadecylenic acid, undecane, the tetradecane, 1,5-phenylbenzene-2-alkene-1-pentanone, TRANSCINNAMIC ACID, positive 20 diester of Hydroxycinnamic acid, 4-ethoxybenzoic acid, (+)-5,7,4 '-trihydroxy-flavan-3-alcohol, 2,6-dimethoxy para benzoquinone, N, N-dimethyl-ASPARTIC ACID, S-(+)-3-hydroxyl-1,5-phenylbenzene-1-pentanone, 3,7,17-trimethylammonium 12 carbon-trans-2, cis-6,10-triolefins (3,7,17-trimethyl-trans-2, cis-6,10-dodecatrienol), 10,13-octadecadienoic acid first (methyl-10,13-oc-tadecadienoate), n-tridecane (n-tridecane), n-dodecane (n-dodecane), 2,6-dimethyl heptane (2,6-dimethylheptanes), anise coumarin (pimpinellin), different bergapten (isober-gapten), 1-phenmethyl propanedione-1,2, octane, Chinese cassia tree phenol, 2,6-dimethyl heptane, 2,6-dimethyl octane, 2,5-dimethyl dodecyl, 7,10-18 dienoic acid methyl ester, the trans-6-of 3,7,11-trimethylammonium 12 carbon-2-cis-10-tri-enol, S-(+)-3-hydroxyl-1,5-phenylbenzene-1-pentanone, 1,5-phenylbenzene-2-alkene-1-pentanone (1,5-diphenyl-2-penten-1-one), 1,5-phenylbenzene-1-pentanone (1,5-diphenyl-1-pentanon), positive 22 (p-coumaricacidn-eicosanylester), positive 20 esters (caffeicacidn-dueicosanylester) of coffic acid, Hydroxycinnamic acid (p-hydroxycinnamicacid) and sulphur eight (sulfur-8) [9-49]
Sphondin (Sphondin) Chinese name: 6-methoxyl group Sodium Ferulate, CASNo.483-66-9, C 12h 8o 4, molecular weight: 216.2, H-Furo (2,3-h)-1-benzopyran-2-one, 6-methoxy-Sphondin.Structural formula is as follows:
Isobergapten (Isobergapten) Chinese name: 5-MOP, 4-methoxyl group-7H-furans chromene-7-ketone, molecular formula: C 12h 8o 4, molecular weight: 216.18952, CASNo.482-48-4,5-Benzofuranacrylicacid, 4-hydroxy-6-methoxy-, d-lactone (7CI); Isobergapten (6CI); 5-Methoxyangelicin; 5-methoxyfuro [2,3-h] chromen-2-one2H-Furo [2,3-h]-1-Benzopyran-2-one.White crystalline powder, has anti-inflammatory, analgesic activity.Structural formula is as follows:
Isopimpinellin (Isopimpinellin) has another name called: Isopimpinellin, pimpinellin, isopimpinellin, isopimpinellin, molecular formula: C 13h 10o 5, molecular weight: 246.22, CASNo.482-27-9,7H-Furo [3,2-g] [1] Benzopyran-7-one, 4,9-dimethoxy5,8-Dimethoxypsoralen (e) Dimethoxy-7H-furo [3,2-g] chromen-7-one.Light yellow crystal, m.p.148-151 DEG C, anti-tumor activity, has restraining effect to the propagation of HeLa cell.Structural formula is as follows:
Umbelliferone (umbelliferone) has another name called: Umbelliferone, umbelliferone, 7-hydroxyl-2H-1-chromen-2-one, molecular formula: C 9h 6o 3, molecular weight: 162.14, CASNo.93-35-6, MDLNo.MFCD00006878, EINECSNo.202-240-3, RTECSNo.GN6820000, BRNNo.127683, PubChemNo.24889947.7-Hydroxy-2H-1-benzopyran-2-oneButylidene-4，5-dihydro-3H-isobenzofUran-1-one。White, needle-shaped crystals, has tonka bean camphor smell during heating, can distil, and between 90-130 DEG C, carry out condensation in the presence of sulphuric acid by 2,4-dihydroxyacetophenone and oxysuccinic acid, namely cancellation ethanoyl obtains Umbelliferone.M.p.225-228 DEG C, 1g are dissolved in about 100mL boiling water, are dissolved in ethanol, chloroform, acetic acid, are dissolved in diluted alkaline and are blue-fluorescence, are slightly dissolved in ether.There is antibacterial, step-down, anticancer, calm and spasmolysis.Structural formula is as follows:
Daphnetin (Daphnetin) has another name called: daphnetin, Daphnelin (7,8-Dihydroxycoumarin), daphnetin-7-methyl esters, daphnetin, daphnetin daphnetin, daphnetin.Molecular formula: C 9h 6o 4, CASNo.486-35-1, EINECSNo.207-632-8,7,8-Dihydroxy-2h-1-Benzopyran-2-One7,8-Dihydroxy-Chromen-2-One7,8-Dihydroxycoumarin.This product is off-white color or pale powder, and odorless is tasteless.Slightly soluble in methyl alcohol, ethanol, insoluble in water.Tool step-down, cardiac stimulant, antithrombotic shape, anticoagulant, reducing blood-fat, analgesia, tranquilizing soporific, anticonvulsion, anti-inflammatory, antimalarial, killing aphis, antibacterial, diarrhea, anti-hypoxia, arrestin kinases, reduce glutamate induction necrocytosis, improve neural function, reduce the area of cerebral infarction and the provide protection to cerebral ischemia.For thromboangiitis obliterans, coronary heart disease and angina pectoris, analgesic activity and arthritic treatment.Structural formula is as follows:
Daphnoretin ((Daphnoretin, Thymelol) molecular formula: C 19h 12o 7molecular weight: 352.297, CASNo.2034-69-72, H-1-Benzopyran-2-one, 7-hydroxy-6-methoxy-3-[(2-oxo-2H-1-benzopyran-7-yl) oxy]-Coumarin, 7-hydroxy-6-methoxy-3,7 '-oxydi-(7CI, 8CI) NSC29185.Tool is antitumor, anti-inflammatory, antimycotic, antiviral, angst resistance effect, is with a wide range of applications as potential new drug or structural modification parent nucleus.Micro-yellow wool shape fine needle crystalline substance or tubbiness yellow needles m.p.250-252 DEG C.Structural formula is as follows:
Chamajasmin (Chamaejasmin, Chamaejasmine) molecular formula: C 30h 22o 10, CASNo.69618-96-8 [3,3 '-Bi-4H-1-benzopyran]-4,4 '-dione, 2,2 ', 3,3 '-tetrahydro-5,5 ', 7,7 '-tetrahydroxy-2,2 '-bis (4-hydroxyphenyl)-, (2R, 2 ' R, 3S, 3 ' S)-rel-.Structural formula is as follows:
Different chamajasmin (Isochamaejasmin) molecular formula: C 30h 22o 10, molecular weight: 542, CASNo.93859-63-3, (2R, 2 ' S, 3S, 3 ' R)-rel-2,2 ', 3,3 '-Tetrahydro-5,5 ', 7,7 '-tetrahydroxy-2,2 '-bis (4-hydroxyphenyl)-[3,3 '-bi-4H-1-benzopyran]-4,4 '-dione, amorphous powder, suppresses ornithine decarboxylase and Protein kinase C activation effect, suppresses the tumor promotion caused by teleocidin.Structural formula is as follows:
New stellerin A (NeochamaeiasminA) molecular formula: C 30h 22o 10, molecular weight: 542.5, CASNo.90411-13-5, [3, 3 '-Bi-4H-1-benzopyran]-4, 4 '-dione, 2, 2 ', 3, 3 '-tetrahydro-5, 5 ', 7, 7 '-tetrahydroxy-2, 2 '-bis (4-hydroxyphenyl)-, (2R, 2 ' R, 3R, 3 ' R)-rel-(+)-[3, 3 '-Bi-4H-1-benzopyran]-4, 4 '-dione, 2, 2 ', 3, 3 '-tetrahydro-5, 5 ', 7, 7 '-tetrahydroxy-2, 2 '-bis (4-hydroxyphenyl)-, [2a, 3a (2 ' R*, 3 ' R*)]-(+)-, (+)-, m.p.278 DEG C.Suppress ornithine decarboxylase and Protein kinase C activation effect, have the tumor promotion suppressed caused by teleocidin.Structural formula is as follows:
Scopoletin (Buxuletin, Scopoletin, Murrayetin, Scopoletine, Escopoletin, Scopoletol, Chrysatropicacid) molecular formula: C 10h 8o 4, molecular weight: 192.17, CASNo.92-61-5, EINECSNo.202-171-9, structural formula is as follows:
Dephnin (Daphnoside) has another name called: 2,6-dimethoxy-naphthalene, Daphne giraldii Nitsche's B prime, molecular formula: C 15h 16o 9, CASNo.486-55-5, EINECSNo.226-816-9, H-1-Benzopyran-2-one, 7-(b-d-glucopyranosyloxy)-8-hydroxycoumarin.Structural formula is as follows:
Crepitin (huratoxin, StelleramacrinB) has another name called: reddish brown thunder toxin, huratoxin, molecular formula: C 34h 48o 9, CASNo.150216-83-4,6H-2,8b-Epoxyoxireno [6,7] azuleno [5,4-e]-1,3-benzodioxol-6-one, 3a, 3b, 3c, 4a, 5,5a, 8a, 9,10,10a-decahydro-5,5a, 10-trihydroxy-4a-(hydroxymethyl)-7,9-dimethyl-10a-(1-methylethenyl)-2-(1E, 3E)-1,3-tridecadieny1-, (2S, 3aR, 3bS, 3cS, 4aR, 5S, 5aS, 8aR, 8bR, 10aS)-[partial]-.Structural formula is as follows:
Simplexin (simplexin, pimeleafactorP2) has another name called: 18-removes-(benzoyloxy)-28-deoxidation Ge Nidi wood times, DaphnopsisfactorR3, PimeleafactorP1, WikstrotoxinD).Molecular formula: C 30h 44o 8, CASNo.1404-62-2.6H-2，8b-Epoxyoxireno[6，7]azuleno[5，4-e]-1，3-benzodioxol-6-one，3a，3b，3c，4a，5，5a，8a，9，10，10a-decahydro-5，5a-dihydroxy-4a-(hydroxymethyl)-7，9-dimethyl-10a-(1-methylethenyl)-2-nonyl-，(2S，3aR，3bS，3cS，4aR，5S，5aS，8aR，8bR，9R，10aR)-。Structural formula is as follows:
Gnidimacrin (Gnidimacrin) has another name called: gnidimacrin, Buddhist nun's morpholine.Molecular formula: C 44h 54o 12, molecular weight 775.36, CASNo.60796-70-5.[1R-(1R*，2R*，4S*，4aR*，6S*，7R*，14R*，14aS*，15S*，16S*，16aS*，16bR*，17S*，17aR*，18aS*，18bS*)]-4-[(benzoyloxy)methyl]eicosahydro-7，16a，17-trihydroxy-17a-(hydroxymethyl)-14，15-dimethyl-2-(1-methylethenyl)-2H-1，6：2，6-diepoxybenz[7.8]oxirino[5，6]azuleno[8，1-bc]oxacyclotridencin-16-ylbenzoate。Structural formula is as follows:
Lirioresinol A dme (Epiyangambin) has another name called: O, O-dimethyl lirioresinol A, molecular formula: C 24h 30o 8, molecular weight: 446.4902, CASNo.24192-64-1, (1S)-1 β, 4 α-Bis (3,4-dimethoxyphenyl)-3a β, 4,6,6a β-tetrahydro-1H, 3H-furo [3,4-c] furan; (1S, 3a β, 6a β)-1 β, 4 α-Bis (3,4-dimethoxyphenyl) tetrahydro-1H, 3H-furo [3,4-c] furan; (1S, 3a β, 6a β)-Tetrahydro-1 β, 4 α-bis (3,4-dimethoxyphenyl)-1H, 3H-furo [3,4-c] furan.Structural formula is as follows:
Lirioresinol B dme (Yangabin, (+)-Yangambin, LirioresinolB) molecular formula: C 24h 30o 8, molecular weight: 446.49000, CASNo.13060-14-5, (+)-O, O-DimethyllirioresinolB; (1S)-1 β, 4 β-Bis (3,4,5-trimethoxyphenyl)-3a β, 4,6,6a β-tetrahydro-1H, 3H-furo [3,4-c] furan; (1 β, 5 β)-2 β, 6 β-Bis (3,4,5-trimethoxyphenyl)-3,7-dioxabicyclo [3.3.0] octane; [1S, (+)]-3a β, 4,6,6a β-Tetrahydro-1 β, 4 β-bis (3,4,5-trimethoxyphenyl)-1H, 3H-furo [3,4-c] furan.Structural formula is as follows:
Lirioresinol A (LirioresinolA, Syringaresinol, Episyringaresinol), molecular formula: C 22h 26o 8, molecular weight: 418.44, CASNo.24192-64-1,1H, 3H-Furo [3,4-c] furan, 3aa, 4,6,6aa-tetrahydro-1a, 4b-bis (3,4,5-trimethoxyphenyl)-(8CI); 1H, 3H-Furo [3,4-c] furan, tetrahydro-1,4-bis (3,4,5-trimethoxyphenyl)-, [1S-(1a, 3aa, 4b, 6aa)]-; LirioresinolA, O, O-dimethyl-; O, O-DimethyllirioresinolA.Structural formula is as follows:
Lirioresinol B (Syringaresinol, LirioresinolB) has another name called: syringaresinol, syringaresinol, syringaresinol.Molecular formula: C 22h 26o 8, CASNo.21453-69-0, Phenol, 4,4 '-(3aa, 4,6,6aa-tetrahydro-1H, 3H-furo [3,4-c] furan-1a, 4a-diyl) bis [2,6-dimethoxy-(8CI) Phenol, 4,4 '-(tetrahydro-1H, 3H-furo [3,4-c] furan-1,4-diyl) bis [2,6-dimethoxy-, [1S-(1a, 3aa, 4a, 6aa)]-; 1H, 3H-Furo [3,4-c] furan, phenolderiv.Structural formula is as follows:
Podocarpus macrophyllus resinol (-Matairesinol) molecular formula: C 20h 22o 6, molecular weight: 358.39, CASNo.580-72-3,2 (3H)-Furanone, dihydro-3,4-bis [(4-hydroxy-3-methoxyphenyl) methyl]-, (3R-trans)-; 2 (3H)-Furanone, dihydro-3,4-divanillyl-(8CI).
Arhat rosin glycosides (Matairesinoside) molecular formula: C 26h 32o 11cASNo.23202-85-92 (3H)-Furanone, 3-[[4-(b-D-glucopyranosyloxy)-3-methoxyphenyl] methyl] dihydro-4-[(4-hydroxy-3-methoxyphenyl) methyl]-, (3R-trans)-.Structural formula is as follows:
Matairesinol (Matairesinol) molecular formula: C 20h 22o 6, molecular weight: 358.39, CASNo.580-72-3,2 (3H)-Furanone, dihydro-3,4-bis [(4-hydroxy-3-methoxyphenyl) methyl]-, (3R-trans)-; 2 (3H)-Furanone, Dihydro-3,4-divanillyl-(8CI).Structural formula is as follows:
Methyl arctigenin-4'-gentiobioside (Methylarctigenin) has another name called: methyl arctigenin, molecular formula: C 22h 26o 6molecular weight: 386.44, CASNo.25488-59-9,2 (3H)-Furanone, 3,4-bis [(3,4-dimethoxyphenyl) methyl] dihydro-, (3R, 4R)-2 (3H)-Furanone, dihydro-3,4-diveratryl-, trans-(8CI); (-)-Arcitin; (-)-Maculatin.Structural formula is as follows:
Eudesmin (Eudesmin) molecular formula: C 22h 26o 6, CASNo.526-06-7,1H, 3H-Furo [3,4-c] furan, Isosorbide-5-Nitrae-bis (3,4-dimethoxyphenyl) tetrahydro-, (1R, 3aS, 4R, 6aS)-1H, 3H-Furo [3,4-c] furan, 1a, 4a-bis (3,4-dimethoxyphenyl)-3aa, 4,6,6aa-tetrahydro-.Structural formula is as follows:
Japan cypress alicyclic lactone (Hinokinin, Isohinokinin) has another name called: hinokinin, molecular formula C 20h 18o 6, molecular weight 354.35332, CASNo.103063-07-62, (3H)-Furanone, 3,4-bis (1,3-benzodioxol-5-ylmethyl) Dihydro-, (3S-cis)-; 2 (3H)-Furanone, dihydro-3,4-dipiperonyl-, cis-(8CI); Heliobuphthalminlactone, (3R, 4R)-type is separated out as plate crystal m.p.64-65 DEG C in ethanol or benzene.Specific rotation 33.7 °.(3S, 4S)-type is prismatic crystallization, m.p.64-65 DEG C ,+32.4 ° (chloroform).(3RS, 4RS)-type, m.p.108 DEG C, insecticidal synergistic.Structural formula is as follows:
Dihydrohibalactone, molecular formula: C 20h 18o 6, molecular weight: 354.35332, CASNo.26543-90-82 (3H)-Furanone, 3,4-bis (1,3-benzodioxol-5-ylmethyl) dihydro-, (3S-cis)-; 2 (3H)-Furanone, dihydro-3,4-dipiperonyl-, cis-(8CI).Structural formula is as follows:
The root of langdu is Isolated From Thymelaeaceae Species, per nnial herb, leaf alternate, flower both sexes, very beautiful, for viewing and admiring.On plateau, herdsman have got such name because of its toxic juice to it.Root of langdu flower root system is large, and water-retaining capacity is strong, can adapt to the weather that arid is cold, and vitality is strong, and around herbaceous plant is difficult to resist with it, has been regarded as the warning lamp of grassland desertification in some places.And on plateau the spreading unchecked of the root of langdu, most important reason is then people's orazing too closely, and other species have lacked, and the root of langdu is taken advantage of a weak point, and the root of the plant root of langdu and stem micromicro are used as papermaking etc. as industrial raw material.There is following pharmacological action:
1. anticancer, antitumor action Feng Wei is good for, Ikekawa Tero reports the diterpene compound Buddhist nun morpholine (gnidimacrin) be separated in the methanol extract of Stellera chamaejasme L. in " antitumour activity of stellera chamaejasme L extract Buddhist nun morpholine ", result shows, showing that Buddhist nun's morpholine has stronger antitumour activity, is the main component of Stellera chamaejasme L. antitumous effect.Yang Baoyin, Yang Zhengyu, Gao Guodong, wait the antitumous effect reporting Stellera chamaejasme L. in " Stellera chamaejasme L. is to the restraining effect of mouse transplanting tumor " to carry out experimental observation, find that the water solubles of this medicine and volatile matter all have tumor-inhibiting action.Fan person of outstanding talent, Jia Zhengping, Xie Jingwen, waits the anticancer mechanism reporting Stellera chamaejasme L. aqueous extract (SCLA) in " Stellera chamaejasme L. aqueous extract mouse drug serum is on the impact of human hepatoma cell proliferation ", and direct anticancer propagation is the main anticancer mechanism of Stellera chamaejasme L..Jia Zhengping, Fan person of outstanding talent, Wang Yanguang, waits for " Stellera chamaejasme L. aqueous extract mouse drug serum is to mouse leukemia L 1210the impact of cell proliferation, Clone formation and DNA synthesis " in report direct antiproliferative effect and DNA synthesis is the important anticancer mechanism of Stellera chamaejasme L..Fan person of outstanding talent, Jia Zhengping, Xie Jingwen, Deng reporting Stellera chamaejasme L. (SCL) Antitumor Mechanism in " Stellera chamaejasme L. drug-serum of mouse induced apoptosis of K 562 cells ", the collaborative anti-liver cancer effect of Stellera chamaejasme L. (SC) and cellulotoxic chemotherapeutics, Xie Hua, Jia Zhengping, Xu Liting, Deng reporting Stellera chamaejasme L. (SCA) antitumous effect mechanism in " drug serum of Stellera chamaejasme L. aqueous extract mouse is on the impact of K562 cell proliferation ", after oral SCA, the direct anticancer proliferation function of the effective constituent of body absorbed into serum may be its important anticancer mechanism.Fan person of outstanding talent, Jia Zhengping, Xie Jingwen, cellulotoxic chemotherapeutics resisting liver cancer activity can be strengthened Deng reporting Stellera chamaejasme L. in " Stellera chamaejasme L. mouse drug serum works in coordination with the anti-liver cancer of cellulotoxic chemotherapeutics and Mechanism Study ", co-induction apoptosis of tumor cells, reduce bcl-2 positive expression, stop tumour cell cycle in G 2/ M the phase is its main mechanism.Jiao Xiaolan, Jia Zhengping report the main anticancer mechanism that direct cancer inhibitor cell propagation is Stellera chamaejasme L. in " impact that Stellera chamaejasme L. water extraction aqueous extract mouse drug serum is bred Human gastric adenocarcinoma ".Huang takes auspicious, Jia Zhengping, Fan person of outstanding talent, be less than 10000 molecular weight alcohol extracting position (SCES) anti-tumor activities Deng reporting Stellera chamaejasme L. in " the Stellera chamaejasme L. alcohol extracting position anti-tumor activity that molecular weight is less than 10,000 ", the propagation of SCES to the tumour cell of vitro culture and mouse transplanting tumor all has obvious restraining effect.Wang Runtian, Zhang Kunjuan, Tong Hui, Deng report in " the anti-knurl study mechanism of Stellera chamaejasme L. methanol extract " Stellera chamaejasme L. alcohol extract in range of doses can inhibition tumor cell growth, improve mice with tumor immunologic function, anti-knurl mechanism and its can stimulate Spleen cell proliferation, collaborative ConA stimulates splenocyte to transform and improves splenocyte NK killing activity and blocks tumor cells cycle.Duan Xin, Jia Chunfang report Stellera chamaejasme L. and have the multiple biological activitys such as antitumor, antibacterial in the clinical study of lung cancer " Stellera chamaejasme L. treatment ", and pharmacologically active is strong, and assisting therapy nonsmall-cell lung cancer clinical has can obtain better short-term curative effects.Mao Gang, Wang Jian, Chen Guojun, wait and report Stellera chamaejasme L. suppression human bladder cancer T24 cell proliferation in " Stellera chamaejasme L. aqueous extract mice serum be on the impact of human bladder cancer T24 cell proliferation ", may become the medicine that bladder cancer is new.Jia Zhengping, Fan person of outstanding talent, Xie Jingwen, the susceptibility of cellulotoxic chemotherapeutics to K562/VCR mdr cell is significantly increased Deng reporting 5%SC drug serum in " Mouse serum of Stellera chamaejasme chemotherapeutics is to the antitumour activity of K562/VCR mdr cell ", VCR, Dox, the more independent chemotherapy drug component of the IC50 of VP-16 to K562/VCR does not reduce 6.3, 15.0 and 18.5 times, number of cell clones reduces 45.1% respectively, 66.6% and 58.6%, [3H] TdR mixes K562/VCR cell DNA also significantly to be reduced, sensitization increases with SC drug serum ratio and strengthens.Pan Guofeng, Yang Qing, Liu An, there is certain apoptosis-induced effect Deng reporting Stellera chamaejasme L. composition and effectiveness Zp1111 in " Stellera chamaejasme L. composition and effectiveness induction apoptosis of human hepatoma cell and the impact of cell cycle deopendent protein kinase CDK2 ", BEL-7402 cell-cycle arrest can be made in the G1 phase, and its mechanism of action may be relevant with suppression CDK2.Pan Guofeng, Yang Qing, Liu An, to human liver cancer cell BEL-7402 transplanted tumor in nude mice, there is stronger restraining effect in vivo Deng reporting Stellera chamaejasme L. composition and effectiveness in " Stellera chamaejasme L. composition and effectiveness is to the suppression of hepatocellular carcinoma in nude mice transplanted tumor and mechanism thereof " and present certain dose-dependence, this component has certain apoptosis-induced effect, may be relevant with rise Bax.Wang Liping, Wang Yishan, Zhang Guoying, waits in " research of the impact that the root of langdu grows malignant melanoma cell and molecular mechanism of action thereof ", to report euphorbia extracting solution lower anti-apoptotic Bcl-2 albumen and raise the expression of short apoptosis Bax albumen, reduce Bcl-2/Bax Protein ratios and may be euphorbia extracting solution inducing apoptosis of tumour cell, suppress malignant melanoma B 16the molecular mechanism of Growth of Cells vital role.Liu Xiaoni, Li Yujie, Yang Qing, Deng in " stellera chamaejasme L extract external evoked apoptosis of tumor cells effect comparative studies ", report stellera chamaejasme L extract inducing apoptosis of tumour cell may be relevant with regulation and control death receptor pathway * pathway protein, stellera chamaejasme L extract inducing tumor cell mechanism is complicated, may there is the effect of two-ways regulation, it is apoptosis-induced is the result of comprehensive regulation.Zhang Qi, Sun Yifang, Chang Zhenguo, wait to report in Stellera chamaejasme L. rhizosphere microorganism-penicillium verruculosum fermented liquid in " research of Stellera chamaejasme L. rhizosphere penicillium verruculosum bacterium YL-52 secondary metabolite " and there is ursolic acid and evernic acid.Shen Yan, Li Jianwen, Zhang Yangang, Deng in " impact that Stellera chamaejasme L. water extract is expressed human bladder cancer T24 cell Survivin ", report Stellera chamaejasme L. water extract can by lowering the expression of Survivin albumen thus suppressing urinary bladder carcinoma T24 cell line propagation, promote its apoptosis, and there is concentration and time-dependent manner.Duan Xin, Jia Chunfang report Stellera chamaejasme L. and have the multiple biological activitys such as antitumor, antibacterial in the clinical study of lung cancer " Stellera chamaejasme L. treatment ", and pharmacologically active is strong, and assisting therapy nonsmall-cell lung cancer clinical has can obtain better short-term curative effects.Kan Xiaoxi, Wang Zhixin, Yang Qian is vivid, Deng reporting by carrying out gradient column chromatography with the ethanol of different concns to Stellera chamaejasme L. alcohol extract in " antitumor activity of Stellera chamaejasme L. alcohol extract ", obtain 16 components, carry out primary dcreening operation to it, each component is comparatively large to different tumor cell line restraining effect difference, totally to the inhibiting rate of lung carcinoma cell higher than liver cancer cell.Liu Fang, Liu Hua, after Sun Li reports stellera chamaejasme L extract effect human lung carcinoma cell extract NCI-H446 [H446] in " stellera chamaejasme L extract acts on the quantitative expression of human lung carcinoma cell NCI-H446 [H446] Telomerase afterwards ", the quantity of Telomerase obviously reduces and presents the positive correlation with dosage.Wang Bin, Wang Rui, Jia Zhengping, waiting in " anti tumor activity in vitro at Stellera chamaejasme L. systematic solvent extraction separation and Extraction position ", to report Petroleum ether extraction position is anti tumor activity in vitro position in Stellera chamaejasme L..Wang Min, king learns, Jia Zhengping, be 68.24% Deng Stellera chamaejasme L. total alkaloid content after report extraction purification in " anti-tumor activity of Stellera chamaejasme L. total alkaloids and study mechanism ", the three strain tumour cells of total alkaloids to vitro culture have stronger restraining effect, dominant mechanism blocks for causing the cell G0/G1 phase, inducing apoptosis of tumour cell.Xing Liqiang, Zhao Jianqing, Li Wang, Deng the growth reporting Stellera chamaejasme L. water extract can suppress NCI-H520 cell in " impact that Stellera chamaejasme L. water extract is expressed people's squamous cell lung carcinoma Survivin ", and there is concentration and time-dependent manner, Stellera chamaejasme L. water extract can reduce the Survivin protein expression level of NCI-H520 cell, and has no significant effect mRNA level in-site.Li Hongjun, Xing Liqiang, Li Wang, wait in " Stellera chamaejasme L. water extract is on the impact of lung adenocarcinoma cell line resistance and apoptosis ", reports Stellera chamaejasme L. water extract has obvious antitumor action, the susceptibility of drug resistance of lung cancer cell strain to DDP can be strengthened, to drug resistance of lung cancer, there is certain reverse effect.Xing Liqiang, Li Wang, Sun Li, wait in " stellera chamaejasme L extract reverses the immunohistochemical study of lung carcinoma cell resistance ", reporting the expression of stellera chamaejasme L extract to some Drug Resistance Gene Associated Proteins of two kinds of lung cancer cell lines have obvious restraining effect.Pan Guofeng, Yang Qing, Liu An, there is stronger restraining effect Deng reporting Stellera chamaejasme L. composition and effectiveness to mouse subcutaneous transplanting knurl H22 in " Stellera chamaejasme L. composition and effectiveness suppresses the experimental study of mouse subcutaneous transplanting knurl H22 ", and drug safety is better, wherein Zp1111 tumor-inhibiting action is the strongest, and intraperitoneal injection can show good tumor-inhibiting action compared with low dosage.Yang Jun, Wang Shiling, Wu Kun, the Culture of Fibroblasts that rat primary is cultivated bred there is stronger restraining effect Deng reporting Stellera chamaejasme L. extracting solution in " Stellera chamaejasme L. extracting solution is to the suppression of proliferation of lung fibroblasts in rat and its cytotoxic effect ", along with the increase of dosage, on cell proliferation restraining effect strengthens, and in dose-dependent inhibition, in high concentration range, Stellera chamaejasme L. extracting solution has certain toxic action to cell simultaneously.Wang Bin, Jia Zhengping, Cai Wenqing, Deng reporting Stellera chamaejasme L. total lignans composition to tumor cell line SGC-7901 in " anti tumor activity in vitro of Stellera chamaejasme L. total lignans ", the propagation of HEP-7402 and HL-60 and Clone formation have stronger restraining effect, its anti tumor activity in vitro higher than or close to vincristine(VCR).Wang Min, Jia Zhengping, Ma Jun, wait in " antitumor action of effects of total-flavonoid from Stellera chamaejasmel ", reporting effects of total-flavonoid from Stellera chamaejasmel have in stronger body and extracorporeal anti-tumor function.
2. insecticidal action Zhang Guozhou, Zhao Shanhuan reports the biological activity of root of Stellera chamaejasme extraction using alcohol (SCEE) to Ostrinia furnacalis 3 instar larvae and measures in " stellera chamaejasme L extract is to the bioactivity research of Ostrinia furnacalis ", result shows, SCEE has very strong biological activity to Ostrinia furnacalis larvae, along with the increase of SCEE content, larva counterpoise increasing amount also decreases, and after the SCEE process of high-content or low levels, the mortality ratio of larva is all very high.Zhang Guozhou, Wang Yawei, Xu Hanhong, the biological activity of the various insects such as small white is measured Deng reporting Stellera chamaejasme L. StellerachamaejasmeL. root ethanol extraction (be called for short SCEE) in " stellera chamaejasme L extract is to the bioactivity research of insect ", show that SCEE has very strong biological activity to cabbage caterpillar, Ostrinia furnacalis larvae, black peach aphid, and the biological activity of SCEE to Spodoptera litura larvae, diamondback moth larvae is weak.Zhang Guozhou, Chen Yunian, Wang Yawei, the action of contace poison of the different worm state of small white (PierisrapaeL.) is measured Deng reporting Stellera chamaejasme L. (StellerachameajasmeL.) root ethanol extraction (be called for short SCEE) in " Stellera chamaejasme L. root extract is to the action of contace poison of cabbage caterpillar ", adopt baud spray method with regard to SCEE measuring the toxic action of cabbage caterpillar, injection is adopted to measure the toxic action of small white 5 instar larvae with regard to SCEE, result shows: the action of contace poison of SCEE to small white ovum larva prepupa and pupa is poor, SCEE is to the toxic action of cabbage caterpillar comparatively strong (baud spray method), the toxic action of SCEE to small white 5 instar larvae is strong.Zhang Guozhou, Wang Yawei reports Stellera chamaejasme L. (StellerachameajasmeL.) root ethanol extraction (being called for short SCEE) on the repellent rate effect of small white (PierisrapaeL.) and measure the impact of the hatching rate of ovum in " stellera chamaejasme L extract is on the repellent rate of small white and ovicidal action ", result shows, the SCEE of 1.5% is laid eggs to have stronger avoid the rate of keeping away to small white, 1st, 2, 3, the repellent rate rate of 5d is respectively 77.59%, 64.29%, 52.46%, 31.23%, the ovicidal action of SCEE to small white ovum of 1.5% is poor, hatching rate after 7d is 56.41%.Zhang Guozhou, Wang Yawei, Xu Hanhong, wait and report Stellera chamaejasme L. (StellerachamaejasmeL.) extract to the biological activity of small white (PierisrapaeL.) in " the bioactive research of Stellera Chamaejasme Against Pieris Rapae ".Result shows, these extracts have very strong food refusal, stomach toxicity, growth-inhibiting effect to small white 5 instar larvae, but its action of contace poison is poor.Yang Ying, Sun Jianchen, Wang little Gang, Stellera chamaejasme L. is made an addition in feed in varing proportions Deng reporting in " Stellera chamaejasme L. fodder additives is to chicken weightening finish and the research of Anti-human globulin test ", observe its impact on chick weight gains and Anti-human globulin test, feed for a long time and with the addition of the feed of 1.0% Stellera chamaejasme L., chick chronic poisoning can be caused, impaired development, even dead.Cui Haiyan, Jin Hui, wangdan is red, Deng reporting different new stellerin A and neochamaejasmine B all has certain contact toxicity to two kinds of nematodes in " different new stellerin A and neochamaejasmine B are to the contact toxicity research of pine wood nematode and B. mucronatus in root of Stellera chamaejasme ", and under identical treatment time and concentration, neochamaejasmine B is all better than different new stellerin A to the contact toxicity of two kinds of nematodes.He Yiguo, Zhao Xingxiu, Deng Jing, Deng reporting the cytotoxicity of Stellera chamaejasme L. root meal ethanol extraction to rice grub pink rice borer and striped rice borer in " stellera chamaejasme L extract to the snout moth's larva of rice kill activity research ", when concentration be 2.0g/L, action time is 72h, ethanol extraction is 92.4% to pink rice borer lethality rate, and the mortality ratio of striped rice borer is 20.9%.History legend, Wang Chen reports concentration in " research of Stellera chamaejasme L. crude extract insecticidal activity " when being 160moL/L, 4 instar larvaes show as the food refusal phenomenon of height, and concentration is 80moL/L and 40moL/L, and insecticidal effect is similar, during 72h, when concentration is 80moL/L, the highest insecticidal effect reaches 85.36%, and when concentration is 2.5moL/L, insecticidal effect is not high, is only 27.09%, under 3 treatment times, LC50 is respectively 39.36moL/L, 17.02moL/L and 8.8moL/L.Fan person of outstanding talent, Jia Zhengping, Xie Jingwen, K562 cell proliferation is significantly suppressed Deng reporting SCL (5-20) g/kg mouse drug serum in " Stellera chamaejasme L. drug-serum of mouse induced apoptosis of K 562 cells ", the apoptotic morphological change of obvious induction K562 and DNA change, the dosage that apoptotic cell rate and mouse take SCL aqueous extract is proportionate.Guo Xia, Ding Wenjiao, Yang Jiayue, Deng reporting root of Stellera chamaejasme ethanol extraction and sherwood oil, chloroform, ethyl acetate and aqueous phase extract have contact toxicity in various degree to Ditylenchus destructor in " Stellera chamaejasme L. root extract and different solvents extract are to the research of Ditylenchus destructor contact toxicity ", wherein the contact toxicity of acetic acid ethyl ester extract to Ditylenchus destructor is the strongest, be significantly higher than other extracts, along with the increase of concentration for the treatment of and the growth in treatment time, the contact toxicity of this extract to nematode obviously strengthens.Korea S monarch, Sheng Tiefu, Liu Jingwen, distilled water, ethanol, acetone solvent soak extraction is used respectively Deng reporting Stellera chamaejasme L. in " research of Stellera chamaejasme L. vat liquor insecticidal effect ", by to test insect timed spays different types of Stellera chamaejasme L. extracting solution, observe and record in 24h, 48h, 72h, for the dead quantity of examination insect, by supplying examination insect to the sensitivity of the different vat liquor of Stellera chamaejasme L., study the insecticidal activity of Stellera chamaejasme L. extracting solution, to determine the biological effect of Stellera chamaejasme L. in the prevention and control of plant diseases, pest control.Zhou Kang, Zhao Hongmei, Qin Liangbin report Stellera chamaejasme L. in " plant Stellera chamaejasme L. kills the research of effect to oncomelania leaching " stronger snail killing function, and mainly affect energy metabolism in oncomelania histocyte, Stellera chamaejasme L. has fixed toxic action to water fish class.Malin, Kang Xiaohui, Yi Huang, waits and report Stellera chamaejasme L. supercritical CO in " inhibition of stellera chamaejasme L extract seed soaking to stripe rust of wheat " 2extract is to the poison of tagging of carmine spider mite, and SCE can suppress examination mite acetylcholinesterase, monoamine oxidase, Na +-K +-ATP enzyme and Ca 2+-Mg 2+the activity of-ATP enzyme, infers accordingly, and SCE may have neurotoxicity to carmine spider mite.Report root of Stellera chamaejasme ethyl acetate phase extract 200 times of liquid in Sun Kui, Wang Ning " Stellera chamaejasme L. ethyl acetate extract control cucumber liriomyza bryoniae field test ", to liriomyza bryoniae larva, there is ideal preventive effect.Wang Xuangao, Shi Guanglu, Wang Younian, Deng report in " in Stellera chamaejasme L. the chemical composition of flavonoid compound and the research to carmine spider mite contact toxicity thereof " Stellera chamaejasme L. element A, Quercetin and (+)-Biao loquat element all there is certain acaricidal activity, wherein show loquat element acaricidal activity the strongest.High Man the Lushui River, Wu Lang, Chen Long, wait in " Stellera chamaejasme L. activeconstituents be to the biological activity of Asiatic migrotory locust and pathological research ", report Stellera chamaejasme L. activeconstituents, to Asiatic migrotory locust, there is food refusal, tag, stomach poison activity and Growth inhibition, wherein antifeedant activity is the most remarkable.Li Jie, Zhao Fei, Liu Suqi, to have tetranychus viennensis (TetranychusviennensisZacher) well tag and systemic activity Deng reporting Stellera chamaejasme L. root extract in " Stellera chamaejasme L. root extract is to the biological activity of tetranychus viennensis ", the acaricidal activity of ligroin extraction and chloroform extract is the highest, in systemic action, the acaricidal activity of ethanol, chloroform and ligroin extraction is all higher, and miticidal effect is remarkable.Tang Chuanjiang, Hou Taiping, display that in " preliminary study of Stellera Chamaejasme L Against Stored Grain Insect ", to report the prevention effect of Stellera chamaejasme L. root powder to rice weevil, lesser grain borer, sitophilus zea-mais better, in the crude extract of root of Stellera chamaejasme powder, the extracting solution of polarity and non-polar solvent all shows the higher insecticidal activity to rice weevil.Root of langdu ethanol extract, under the dosage of 1.5g/kg, be 90.98%, and root of langdu hexane extract is under the dosage of 0.5g/kg to the lethality rate of rice weevil, to the lethality rate of rice weevil still up to 98.44%.
There is Substance in intelligent the reporting in ethanol extract in " Stellera chamaejasme L. root extract is studied the fungistatic effect of plant pathogenic fungi " of 3 bacteriostatic action Kang Xiao, better to the inhibition of Sclerotinia sclerotiorum, phytophthora capsici, tomato early blight bacterium, Botrytis cinerea germ, certain restraining effect is also shown to other several germs.Deng Xiaoting, Tian Shuqin, Chen Feng beacon, waits in " Stellera chamaejasme L. liniment treatment beaver rabbit skin skin mycotic clinical experimental study ", reporting Stellera chamaejasme L. liniment (by reagent) and hydrochloric acid terbinafine (positive control drug) curative ratio is respectively 92.32% and 69.71%.Stellera chamaejasme L. liniment is better than hydrochloric acid terbinafine, and treatment group, positive controls compare with negative control group, and it is efficient, cure rate is all in pole significant difference.Zhao Lei, Du Juan, Wang Younian, wait in " stellera chamaejasme L extract is to the Antifungal Activity in Vitro of 3 kinds of pathogenic bacterias ", reports Stellera chamaejasme L. methanol extract has stronger bacteriostatic action to 3 kinds of pathogenic bacterias, bacteriostasis rate is all higher than 68%.Zhao Lei, Du Juan, Bu Chunya, Deng reporting Stellera chamaejasme L. (Stellerachamaejasme) extract to the bacteriostatic activity of Botrytis cinerea germ (Botrytiscinerea) in " Stellera chamaejasme L. active substance is to the restraining effect of Botrytis cinerea germ ", found that Umbelliferone havoc Botrytis cinerea germ spore and mycelial morphological structure.Bu Chunya, establish an army, Wang Younian, thick extracted extract should be obtained with ethanol immersion Deng reporting root of Stellera chamaejasme in " suppressing plant pathogenic fungi active substance to be studied in Stellera chamaejasme L. ", extract further by ethyl acetate again, be separated further with macroporous resin subsequently, the component 9 pairs of Botrytis cinereas etc. obtained have good fungistatic effect.Zhao Lei, Du Juan, Bu Chunya, be Umbelliferone Deng the main bacteriostatic active ingredients reporting the most high reactivity stream part 3 of Stellera chamaejasme L. in " Stellera chamaejasme L. active substance is to the restraining effect of Botrytis cinerea germ ", and along with the raising of concentration, the restraining effect of this activeconstituents to Botrytis cinerea germ also strengthens, Umbelliferone havoc Botrytis cinerea germ fibrillae of spores volume morphing structure.Wang Yuhua, Yang Xia, Sun Lijun, Deng the white multicomponent synergy in the main source of cytotoxicity reporting Stellera chamaejasme L. in " research of anaesthetic material Stellera chamaejasme L. vitro cytotoxicity ", its protein may be one of main toxic sites of Stellera chamaejasme L., and concocting method can reduce the toxicity of Stellera chamaejasme L. medicinal material and retain its biological work.Ou Yangqiu, Huang Xiao, Tao Ke, wait in " Stellera chamaejasme L. is on the restraining effect of trichophyton gypseum and on its Ultrastructural impact ", reports Stellera chamaejasme L. has stronger restraining effect to trichophyton gypseum, has the application potential for the treatment of skin tinea.Guo Dongyan, Yang Shunyi, Zhang Xinhu, be the optimum solvent that root of Stellera chamaejasme Substance extracts Deng reporting ethanol in the preliminary study of antipathogenic composition " in the root of Stellera chamaejasme ", and continuous circumfluence extraction method is optimum extracting method, containing 1 in root of Stellera chamaejasme, 7, the antipathogenic composition that 7-trimethylammonium-two ring [2,2,1]-2-heptanone, N-phenyl--naphthylamines, phthalic acid two-(2-ethyl)-own ester, dioctyl phthalate (DOP) etc. 26 kinds are possible.Wen Zheyi, Shi Guanglu, Su schoolmate, obvious restraining effect is had Deng reporting Stellera chamaejasme L. ethyl acetate extract to 7 kinds in 8 kinds of test plant pathogenic bacterias in " stellera chamaejasme L extract is to the bioactivity research of pathogenic bacteria and peach enzyme ", wherein completely inhibit the former bacterium of peach brown rot, apple decay cause of disease bacterium, gibberella saubinetii cause of disease bacterium, the former bacteria growing of cucumber fusarium axysporum, Stellera chamaejasme L. ethyl acetate, water, methyl alcohol, ethanol, ligroin extraction all has restraining effect (bacteriostasis rate is all higher than 60%) to the former bacterium of peach brown rot, wherein Stellera chamaejasme L. ethyl acetate extract suppresses the growth of pathogenic bacteria mycelia completely, scab through the ethyl acetate extract process peach of 3 kinds of concentration is all less than contrast, and mass concentration to be that 20mg/mL extract controls peach effect of rotting best.Kong Jie, Wu Jiajun, Shi Guanying, be low toxicity Deng reporting Stellera chamaejasme L. acetic acid ethyl ester extract to small white mouse per os acute toxicity in " stellera chamaejasme L extract is to the preliminary study of experimental animal acute toxicity and activity ", nonirritant is belonged to the acute skin irritation of white rabbit, belong to slight pungency to the Eye irritation of white rabbit, belong to poisoning level to the toxicity of crucian, Stellera chamaejasme L. acetic acid ethyl ester extract has good inhibit activities to Phytophthora infestans germ.Yang Jiayue, Yan Zhiqiang, Xu Rui, very strong growth-inhibiting effect is had Deng reporting root of Stellera chamaejasme ethanol extraction to Arabidopis thaliana in " in root of Stellera chamaejasme the isolation identification of active substance and the mechanism of action ", chloroform and acetic acid ethyl ester extract are the main efficient parts of Stellera chamaejasme L. vegetable poison activity, and Umbelliferone and daphnoretin are the effective constituent of Stellera chamaejasme L. vegetable poison activity.Xue little Ping, Wang Maosheng, Chen Yi, wait in " Stellera chamaejasme L. extracting solution control tobacco nematode the test of pesticide effectiveness ", reporting Stellera chamaejasme L. extracting solution have obvious restraining effect to tobacco cucumber mosaic virus, can also prevent and treat other diseases.
4 antioxygenation Li Wenlong, Zhang Pengfei, Li Jianyun, wait in " Chinese stellera root total flavonoids is to the research of Antioxidation Effect ", reports Chinese stellera root total flavonoids oxyradical can be suppressed the damage of body, has the effect improving antioxidant ability of organism.Huo Qiang, Wang Yu, Gao Rongyuan, the effect that Chinese stellera root total flavonoids has significant external removing ultra-oxygen anion free radical, hydroxyl radical free radical is reported Deng in " extraction of Chinese stellera root total flavonoids and Antioxidation in vitro research ", its effect is better than VC, is a kind of natural antioxidants having Development volue.
5 is anticonvulsion, and antiepileptic action Stellera chamaejasme L. can effectively resist maximal electroshock convulsive attack, extends the convulsive attack latent period that Yetrazol brings out, and improves convulsive threshold, can extend the survival time of convulsions mouse simultaneously, reduces mortality ratio; Also good antagonistic action is had to sound source convulsive attack; Also can significantly improve stimulation in rats cortical motor area and bring out convulsive threshold, this medical instrument has anticonvulsant action certainly further.Its anticonvulsant action mechanism is relevant with amino acid neurotransmitter proportional imbalance in animal brain, also may be relevant with apoptosis etc.Experiment kainicacid model and electricity irritation rat cerebral cortex model, find that Stellera chamaejasme L. can reduce rat cerebral cortex, hippocampus excitatory amino acids content, especially L-glutamic acid, aspartic acid, also can improve inhibitory aminoacid content, as γ-aminobutyric acid simultaneously.Zhang Meini, Wang Mingzheng, Liu Yuxi, Deng reporting in " experimental study of Anticonvulsant Spectrum of Compounds Extracted by Pyruvate from Stellera chamaejasme L ", CEPSC is effective to the multiple convulsion model of animal, that a kind of acting duration is long, the anti-epileptic material of what anticonvulsant spectrum was wide have Development volue, its interaction property is similar to VPA.Zheng Xinyuan, Liu Enli, Li Qingshan, report determine that ether extraction position and acetone extraction position are its antiepileptic activity position Deng in " screening of Stellera chamaejasme L. antiepileptic activity position and reactive site in determination of total flavonoids ", ether extraction position shows stronger antiepileptic activity and higher mortality ratio, acetone extraction position shows stronger combined therapy effect, and in ether reactive site, general flavone content is 8.51%, and in acetone reactive site, general flavone content is 5.07%.Zhang Meini, Liu Yuxi, Wang Mingzheng, Deng report in " screening study of stellera chamaejasme L extract anti-experimental character epilepsy " Stellera chamaejasme L. acetone, sherwood oil, ether, ethanol four kinds of extracts to mouse maximal electroshock seizure experiment (MES), pentylenetetrazole convulsion experiment (MET) and electricity irritation rat layer convulsive threshold (TLS) model all there is stronger antagonistic action, and wherein acetone extract toxicity is lower, therapeutic index is up to 14.9.Chinese scholars has risen to the Mechanism Discussion of molecular level from pharmacology originally, clinical study to the research of Stellera chamaejasme L., fully show that Stellera chamaejasme L. is a herbal medicine likely, especially our research is the important breakthrough of Stellera chamaejasme L., be expected to by high-tech means the further separation and Extraction of this medicine effective anti-epileptic composition acetone extract, analyze its chemical structure, establish basic substance for the semi-synthetic Newer antiepileptic of orientation and theoretical foundation is provided.Clinical application in: 1) treat tumour; 2) tuberculosis is treated; 3) tetter is treated; 4) gynecopathy is treated; 5) sciatica is treated; 6) taeniasis bovis is treated; 7) epilepsy etc. is treated.
The Stellera chamaejasme L. extraction and purification process of bibliographical information has: get dry root of Stellera chamaejasme, pulverizes rear extraction using alcohol, and concentrate to obtain medicinal extract, medicinal extract, with organic solvent extraction, obtains each extraction position respectively.Macroporous resin column roughing out, obtains 9 positions, and every position is through silica gel column chromatography separation repeatedly, and gradient elution, the method such as purifying, recrystallization, obtains compound.Dry Stellera chamaejasme L. pulverizing medicinal materials, ethanol percolation, obtains medicinal extract after reclaiming ethanol, mixes sample with diatomite 1, dry rear extraction, obtains extract after recycling design, is separated through silica gel column chromatography, gradient elution, is separated and SephadexLH-20 purifying through silica gel column chromatography repeatedly, obtains compound.Root of Stellera chamaejasme pulverizes rear extraction using alcohol, and extracting solution concentrating under reduced pressure, concentrated solution organic solvent extraction, with silica gel column chromatography, gradient elution, through the separation and purification repeatedly of SephadexLH-20, silica gel and reversed-phase silica gel column chromatography, obtains compound.Get Stellera chamaejasme L. dry root, pulverize rear alcohol reflux, concentrated extracting solution obtains ethanol extract, adopt silica gel column chromatography to be separated, gradient elution, with preparing silicon, glue Thin-layer separation, is separated with petroleum ether-ethyl acetate, and obtained compound is separated through reduce pressure post, Preparative TLC of silica gel.Stellera chamaejasme L extract and diatomite mix, and use organic solvent refluxing extraction, and extract is through silica gel H dry chromatography, silica gel H Preparative TLC chromatography, and scraping colour band, with ethanol recrystallization repeatedly, then carries out silica gel column chromatography, wash-out, recrystallization.Dry Stellera chamaejasme L. pulverizes alcohol reflux, concentrated, obtains medicinal extract, then uses organic solvent extraction, is separated wash-out with silica gel column chromatography separation, silica gel thin-layer.Chameajasme is broken, leach with aqueous sodium hydroxide solution, filter, acidified filtrate, obtain a throw out, throw out is clayed into power, thoroughly extract with ether, dry extraction liquid, obtain Vandyke brown paste, add organic solvent, heating, acetylize, reaction solution is placed and is spent the night, leach white depositions, with sodium hydroxide hydrolysis, filter, acidifying, obtain white precipitate, examine and determine with thin-layer chromatography, thin-layer chromatography separation is carried out with silica gel-G plate, wash out with diluted alkaline, continue with extraction into ethyl acetate, boil off solvent, residue is with Diethyl ether recrystallization, obtain colorless needle crystals.Stellera chamaejasme L. is added ethanol, lixiviate, filter, filtrate reduced in volume, obtain Stellera chamaejasme L. root extract, adding distil water thermosol, extraction, extraction liquid is evaporated to thick paste, silica gel column chromatography is separated, gradient elution, merges after thin-layer chromatography inspection, determine active high flow point, after concentrated highly purified monomeric compound.Chameajasme cleans section airing, and alkali soaks, and filtration, acidification of filtrate, obtain tan precipitate, precipitation grinding powder, extract, recycling design, paste adds anhydrous pyridine, concussion mixing, adds the backflow of a small amount of acetic anhydride, puts into frozen water, placement is spent the night, and has tan precipitate, precipitation hydrochloric acid and cold water washing, alkali dissolution, filtration acidifying, there is tan precipitate, DEAE-Mierocrystalline cellulose chromatography, gradient elution, collect peak elution liquid, concentrate drying obtains finished product.Chameajasme is pulverized, and obtains brown crude product after diluted alkaline, extraction, steams to desolventize and separates out brown crude product.Obtained by DEAE column chromatography, obtaining finished product after concentrate drying is white.With alcohol reflux after dry root of Stellera chamaejasme pulverizing, concentrate and to obtain total medicinal extract, medicinal extract extracts, and extract, through silica gel column chromatography gradient elution, is prepared into compound through HPLC.Root of langdu powder adds organic solvent extraction, and concentrating under reduced pressure obtains medicinal extract, adds distilled water, heating in water bath, leaves standstill, and filters, discards filtrate, obtains total flavones after volatilizing solvent.Root of langdu powder alcohol immersion, ultrasonic extraction, extracting solution concentrating under reduced pressure, extraction, concentrating under reduced pressure obtains medicinal extract, adds distilled water heating in water bath, leaves standstill room temperature, filters, discard filtrate, to volatilize after solvent to obtain total flavones, mix after sample volatilizes with diatomite, load in glass tube column, wash with sherwood oil stream, reload glass tube column, get with the elution of propyl carbinol stream, solvent is volatilized, upper polyamide resin column, wash-out after n-butanol extracting liquid is concentrated, concentrated, dry, obtain total flavones composition [50-63].
The present invention adopts one or more strong polarized mixed solvents the activeconstituents simultaneous extraction in Stellera chamaejasme L. to be gone out, concentrated, obtain the medicinal extract of a constituents mixt, then according to " similar compatibility " principle, the solvent extraction of opposed polarity is adopted to go out corresponding composition, again in conjunction with different chromatography, obtain gnidimacrin, β-amyrin acetic ester, Scopoletin, Podocarpus macrophyllus resinol, Eudesmin, Stellera chamaejasme chromone, 7-methoxyl group chamajasmin, root of langdu B prime, Japan cypress alicyclic lactone, isobergapten, Umbelliferone, daphnoretin, , Isodaphnoretin, Raven's Test, simplexin, crepitin, methyl arctigenin-4'-gentiobioside, Umbelliferone glycosides, syringin, Syringa oblata Lindl. phenolic glycoside, lariciresinol B, matairesinol, pine tree lipidol glycosides, lariciresinol glycosides, neochamaejasmine B, pine tree lipidol glucopyranoside, chamajasmin, different new stellerin, different new stellerin A, excellent chamajasmin, the peaceful B of the root of langdu, Liriodendron Syringaresinol B, each monomer components such as lirioresinol A dme and lirioresinol B dme.New technology is unique, is applicable to suitability for industrialized production.
Reference:
[1]. cloth and Bart's that, E Erdunbaoligao. anaesthetic handbook [M]. Shenyang: Liaoning Nationalities Press, 1995:106.
[2]. Supreme Being Ma Er, red increasing Peng arranges. product pearl book on Chinese herbal medicine [M]. Shanghai: Shanghai science tech publishing house, 1968:102.
[3]. Zhanbra Dorje. the positive allusion quotation of anaesthetic [M]. Huhehaote: the Inner Mongol People's Press, 1984:260.
[4]. Bai Qingyun. Chinese medicine encyclopedia [M]. Chifeng: Inner Mongol science tech publishing house, 1986:322.
[5]. spread out mulberry. know pharmacy [M]. Beijing: Beijing Nationalities Press, 1998:67.
[6]. the new hospital in Jiangsu, Chinese medicine voluminous dictionary [M]. Shanghai sanitation technology press, 1977,1898-1900.
[7]. Deng Jun, Diao Zhimin, Lei Qingjuan, etc. the present Research comprehensive utilization of Qinghai Province's Stellera chamaejasme L. and Preventing Countermeasures [J]. Agriculture of Anhui science, 2006,34 (3): 555-557.
[8]. grain Xiao Li, Lin Ruichao, Wang Zhaoji, etc. toxic traditional Chinese medicine root of langdu quality standard research [J]. Chinese patent medicine, 2006,28 (4): 498-503.
[9] Yang Wei's literary composition, Xing Youquan, Song Maosen, etc. Chemical Components in Stellera Chamaejasme L research [J]. Lanzhou University's journal, 1983,19 (4): 109-111.
[10] Liu Guifang, Fu Yuqin, Hou Fengfei, etc. Chemical Components in Stellera Chamaejasme L research [J]. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 1995,20 (12): 738-740.
[11] Liu Xin, leaf literary talent, Che Zhentao, etc. the chemical constitution study [J] of Stellera chamaejasme L.. herbal medicine, 2004,35 (4): 379-381.
[12] Feng Baomin, bow is outstanding for dawn, Shi Liying, etc. the research [J] of phenolic compounds from Stellera chamaejasme. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 2008,33 (4): 403-405.
[13] Liu Xin, leaf literary talent, Che Zhentao, etc. lignan component research [J] of Stellera chamaejasme L.. China Medicine University's journal, 2003,34 (2): 116-118.
[14] Huang Wenkui, Zhang Zhenjie. the structure [J] of the two flavanone-chamajasmins (Chamaejasmine) in the thymelaeceae root of langdu. Lanzhou University's journal: natural science edition, 1977,12:50-54.
[15] Tian Shangyi, Wei Chunyan, thoughtful Wei, etc. high effective liquid chromatography for measuring root of Stellera chamaejasme, stem, leaf, spend the content [J] of middle Daphnelin. analytical chemistry research notes, 2004,12 (32): 1627-1630.
[16] Yang Guohong, Chen Daofeng. a trombolysan-Isodaphnoretin B [J] in Stellera chamaejasme L.. Chinese natural drug, 2006,11 (4): 425-427.
[17] Yang Wei's literary composition. Chemical Components in Stellera Chamaejasme L research [J]. Lanzhou University's journal, 1983,19 (4): 109.
[18]NiwaMasatake.StructureofisochamaejasminfromStelleraChamaejasmeL[J].Chem.Lett.，
1984，(9)：1587.
[19]IkegawaTetsuo.ChamaejasminandeuchamaejasminextractionfromStelleraChamaejasmeandtheirantiviralactivities[J].Jpn.KokaiTokkyoKohoJP08311，056[96311，056](CI.C07D311/32)，1996，(11)：26.
[20] Liu Guifang. Chemical Components in Stellera Chamaejasme L research [J]. CHINA JOURNAL OF CHINESE MATERIA MEDICA, 1995,20 (12): 738.
[21]RezanovaOI.FlavonoidsofStelleraChamaejasme[J].Rostit.Resur，1976，12(3)：3890.
[22] Feng Baomin. the research [J] of Chemical Components in Stellera Chamaejasme L. Shenyang Pharmaceutical University's journal, 2000,17 (4): 258.
[23]IkekawaTetsuro.Carcinestaticcompoundsandproductionthereof.PCT[J].IntApplWO93，03，039(Cl.C07D493/18)，1993，(2)：18.
[24]NarantuyaaS.Chemicalstudyofplantsofmongolia：coumarinsofStellerachamaejasmestructureofchamaejasmoside，anewbicoumaringlucoside[J].KhimPrirSoedin，1994，(2)：216.
[25] Yang Wei's literary composition. Chemical Components in Stellera Chamaejasme L research [J]. bulletin of Chinese materia medica, 1985,10 (12): 559.
[26]PingGao.Activityofthebotanicalaphicides1，5-diphenyl-1-pentanoneand1，5-diphenyl-2-penten-1-oneontwospeciesofAphididnae[J].PestManage.Sci.，2001，57(3)：307.
[28] Yang Wei's literary composition, punishment is had the right, Song Maosen, waits separation and the structure determination [J] of .7-methoxyl group chamajasmin. SCI, 1984, (5): 671.
[29]NiwaM，ChenXF，LiuGQ，etal.StructureofisochamaejasminfromStellerachamaejasmeL[J].ChemLett，1984，(9)：1587.
[30]RezanovaOI，BubeevvaLI：FlavonoidsofStellerachamaejasme[J].Rostit.Resur，1976，12(3)：389.
[3l]IkegawaT，IkegawaA.ExtractionofanticancerandantiviralsubstancesfromStellerachamaejasmefortherapeuticuse[P].JpnKokaiTokkyoKohoJP0892，118[9692，118](Cl.A61K35/78)，1996-04-09.
[32]EndoY，MarunoM，MiuraNetal.Novelditerpenesandtheiruseanantiviralandanti-HIVagentswithlowtoxicity[P].Jpn.KkaiTokkyoKohoJP10287，617[98287，617](Cl.C07C69/21)，1998-10-27.
[33]NiwaM，TakamizawaM，TatematsuH，etal.PiscicidalconstituentsofStellerachamaejasmeL.[J].ChemPharmBu11，1982，30(12)：4518-4520.
[34]YoshidaMitsuzi，FengWeijian，SaijoNagahiro，etal.Antitumoractivityofdaphane-typediterpenegnidimacrinisolatedfromStellerachamaejasmeL.[J].IntJCancer，1996，66：268-273.
[35] IkekawaTetsuro, IkekawaNobuo.Cacinostaticcompoundsandproductionthereof [P]. Japanese Patent: 91285390,1991-08-08.
[36] IkegawaTetsuo, IkegawaAkiko.ExtractionofantitumordeterpenesfromSteliera chamaejasme [P]. Japanese Patent: 08310993,1996-11-26.
[37]TatematsuH，KurokawaM，NiwaM，etal.PiscicidalconstituentsofStellerachamaejasmeL.[J].ChemPharmBull，1984，32(4)：1612-1613.
[38] IkegawaTetsuo, IkegawaAkiko.Extractionofanticancerandantiviralsubstance sfromStellerachamaejasmefortherapeuticuse [P]. Japanese Patent: 0892118,1996-04-09.
[39]ModonovaLD，ZhapovaTS，BulatovaNV，etal.CoumarinsfromStellerachamaejasmeL.[J].KhimPtirSoedin，1985，(5)：709.
[40]JinCD，RonaldGM，MohsenDaneshtalab.PhenylpropanoidglycosidesfromStellerachamaejasme[J].Phytochemistry，1999，50：677-680.
[41] Yang Wei's literary composition, Xing Youquan, Song Maosen, wait separation and the Structural Identification [J] of .7-methoxyl group chamajasmin. SCI, 1984,5 (5): 671-673.
[42]NiwaM，OtsujiS，TatematsuH，etal.StereostructuresoftwobiflavanonesfromStellerachamaejasmeL.[J].ChemPharmBul1，1986，34(8)：3249-3251.
[43]NiwaM，TatematsuH，LiuGQ，etal.IsolationandstructuresoftwonewC-3/C-3″-biflavanonesneochamaejasminAandneochamaejasminB[J].ChemistryLett，1984，148(4)：539-542.
[44]NiwaM，LiuGQ，TatematsuH，etal.Chamaejasmone，anovelrearrangedbiflavanoidfromStellerachamaejasmeL.[J].TetrahedronLett，1984，25(34)：3735-3738.
[45] Yang Wei's literary composition, Li Zhaolin, Yang Yucheng, etc. research (II) [J] of Chemical Components in Stellera Chamaejasme L. Lanzhou University's journal, 1983,19 (4): 109-111.
[46] IkegawaTetsuo, IkegawaAkiko.ChamaejasminandeuchamaejasminextractedfromS tellerachamaejasmeandtheirantiviralactivities [P]. Japanese Patent: 08311056,1995-05-19.
[47]JinC，MichetichRG，DaneshtalabM.FlavonoidsfromStellerachamaejasmeL.[J].Phytochemistry，1999，50：505-508.
[48] Feng Baomin, Pei Yuehu. the flavonoid compound [J] in Stellera chamaejasme L.. herbal medicine, 2001,32 (1): 14-15.
[49] Yang Wei's literary composition, vertical million beautiful jades, Yang Yucheng, etc. research (V) [J] of Chemical Components in Stellera Chamaejasme L. bulletin of Chinese materia medica, 1985,10 (12): 31-32.
[50]. Cao Xinwei, Feng Weisheng. the Recent Advances of Chemical Constituents [J] of the root of langdu. Henan College Of Traditional Chinese Medicine journal, 2004,19 (115): 81-84
[51]. Yan little Hong, Wang Canjian, Jiang Yingqiao. the chemical composition of the root of langdu, pharmacological action and quality standard research overview [J]. modern traditional Chinese medicine, 2009,29 (6): 67-70
[52]. Wang Wenxiang, fourth apricot bud. the chemistry of the root of langdu and pharmacological research are in progress [J]. external Medicinal Plants medicine fascicle, 1996,11 (6): 252-253
[53]. He Yufang, Xie Xiujuan, Wang Meiying. the pharmacological action of the root of langdu and Recent Advances of Chemical Constituents [J]. University Of Science and Technology Of He'nan's journal (medicine), 2004,22 (1): 79-80
[54]. Sun Lijun, Wang Wei, Wang Yuhua. the chemical constitution study [J] of anaesthetic material Stellera chamaejasme L.. research and development of natural products, 2012,24:188-190
[55]. Liu Xin, leaf literary talent, Che Zhentao, etc. the chemical constitution study [J] of Stellera chamaejasme L.. herbal medicine, 2004,35 (4): 379-381
[56]. Yang Jiayue, Yan Zhiqiang, Xu Rui, etc. the isolation identification of active substance and the mechanism of action [J] in root of Stellera chamaejasme. northwest Botany Gazette, 2011,31 (2): 291-297
[57]. Feng Baomin, Pei Yuehu, Han Bing. the research [J] of Chemical Components in Stellera Chamaejasme L. Shenyang Pharmaceutical University's journal, 2000,17 (4): 258-259
[58]. Cai, Zhang Fangxiang, Zou Zhenhong, etc. Chemical Components in Stellera Chamaejasme L research (V) chemical composition of volatile oil research [J]. contemporary Chinese medicinal application, 2012,6 (19): 120-121
[59]. Yang Weiwen, Xing Youquan, Song Maosen, etc. Stellera chamaejasme L. Chemical Composition research (I) [J]. Lanzhou University's journal (natural science edition) 1994 (4) 109-111,
[60]. Wang Yawei, Zhang Guozhou, Xu Hanhong, etc. the Extraction and isolation [J] of Stellera chamaejasme L. active insecticidal components. Agriculture of Anhui science, 2004,32 (4): 671-672
[61]. Li Yunbi, Fang Tianqi, Yu Hairui, etc. the extraction of Stellera chamaejasme L. effective constituent and property analysis [J]. biological processing, 2003,1 (2): 43-45
[62]. Feng Baomin, Pei Yuehu, Zhang Hailong, etc. the chemical composition [J] in Stellera chamaejasme L.. herbal medicine, 2004,35 (1): 12-14
[63]. Wu Xiaoliang, Han Min, Liu Xiaosong, etc. the comparison [J] of Chinese stellera root total flavonoids 3 kinds of extracting method. herding and forage science, 2009,30 (1): 39-40
Summary of the invention
For overcoming the deficiency in background technology, the present invention aims to provide the integrated extraction and separation method of Stellera chamaejasme L. effective constituent.
Technical solution of the present invention is:
The integrated extraction and separation method of Stellera chamaejasme L. effective constituent, comprises the steps:
(1) extraction of Stellera chamaejasme L., concentrated, add water-dispersion.
(2) concentrated solution petroleum ether extraction, chromatographic separation.
(3) the residual solution extracted with diethyl ether after petroleum ether extraction, chromatographic separation.
(4) the residual solution chloroform extraction after extracted with diethyl ether, chromatographic separation.
(5) the residual solution extraction into ethyl acetate after chloroform extraction, chromatographic separation.
(6) the residual solution acetone extract after extraction into ethyl acetate, chromatographic separation.
(7) the residual solution methanol extraction after acetone extract, chromatographic separation.
Embodiment
1. after the preparation of general extractive checks that disintegrator sieving net is intact, the Stellera chamaejasme L. gradation of drying is joined in shredder hopper, open pulverizer power knob, regulate hopper feed mouth size, comminuting matter, and check the charging of charging bag material, timely replacing, pulverizing completes, and opens pulverizing cover, dismounting lower screen cloth, splicing bag and dust settling pocket, clean with tap water; Screen cloth being put into tub brush scrubs to visual noresidue; Then rinse 3 secondary internal surface faces, screen cloth with tap water, install and close and pulverize cover, then clean shell with rag and dry.Pulverized and sieved on pulverizer by the Stellera chamaejasme L. infiltrated, sieve number is 30 orders.Pour in extractor after Stellera chamaejasme L. after pulverizing and sieving is weighed, inject 5000kg dimethyl formamide to extractor, open extractor steam valve and be heated to boiling, keep boiling state 2.5h; Steam off valve, opens fluid valve, decoction liquor in extractor is squeezed in thickener.Repeat to extract secondary, be respectively 4000kg solvent extraction 2.0h, 3000kg solvent extraction 1.5h.Third time, extracting solution was as the extraction agent of next batch of material, so circulated.By the extracting solution concentrating under reduced pressure of first twice, thickening temperature 70-80 DEG C, vacuum tightness-(0.090-0.095) Mpa, enriched material proportion, at 1.15-1.20, obtains general extractive condensed cream.The water-soluble abundant stirring of 5-10 times amount, dispersion is added in condensed cream, for subsequent use.
2. petroleum ether extraction, column chromatography Stellera chamaejasme L. extracts dispersion liquid isopyknic petroleum ether extraction 3-5 time, extraction liquid concentrates, by silica gel chromatographic column (200-300 order) (150mm × 1500mm) chromatographic separation, use sherwood oil successively, sherwood oil-vinyl acetic monomer (100: 5 ~ 100: 10, v/v) gradient elution, every 10mL receives 1 part, TLC detects, same section merges, collect the elutriant containing gnidimacrin (Gnidimacrin), add 3-5% gac, reflux decolour 30min, hot suction filtration, filtrate concentrates, crystallization, suction filtration, dry, obtain gnidimacrin.
3. isopyknic extracted with diethyl ether 3-5 time of the residual solution after extracted with diethyl ether, column chromatography petroleum ether extraction, extraction liquid concentrates, through dry method neutral alumina column (200-300 order) (150mm × 1500mm) chromatographic separation, neutral alumina column absorption is added after ethereal extract is concentrated, effluent liquid look is eluted to successively shallow with sherwood oil, elutriant merges, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain colourless acicular crystal β-amyrin acetic ester; Be eluted to effluent liquid look with ether more shallow, elutriant merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound Scopoletin; Then use E-C (100: 5 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, every 10mL receives 1 part, thin-layer chromatography detects, and merges same section, and 6-15 part merges, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, drying, obtains compound Podocarpus macrophyllus resinol; 16-30 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound Eudesmin; 31-52 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound Stellera chamaejasme chromone; 53-62 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound 7-methoxyl group chamajasmin; 54-68 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains colorless needles compound root of langdu B prime; 69-87 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains colorless needles compound Japan cypress alicyclic lactone; 88-99 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound sphondin; 100-112 part merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound isobergapten.
4. isopyknic chloroform extraction 3-5 time of the residual solution after chloroform extraction, column chromatography extracted with diethyl ether, extraction liquid concentrates, by wet method silicagel column (200-300 order) (150mm × 1500mm) chromatogram, chloroform extract is concentrated dry, dissolve with a small amount of chloroform, mix with silica gel, under room temperature, volatilization eliminates solvent, is added on silicagel column.First with sherwood oil wash-out, then with sherwood oil-chloroform (100: 10 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, every 10mL receives 1 part, and thin-layer chromatography detects, merge same section, obtain 112 flow points, 1-12 flow point is sherwood oil-chloroform (100: 10, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound Umbelliferone; 13-24 flow point is sherwood oil-chloroform (100: 15, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound daphnoretin; 24-38 flow point is sherwood oil-chloroform (100: 20, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound Isodaphnoretin; 39-51 flow point is sherwood oil-chloroform (100: 25, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound Raven's Test; 52-74 flow point is sherwood oil-chloroform (100: 30, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound simplexin; 75-96 flow point is sherwood oil-chloroform (100: 30, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound crepitin; 97-112 flow point is sherwood oil-chloroform (100: 30, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compounds methyl arctigenin-4'-gentiobioside.
5. isopyknic extraction into ethyl acetate 3-5 time of the residual solution after extraction into ethyl acetate, column chromatography chloroform extraction, extraction liquid concentrates, by wet method silicagel column (200-300 order) (150mm × 1500mm) chromatogram, acetic acid ethyl ester extract is concentrated dry, use a small amount of acetic acid ethyl dissolution, mix with silica gel, under room temperature, volatilization eliminates solvent, be added on silicagel column, with petroleum ether-ethyl acetate-acetone-methanol eluent system gradient elution, control elution flow rate 1mL/min, every 10mL receives 1 part, thin-layer chromatography detects, and merges same section, obtains 10 compounds.With petroleum ether-ethyl acetate (100: 5, v/v) wash-out, obtain 12 components, merge and obtain F1 (F1-1 ~ F1-12), add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound Umbelliferone glycosides.Petroleum ether-ethyl acetate (100: 10, v/v) wash-out, obtain 15 components, these 15 components are merged to concentrate and obtains F2, carry out silica gel column chromatography separation, use petroleum ether-ethyl acetate-acetone (100: 8: 5 ~ 100: 10: 8, v/v) wash-out successively, obtain 23 components (F2-1 ~ F2-33), detect according to thin-layer chromatography, F2-1 ~ F2-13 is merged, adds 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound syringin; Merged by F2-14 ~ F2-33, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound Syringa oblata Lindl. phenolic glycoside.Silicagel column, with petroleum ether-ethyl acetate (100: 20, v/v) chromatographic separation, obtains 36 components.These 36 components are merged to concentrate and obtains F3, carry out silica gel column chromatography separation, use petroleum ether-ethyl acetate-acetone (100: 8: 10 ~ 100: 10: 15, v/v) wash-out successively, obtain 43 components (F3-1 ~ F3-43).Detect according to thin-layer chromatography, merged by F3-1 ~ F3-16, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound lariciresinol B; Merged by F3-17 ~ F3-30, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound matairesinol; Merged by F3-31 ~ F3-43, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound pine tree lipidol glycosides.Silicagel column, with ethyl acetate-acetone (100: 20, v/v) chromatographic separation, obtains 35 components.These 35 components are merged to concentrate and obtains F4, carry out silica gel column chromatography separation, use ethyl acetate-acetone-methyl alcohol (100: 8: 10 ~ 100: 15: 20, v/v) wash-out successively, obtain 68 components (F4-1 ~ F4-68).Merged by F4-1 ~ F4-22, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound lariciresinol glycosides; Merged by F4-23 ~ F4-42, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound neochamaejasmine B; Merged by F4-432 ~ F4-68, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound pine tree lipidol glucopyranoside.
6. isopyknic acetone extract 3-5 time of the residual solution after acetone extract, column chromatography extraction into ethyl acetate, extraction liquid concentrates, by wet method neutral alumina column (200-300 order) (150mm × 1500mm) chromatogram, acetone extract thing is concentrated dry, use a small amount of acetone solution, mix with neutral alumina, under room temperature, volatilization eliminates solvent, be added on alumina column, with chloroform-methanol eluent system gradient elution.Control elution flow rate 1mL/min, every 10mL receives 1 part, and thin-layer chromatography detects, and merges same section, obtains 5 compounds.1-15 flow point is chloroform-methanol (100: 10, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound chamajasmin; 16-32 flow point is chloroform-methanol (100: 15, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains the different new stellerin of compound; 33-45 flow point is chloroform-methanol (100: 20, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains the different new stellerin A of compound; 46-61 flow point is chloroform-methanol (100: 25, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains the excellent chamajasmin of compound; 46-61 flow point is chloroform-methanol (100: 30, v/v) eluate, adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains the peaceful B of the compound root of langdu.
7. isopyknic methanol extraction 3-5 time of the residual solution after methanol extraction, column chromatography acetone extract, extraction liquid concentrates, by dry method silicagel column (200-300 order) (150mm × 1500mm) chromatogram, methanol extraction thing is concentrated dry, use a small amount of dissolve with methanol, mix with silica gel, under room temperature, volatilization eliminates solvent, is added on silicagel column.With acetate-methanol eluent system gradient elution.Control elution flow rate 1mL/min, every 10mL receives 1 part, and thin-layer chromatography detects, and merges same section, obtains 2 compounds.First use eluent ethyl acetate, receive 1 part with the every 10mL of acetate-methanol (100: 20 ~ 100: 30, v/v) again, thin-layer chromatography detects, merge same section, 1-18 flow point merges, and adds 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound Liriodendron Syringaresinol B; 19-43 flow point merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound lirioresinol A dme; 44-68 flow point merges, and adds 3-5% gac reflux decolour 30min, heat filtering, and filtrate concentrates, crystallization, dry, obtains compound lirioresinol B dme.

Claims (8)

1. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent, be raw material with Stellera chamaejasme L., the method includes the steps of:
(1) extraction of Stellera chamaejasme L., concentrated, add water-dispersion.
(2) concentrated solution petroleum ether extraction, chromatographic separation.
(3) the residual solution extracted with diethyl ether after petroleum ether extraction, chromatographic separation.
(4) the residual solution chloroform extraction after extracted with diethyl ether, chromatographic separation.
(5) the residual solution extraction into ethyl acetate after chloroform extraction, chromatographic separation.
(6) the residual solution acetone extract after extraction into ethyl acetate, chromatographic separation.
(7) the residual solution methanol extraction after acetone extract, chromatographic separation.
2. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, in step (1), Stellera chamaejasme L. is crushed to 30 orders, to extract one of in dimethyl formamide, morpholine, dimethyl sulfoxide (DMSO), tetrahydrofuran (THF) and pyridine, with the solvent of 8,6,5 times amount respectively at 70-90 DEG C extract 2.5,2.0,1.5h, by the extracting solution of first twice merge, concentrating under reduced pressure, third time, extracting solution was as the extraction agent of next batch of material, so circulated.Thickening temperature 70-80 DEG C, vacuum tightness-(0.090-0.095) Mpa, enriched material proportion 1.15-1.20, obtains general extractive condensed cream, and the water adding 5-10 times amount in condensed cream fully stirs, disperses, for subsequent use.
3. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, in step (2), Stellera chamaejasme L. extracts dispersion liquid isopyknic petroleum ether extraction 3-5 time, extraction liquid concentrates, use silica gel chromatography pillar layer separation, use sherwood oil, sherwood oil-vinyl acetic monomer (100: 5 ~ 100: 10, v/v) gradient elution successively, thin-layer chromatography detects, same section merges, and adds 3-5% gac, reflux decolour 30min, hot suction filtration, filtrate concentrates, crystallization, suction filtration, drying, obtains gnidimacrin.
4. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, residual solution isopyknic extracted with diethyl ether after step (3) PetroChina Company Limited. ether extracts 3-5 time, extraction liquid concentrates, be separated through dry method neutral aluminum oxide column chromatography, neutral alumina column absorption is added after ethereal extract is concentrated, use sherwood oil successively, ether, E-C (100: 5 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, thin-layer chromatography detects, merge same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound β-amyrin acetic ester, Scopoletin, Podocarpus macrophyllus resinol, Eudesmin, Stellera chamaejasme chromone, 7-methoxyl group chamajasmin, root of langdu B prime, Japan cypress alicyclic lactone and isobergapten.
5. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, residual solution in step (4) after extracted with diethyl ether isopyknic chloroform extraction 3-5 time, extraction liquid is concentrated dry, dissolve with a small amount of chloroform, mix with silica gel, under room temperature, volatilization eliminates solvent, is added on silicagel column.First with sherwood oil wash-out, again with sherwood oil-chloroform (100: 10 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, thin-layer chromatography detects, merge same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain Umbelliferone, daphnoretin respectively; , Isodaphnoretin, Raven's Test, simplexin, crepitin and methyl arctigenin-4'-gentiobioside.
6. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, is characterized in that, isopyknic extraction into ethyl acetate 3-5 time of the residual solution in step (5) after chloroform extraction, extraction liquid concentrates, dry, use a small amount of acetic acid ethyl dissolution, mix with silica gel, under room temperature, volatilization eliminates solvent, be added on silicagel column, with petroleum ether-ethyl acetate-acetone-methanol eluent system gradient elution, control elution flow rate 1mL/min, thin-layer chromatography detects, and merges same section.With petroleum ether-ethyl acetate (100: 5, v/v) wash-out, merge and add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtains compound Umbelliferone glycosides.Petroleum ether-ethyl acetate (100: 10, v/v) wash-out, merges to concentrate and carries out silica gel column chromatography separation again, use petroleum ether-ethyl acetate-acetone (100: 8: 5 ~ 100: 10: 8 successively, v/v) wash-out, thin-layer chromatography detects, and merges same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, drying, obtains compound syringin and Syringa oblata Lindl. phenolic glycoside.Silicagel column, again with petroleum ether-ethyl acetate (100: 20, v/v) chromatographic separation, merges to concentrate and carries out silica gel column chromatography separation again, use petroleum ether-ethyl acetate-acetone (100: 8: 10 ~ 100: 10: 15 successively, v/v) wash-out, thin-layer chromatography detects, and merges same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, drying, obtains compound lariciresinol B, matairesinol and pine tree lipidol glycosides.Silicagel column, again with ethyl acetate-acetone (100: 20, v/v) chromatographic separation, merges to concentrate and carries out silica gel column chromatography separation again, use ethyl acetate-acetone-methyl alcohol (100: 8: 10 ~ 100: 15: 20 successively, v/v) wash-out, thin-layer chromatography detects, and merges same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, drying, obtains compound lariciresinol glycosides, neochamaejasmine B and pine tree lipidol glucopyranoside.
7. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, residual solution in step (6) after extraction into ethyl acetate isopyknic acetone extract 3-5 time, extraction liquid is concentrated dry, use a small amount of acetone solution, mix with neutral alumina, under room temperature, volatilization eliminates solvent, be added on alumina column, with chloroform-methanol (100: 10 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, thin-layer chromatography detects, merge same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound chamajasmin, different new stellerin, different new stellerin A, excellent chamajasmin and the peaceful B of the root of langdu.
8. the integrated extraction and separation method of Stellera chamaejasme L. effective constituent as claimed in claim 1, it is characterized in that, residual solution in step (7) after acetone extract isopyknic methanol extraction 3-5 time, extraction liquid is concentrated dry, use a small amount of dissolve with methanol, mix with silica gel, under room temperature, volatilization eliminates solvent, is added on silicagel column.First use eluent ethyl acetate, again with acetate-methanol (100: 20 ~ 100: 30, v/v) gradient elution, control elution flow rate 1mL/min, thin-layer chromatography detects, merge same section, add 3-5% gac reflux decolour 30min, heat filtering, filtrate concentrates, crystallization, dry, obtain compound Liriodendron Syringaresinol B, lirioresinol A dme and lirioresinol B dme.
CN201510414030.1A 2015-07-10 2015-07-10 Integrated extracting and separating method for active ingredients of Chinese stellera roots Pending CN105315118A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510414030.1A CN105315118A (en) 2015-07-10 2015-07-10 Integrated extracting and separating method for active ingredients of Chinese stellera roots

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510414030.1A CN105315118A (en) 2015-07-10 2015-07-10 Integrated extracting and separating method for active ingredients of Chinese stellera roots

Publications (1)

Publication Number Publication Date
CN105315118A true CN105315118A (en) 2016-02-10

Family

ID=55243529

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510414030.1A Pending CN105315118A (en) 2015-07-10 2015-07-10 Integrated extracting and separating method for active ingredients of Chinese stellera roots

Country Status (1)

Country Link
CN (1) CN105315118A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109674747A (en) * 2019-01-25 2019-04-26 甘肃兰药药业有限公司 A kind of preparation method reducing girald daphne bark's injection toxic side effect
CN110100678A (en) * 2019-04-29 2019-08-09 山东省农业科学院植物保护研究所 A kind of control method of the late blight of potato
CN110960599A (en) * 2019-12-31 2020-04-07 西安交通大学医学院第二附属医院 Method for extracting total alkaloids of stellera chamaejasme and application thereof
CN112903876A (en) * 2021-03-02 2021-06-04 中国科学院兰州化学物理研究所 Method for extracting root soil and root allelochemical substances of stellera chamaejasme and detecting content of root allelochemical substances

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5616609A (en) * 1991-08-08 1997-04-01 Ikekawa; Tetsuro Carcinostatic compound and production thereof
CN1410424A (en) * 2002-09-18 2003-04-16 张杰克 Extraction technology of new stellerin A
CN1544433A (en) * 2003-11-20 2004-11-10 乐 周 Extracting and separating method of novel langdu root essence B from stellera chamaejasme L and its uses

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5616609A (en) * 1991-08-08 1997-04-01 Ikekawa; Tetsuro Carcinostatic compound and production thereof
CN1410424A (en) * 2002-09-18 2003-04-16 张杰克 Extraction technology of new stellerin A
CN1544433A (en) * 2003-11-20 2004-11-10 乐 周 Extracting and separating method of novel langdu root essence B from stellera chamaejasme L and its uses

Non-Patent Citations (6)

* Cited by examiner, † Cited by third party
Title
刘文粢等: "狼毒大戟的化学成分研究", 《中国中药杂志》 *
刘欣等: "瑞香狼毒的化学成分研究", 《中草药》 *
孙丽君等: "蒙药材瑞香狼毒的化学成分研究", 《天然产物研究与开发》 *
张天柱等: "瑞香狼毒生物活性成分的提取与分离、纯化方法", 《特产研究》 *
王亚维等: "瑞香狼毒杀虫活性成分的提取与分离", 《安徽农业科学》 *
韩文雪: "瑞香狼毒根部化学成分的研究", 《万方数据资源系统学术论文》 *

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109674747A (en) * 2019-01-25 2019-04-26 甘肃兰药药业有限公司 A kind of preparation method reducing girald daphne bark's injection toxic side effect
CN109674747B (en) * 2019-01-25 2022-03-08 甘肃兰药药业有限公司 Preparation method for reducing toxic and side effects of girald daphne bark injection
CN110100678A (en) * 2019-04-29 2019-08-09 山东省农业科学院植物保护研究所 A kind of control method of the late blight of potato
CN110960599A (en) * 2019-12-31 2020-04-07 西安交通大学医学院第二附属医院 Method for extracting total alkaloids of stellera chamaejasme and application thereof
CN110960599B (en) * 2019-12-31 2023-11-07 西安交通大学医学院第二附属医院 Extraction method and application of stellera chamaejasme total alkaloids
CN112903876A (en) * 2021-03-02 2021-06-04 中国科学院兰州化学物理研究所 Method for extracting root soil and root allelochemical substances of stellera chamaejasme and detecting content of root allelochemical substances
CN112903876B (en) * 2021-03-02 2022-04-01 中国科学院兰州化学物理研究所 Method for extracting root soil and root allelochemical substances of stellera chamaejasme and detecting content of root allelochemical substances

Similar Documents

Publication Publication Date Title
Heitzman et al. Ethnobotany, phytochemistry and pharmacology of Uncaria (Rubiaceae)
Hussain et al. The chemistry and biology of bicoumarins
CN106265754A (en) A kind of method that a chain of extraction obtains two kinds of effective ingredient from periplaneta americana
Wang et al. Annona squamosa Linn: cytotoxic activity found in leaf extract against human tumor cell lines
CN105315118A (en) Integrated extracting and separating method for active ingredients of Chinese stellera roots
CN107522680A (en) South America amphibious crab chrysanthemum antineoplastic extract and its production and use
CN101157717B (en) Preparation method of Ardisia mamillata B and uses thereof
Ding et al. Artemilavanolides A and B, two sesquiterpenoids with a 6-oxabicyclo [3.2. 1] octane scaffold from Artemisia lavandulaefolia
El-Askary et al. Quinic acid derivatives from Artemisia annua L. leaves; biological activities and seasonal variation
Wei et al. Antiproliferative piperidine alkaloids from giant taro (Alocasia macrorrhiza)
CN106946903A (en) One class drop diterpene compound, its extraction separation method and its application in antineoplastic is prepared
CN106619674A (en) Application of effective part or effective component of jasmines in preparation of medicine or health-care food for treating heterogeneitys and multi-factors' alzheimer's diseases
KR100313323B1 (en) Method for Extraction Isolation and Identification of trans-Resveratrol from Paeonia lactiflora Seeds
KR20130051142A (en) Medical composition comprising perilla frutescens extract for preventing or treating brain neuronal disease
CN103610682A (en) Preparation method of 3(alpha)-hydroxyl-30-olive-12,20(29)-diene-28-acid and application in preparing anti-tumor drug
Huang et al. Herbicidal activity and bioactive components of Brucea javanica (L.) Merr. residue
CN104829529B (en) Artabotrys pilosus total alkaloid extract and application thereof
Tsivileva et al. Fungal coumarins: biotechnological and pharmaceutical aspects
Sun Identification of diterpenoids from Icacina Oliviformis
CN113214154B (en) Tribenzyl isoquinoline alkaloid, preparation method, pharmaceutical composition and application thereof
CN102188459A (en) Brucea javanica total terpenoid extractive, and preparation method and application thereof
CN110204477B (en) Diterpene alkaloid with antioxidant effect and application thereof in preparation of medicines
Maryjane N et al. Isolation and Characterization of Glucocorticoid Steriod from the Leaf of Rauvolfia vomitoria
Xing et al. Inhibition of tumor cell proliferation by coleon C
Revathi et al. Antitumour activity of quercetin-3-o-β-glucoside isolated from Cansjera rheedii (Opiliaceae) against Dalton’s ascitic lymphoma

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
DD01 Delivery of document by public notice

Addressee: Li Yushan

Document name: the First Notification of an Office Action

DD01 Delivery of document by public notice
DD01 Delivery of document by public notice

Addressee: Li Yushan

Document name: Notification that Application Deemed to be Withdrawn

DD01 Delivery of document by public notice
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20160210

WD01 Invention patent application deemed withdrawn after publication