CN100439362C - Extracting and separating method of novel langdu root essence B from stellera chamaejasme L and its uses - Google Patents
Extracting and separating method of novel langdu root essence B from stellera chamaejasme L and its uses Download PDFInfo
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Abstract
The present invention relates to a method for extracting and separating novel radix euphorbiae ebracteolatae B from Daphnetin radix euphorbiae ebracteolatae and the application thereof. The novel radix euphorbiae ebracteolatae B is isolated and identified from the Daphnetin radix euphorbiae ebracteolatae, and the novel radix euphorbiae ebracteolatae B can suppress and kill various phytopathogen and has broad spectrum bactericidal activity ingredients. The present invention comprises the operating procedures that roots of the Daphnetin radix euphorbiae ebracteolatae are used as a raw material; 4 to 10 weight times of ethyl acetate or acetone or a mixture of the ethyl acetate and the acetone is used as a solvent; 30 to 55 DEG C of ultrasonic is used for 3 times of atmospheric pressure continuous extraction, and the extraction time of each time is 30 to 50 min. 60 to 99% of the novel radix euphorbiae ebracteolatae B is obtained from the extracting solution via filtration, concentration and chromatography laminar analysis.
Description
One, technical field:
The present invention relates to the comprehensive utilization of Stellera chamaejasme L. in a kind of medicine, veterinary drug and pesticide intermediate or the former medicine field, especially relate to the extraction and separation method of new stellerin B in a kind of Stellera chamaejasme L. and as the application of bactericide.
Two, background technology:
Stellera chamaejasme L. (Stellera Chamae jasme L.) is a thymelaeceae stellera plant, and another name has the root of langdu, Graceful Jessamine Herb etc., and its root is the matrix of traditional Chinese medicine viciousness, has dissipating bind to relieve oedema or abdominal distension through diuresis or purgation pain relieving and insecticidal action.The record that Stellera chamaejasme L. is used as botanical pesticide is just arranged in " the Chinese soil pesticide will " of nineteen fifty-nine publication, people imbedded the underground field subterranean pest-insect that is used to prevent and treat with the powder of chameajasme at that time, or the water extract of the root of langdu is sprayed at plant leaf surface was used to prevent and kill off blade face bean aphid, vegetable aphid, leaf rust etc.In recent years, there is the investigator to develop the former agricultural chemicals of the plant that contains root of langdu crude extract, the patent applied for that has in succession.But these root of langdu type botanical pesticides are sterilant, and a few has clear and definite effective constituent and content, then do not know its active insecticidal components in most of patent.Zhang Jie etc. (number of patent application 00116146) have invented by Hemp Eupatorium, Stellera chamaejasme L. and trifoliate jewelvine and have prepared the method that broad spectrum is given birth to insecticide, and the insecticide of this method preparation belongs to compound preparation, and its insecticidal active ingredient is unclear, and effective object does not contain phytopathogen.Zhang Kejie etc. (number of patent application 02133769) have narrated the technology that is prepared biological pesticide chamaejasmine aqueous emulsion by chameajasme, stem, and the product of this method preparation belongs to single preparations of ephedrine, and insecticidal active ingredient and content thereof are clear and definite, are 1.1%～5%.But its effective object only is a plant insect equally, does not contain phytopathogen.Liu Shigui etc. (number of patent application 02133971) disclose the method that is prepared vegetable insecticide by the root of langdu short extract, nimbin and Motherwort Herb alkaloid etc., the product that this method obtains is a compound preparation, wherein the effective constituent in the root of langdu extract is unclear, and effective object equally only is a plant insect.Han Mingli etc. (number of patent application 02100771.3) have narrated and have prepared 0.3% chamajasmin by Stellera chamaejasme L. and plant the extremely preparation method of aqua, and this product is a single preparations of ephedrine, and effective constituent is chamajasmin, and effective object still is plant insect just.Only relate to the crude extract of chameajasme in its production technique, and do not relate to the separation of chamajasmin.In sum, as can be seen, the root of langdu is mainly sterilant as the application of botanical pesticide, also belongs to blank about the research and development of its sterilant.
People such as Niwa (Tetrahydron Letters, 1984,25 (34): 3735-3738) the earliest from the Stellera chamaejasme L. root isolation identification go out new stellerin B.Feng Baomin is arranged subsequently, and (herbal medicine, 2001,32 (1): 14-15) etc. many people's research has confirmed people's such as Niwa result of study in succession.These researchs have common characteristic, promptly all are the fundamental research that belongs to vegetable chemistry or natural product chemistry, and its research method is breadboard ordinary method, and extraction efficiency is low, and the separation method complexity is loaded down with trivial details, is not suitable for commercial scale production.Secondly, seldom relate to its bioactive research all about the research report of new stellerin B, more not about new stellerin B to phytopathogen promptly as the research of bactericide.
Three, summary of the invention:
The present invention is in order to solve the weak point in the above-mentioned background technology; extraction and separation method and the application thereof of new stellerin B in a kind of Stellera chamaejasme L. are provided; its isolation identification from the Stellera chamaejasme L. root goes out a broad spectrum fungicide active ingredient that the various plants pathogenic bacteria is had inhibition and killing action; be new stellerin B; be fit to mass-producing extraction separation new stellerin B from chameajasme; production method and technology are easy, economical, reasonable; simultaneously, provide new stellerin B application as broad spectrum plant sterilization activeconstituents.
For achieving the above object, the technical solution used in the present invention is:
The extraction and separation method of new stellerin B in a kind of Stellera chamaejasme L., its special character is to comprise following operation steps: the chameajasme powder is added solvent extract, carry out the silica gel column chromatography rough segmentation first time then, get a rough segmentation thing, carry out the silica gel column chromatography rough segmentation second time again, get secondary rough segmentation thing, again secondary rough segmentation thing is carried out purifying.
The aforesaid operations step comprises: with the Stellera chamaejasme L. root is raw material, is solvent with the ethyl acetate of 4～10 times of weight or the mixture of acetone or ethyl acetate and acetone, adopts 30 ℃～55 ℃ ultrasonic wave normal pressures to extract 3 times continuously, each extraction time 30～50min.Extracting solution after filtration, concentrate and column chromatogram chromatography obtains 60%～99% new stellerin B.
The aforesaid operations step comprises:
(1) chameajasme is crushed to a certain degree, according to chameajasme grain weight amount (kg) and 1: 4～1: 10 ratio of solvent volume (L), adopt the intermittent type ultrasonic extraction, extract 30 ℃～55 ℃ of temperature, every batch of starting material adopt homogeneous solvent to extract 3 times continuously, and each extraction time is 30～50min, and ultrasonic power is 1.8W, each ultrasonic time is 6s, and twice timed interval between ultrasonic is 4s;
(2) after each extraction finishes, adopt centrifuging, collect filtrate, No. 3 extracting solutions are merged, after negative pressure is steamed and is desolventized, get crude extract, recovered solvent can use repeatedly, total extraction yield is different and different according to solvent types, is generally 7%～21%, and the content of new stellerin B is 5%～25% in the crude extract, crude extract need not separation and purification, can be directly used in preparation bactericide aqueous emulsion, also can select for use other organic solvents that this crude extract is carried out twice ultrasonic and extract, extract of gained crude extract or second extract are used for the rough segmentation of new stellerin B;
(3) with acetone or methyl alcohol or the mixture of the two dissolving crude extract, be made into the solution of mass concentration about 20%, under constantly stirring, add the about 200 purpose column chromatography silica gels that are equivalent to 3～7 times of quality of crude extract, the silica gel of mixing behind the sample is dried at normal temperatures, be added to the top of silicagel column, carry out dry chromatography, adopt chloroform, ethyl acetate to carry out wash-out successively, collect ethyl acetate stream part, negative pressure gets a rough segmentation thing after steaming and desolventizing, new stellerin B content in this rough segmentation thing is 45%～55%, can be directly used in the medical or disinfectant use in agriculture of preparation;
(4) a rough segmentation thing employing and (3) similar method are carried out column chromatography, different is to adopt the mixed solvent of chloroform-acetone 7: 3 (V/V) as eluent, with new stellerin B standard substance is contrast, adopt TLC method or HPLC method that each stream part is detected, merge stream part of containing new stellerin B, negative pressure gets secondary rough segmentation thing after steaming and desolventizing, new stellerin B content in this rough segmentation thing is 80%～90%, can be directly used in the medical or disinfectant use in agriculture of preparation;
(5) with dissolve with methanol secondary rough segmentation thing, last sephadex LH-20 post carries out purifying, collects stream part of containing new stellerin B, and negative pressure gets new stellerin B elaboration after steaming and desolventizing, and content is 95%～99%, can be used as standard model or analytical pure chemical reagent and uses.
In the above-mentioned steps (1), extract solvent and select a kind of in chloroform, ethyl acetate, acetone, ethanol or the methyl alcohol for use, extraction scheme comprises: A. directly carries out supersound extraction with ethyl acetate or acetone, material (kg)/liquid (L) is than being controlled at 1: 4～1: 10,, extracting temperature is 30 ℃～55 ℃, the gained crude extract is faint yellow amorphism powder, contain 5%～10% new stellerin B, be directly used in column chromatography for separation.The extraction yield of ethyl acetate and acetone is respectively 5%～6% and 7%～8%; B. at first adopt methyl alcohol to carry out supersound extraction, extraction conditions is with the ethyl acetate method, the gained crude extract can be directly used in preparation bactericide or second extraction, this extraction yield is 18%～25%, with acetone methanol crude extract is carried out twice ultrasonic and extracts, and extraction conditions is with the ethyl acetate method, gained acetone crude extract is equivalent to 10%～12% of used vegetable material, be yellow amorphism powder, contain 5%～10% new stellerin B, be directly used in column chromatography for separation.
In the above-mentioned steps (2), crude extract is made into the solution of mass concentration about 20% with acetone, the column chromatography silica gel that adds 3～7 times of quality, room temperature is dried the silica gel mixed behind the sample or with 40 ℃ of hot blast constant pressure and dries, be added to the silicagel column top then and carry out the dry chromatography rough segmentation first time, the specification of silicagel column is: height/diameter 10: 1, the granularity of silica gel stopping composition is 100～300 orders, its consumption is 1～3 times of applied sample amount, at first adopt chloroform to carry out wash-out, till effluent liquid is almost colourless, use eluent ethyl acetate then instead, detect no new stellerin B outflow until TLC or HPLC, combined ethyl acetate stream part, get a rough segmentation thing after steaming desolventizes, its quality is about 40%～50% of applied sample amount.The new stellerin B content of this rough segmentation thing is 45%～55%.
In the above-mentioned steps (3), a rough segmentation thing is made into saturated solution with acetone, is added to the silicagel column top post silica gel column chromatography that wets, the specification of silicagel column is: height/diameter 20: 1.The granularity of silica gel stopping composition is 100～300 orders, its consumption is 50～100 times of applied sample amount, with the mixed solvent of chloroform-acetone 7: 3 (V/V) as eluent, collection contains main stream part of new stellerin B, after desolventizing, steaming gets secondary rough segmentation thing, yellow amorphism powder, its quality is about 40%～50% of applied sample amount, and the content of new stellerin B is 80%～90%.
In the above-mentioned steps (4), secondary rough segmentation thing is made into saturated solution with methyl alcohol, and the sephadex LH-20 that crosses with the methyl alcohol balance in advance carries out purifying, the specification of pillar is: height/diameter 10: 1, the granularity of sephadex LH-20 is 200～400 orders, applied sample amount is 50～100 times of sephadex LH-20 consumption in the post, with methyl alcohol is eluent, concentrating under reduced pressure contains stream part of new stellerin B, get new stellerin B elaboration, its quality is about 85%～90% of applied sample amount, and it is raw-material 0.5%～1.5% that the total recovery of whole technology is equivalent to chameajasme, and purity is 95%～99%.
The physical parameter of above-mentioned new stellerin B is as follows:
New stellerin B, faint yellow unformed solid, mp261 ℃ (decomposition), [α]
D=+161.685 ° (c 0.089, EtOH), UV (MeOH, nm): λ
Max298,221.IR(KBr)：υ
maxcm
-13422(O-H)，1640(C＝O)，1517(C＝C)，1254、1160、1088(C-O)。FAB?MS?e/z：541([M+1]
+，100)，272([1/2M+1]
+，42)。
1H NMR δ (CD
3COCD
3): 2.91 (4H, s, br, HO-7, HO-7 ", HO-4 ', HO-4 " '), 3.15 (1H, d, J=4.4Hz, H-3), 3.40 (1H, d, J=7.2Hz, H-3 "), 5.14 (1H, d, J=8.4Hz, H-2 "), 5.75 (1H, d, J=4.8Hz, H-2), 5.86 (2H, s, H-6, H-6 "), 5.95 (1H; d, J=2.0Hz, H-8 or H-8 "), 6.08 (1H, d, J=2.0Hz, H-8 or H-8 "); 11.69 (1H, s, HO-5 "), 11.97 (1H, s, HO-5).Below be H-2 ', H-2 ", H-3 ', H-3 " and, H-5 ', H-5 ", H-6 ', H-6 ": 6.76 (2H, d, J=8.4Hz), 6.89 (2H, d, J=8.4Hz), 7.00 (2H, d, J=8.4Hz), 7.28 (2H, d, J=8.8Hz).
13CNMR?δ(CD
3COCD
3)：48.27，49.14(C-3，C-3″)，80.15，82.07(C-2，C-2″)，95.38，95.10(C-8，C-8″)，96.37，96.16(C-6，C-6″)，103.02，104.07(C-10，C-10″)，115.39，115.65(C-3′，C-3″′)，127.51，127.78(C-1′，C-1″′)，127.89，129.21(C-2′，C-2″′)，157.63，157.93(C-4′，C-4″′)，162.17，164.05(C-9，C-9″)，166.97，166.76(C-7，C-7″)，195.37，197.49(C-4，C-4″)。
HPLC collection of illustrative plates: eluent CH
3OH/H
2O (V/V) 47: 5, Waters ALC/JPC-201 high pressure liquid chromatograph, pillar are Nova.Pak C18,150mm * 4mm (i.d), particle diameter 4.5 μ m, flow velocity 0.7mlmin
-1, UV-detector detects wavelength 296nm.
New stellerin B is as the application of bactericide in a kind of Stellera chamaejasme L., its special character is: described sterilant is a raw material with the Stellera chamaejasme L. root extract, with new stellerin B is main bactericidal active ingredient, be used for prevention and treatment by dry rot of apple bacterium (Bakeri Rehm), fusarium graminearum (Fusarium graminearum), tomato early blight bacterium (Alternariasolani), pumpkin wilt (Fusarium bulbigenum), Exserohilum turcicum (Exserohilum turcicum), the Plant diseases that tobacco brown spot pathogen (Alternaria alternata) and Phytophthora capsici germ (Phytophthora capsici.) etc. causes.
Above-mentioned new stellerin B is 2200mgL
-1Concentration.
Compared with prior art, the advantage and the effect that have of the present invention is as follows:
The present invention adopts biological activity tracing and fractionation first, and isolation identification goes out one and the various plants pathogenic bacteria had suppresses and the broad spectrum fungicide active ingredient of killing action from the Stellera chamaejasme L. root, i.e. new stellerin B (chamaechromone).Simultaneously, develop the production technique of extraction separation new stellerin B from chameajasme, the extraction efficiency height, separation method is simple, is suitable for commercial scale production, and first new stellerin B is used as bactericide.
Four, description of drawings:
Fig. 1 is a process flow sheet of the present invention;
Fig. 2 is the chemical structural formula of new stellerin B;
Fig. 3 is the HPLC collection of illustrative plates of new vicious plain B.
Five, embodiment:
1, referring to Fig. 1, the present invention adopts 4 footworks to obtain the new stellerin B of different content, i.e. extraction, silica gel column chromatography rough segmentation for the first time, the silica gel column chromatography rough segmentation second time, sephadexLH-20 purifying, the content that each step is separated the new stellerin B in the target compound that obtains is respectively 5%～25%, 45%～55%, 80%～90%, 95%～99%.Its technical process is as follows:
1.1, chameajasme is crushed to a certain degree, its fineness does not have strict demand, is generally diameter 1mm.According to chameajasme grain weight amount (kg) and 1: 8 ratio of solvent volume (L), adopt the intermittent type ultrasonic extraction, extracting temperature is 40 ℃.Every batch of starting material adopt homogeneous solvent to extract 3 times continuously, and each extraction time is 40min.Ultrasonic power is 1.8W, and each ultrasonic time is 6s, and twice timed interval between ultrasonic is 4s.If to separate new stellerin B elaboration is final purpose, 1: 1 (V/V) is solvent to select ethyl acetate or acetone or ethyl acetate/acetone for use.If to be used to prepare the Stellera chamaejasme L. sterilant be final purpose to extract thick extraction, then selecting methyl alcohol for use is solvent.
1.2, the solid-liquid separation when extracting, can adopt one of negative pressure filtration, centrifuging or three kinds of methods of squeeze and filter, preferably adopt centrifuging.Filtrate is reduced pressure through water pump, after 38 ℃ steaming desolventizes down, gets crude extract.Recovered solvent can use repeatedly.Total extraction yield is different and different according to solvent types, and the extraction yield of ethyl acetate, acetone and methyl alcohol is respectively 5.2%, 6.4% and 21%.The content of new stellerin B approximately is respectively 20%, 6% and 5% in three kinds of crude extracts.Three kinds of crude extracts need not separation and purification, all can be directly used in preparation bactericide aqueous emulsion.If to separate new stellerin B elaboration is final purpose, then select ethyl acetate or acetone extract for use.
1.3, the thick extraction of ethyl acetate or acetone carried out first time during silica gel column chromatography, selection acetone solution crude extract is made into the solution of mass concentration about 20%.Then, add the about 200 purpose column chromatography silica gels that are equivalent to 3～7 times of quality of crude extract, after mixing thoroughly fast, normal temperature dries.Be added to the top of 1/8 the silicagel column that is equivalent to mix sample silica gel quality, carry out dry chromatography.Adopt chloroform, ethyl acetate to carry out wash-out successively.New stellerin B is present in ethyl acetate stream part, after water pump removes solvent under reduced pressure, gets a rough segmentation thing.New stellerin B content in this rough segmentation thing is 45%～55%, can be directly used in the medical or disinfectant use in agriculture of preparation, also can be used as the former medicine of disinfectant use in agriculture and sells.
1.4, when a rough segmentation thing is carried out silica gel column chromatography, adopt conventional dry chromatography.Adopt the mixed solvent dress post of chloroform-acetone 7: 3 (V/V), simultaneously again as eluent.With new stellerin B standard substance is contrast, adopts TLC method or HPLC method that each stream part is detected.Merge all stream parts of containing new stellerin B, negative pressure gets secondary rough segmentation thing after steaming and desolventizing.New stellerin B content in this rough segmentation thing is 80%～90%, can be directly used in the medical or disinfectant use in agriculture of preparation.
1.5, adopt sephadex LH-20 gel chromatography to carry out to the purifying of secondary rough segmentation thing.The specification of pillar is: height/diameter 10: 1.The granularity of sephadex LH-20 is 300 orders.Applied sample amount is 1/50 times of sephadex LH-20 consumption in the post.With methyl alcohol is eluent, collect to merge the stream part that only contains new stellerin B, can obtain new stellerin B elaboration behind the concentrating under reduced pressure, and its yield is about 85%～90% of applied sample amount, and it is raw-material 0.5%～1.5% to be equivalent to chameajasme, and purity is 95%～99%.
2, new stellerin B is as the application of bactericide
The present invention has found the new role of new stellerin B aspect plant sterilization and new purposes first, has filled up the root of langdu and the new stellerin B research blank aspect plant sterilization.Result of study confirms that new stellerin B is at 2200mgL
-1Concentration is to dry rot of apple bacterium (Bakeri Rehm), fusarium graminearum (Fusarium graminearum), tomato early blight bacterium (Alternariasolani), pumpkin wilt (Fusarium bulbigenum), Exserohilum turcicum (Exserohilum turcicum), the inhibiting rate of tobacco brown spot pathogen (Alternaria alternata) and Phytophthora capsici germ phytopathogens such as (Phytophthora capsici.) is respectively 81.1%, 80.0%, 77.3%, 87.8%, 98.5%, 96.8%, 81.0%.Therefore, new stellerin B is expected to become new botanical disinfectant use in agriculture.
3, referring to Fig. 2, Fig. 2 is the chemical structural formula of new stellerin B, and physical parameter is as follows: new stellerin B, faint yellow unformed solid, mp261 ℃ (decomposition), [α]
D=+161.685 ° (c 0.089, EtOH), UV (MeOH, nm): λ
Max298,221.IR(KBr)：υ
maxcm
-13422(O-H)，1640(C＝O)，1517(C＝C)，1254、1160、1088(C-O)。FAB?MS?e/z：541([M+1]
+，100)，272([1/2M+1]
+，42)。
1H NMR δ (CD
3COCD
3): 2.91 (4H, s, br, HO-7, HO-7 ", HO-4 ', HO-4 " '), 3.15 (1H, d, J=4.4Hz, H-3), 3.40 (1H, d, J=7.2Hz, H-3 "), 5.14 (1H, d, J=8.4Hz, H-2 "), 5.75 (1H, d, J=4.8Hz, H-2), 5.86 (2H, s, H-6, H-6 "), 5.95 (1H; d, J=2.0Hz, H-8 or H-8 "), 6.08 (1H, d, J=2.0Hz, H-8 or H-8 "); 11.69 (1H, s, HO-5 "), 11.97 (1H, s, HO-5).Below be H-2 ', H-2 ", H-3, H-3 " and, H-5 ', H-5 ", H-6 ', H-6 ": 6.76 (2H, d, J=8.4Hz), 6.89 (2H, d, J=8.4Hz), 7.00 (2H, d, J=8.4Hz), 7.28 (2H, d, J=8.8Hz).
13CNMRδ(CD
3COCD
3)：48.27，49.14(C-3，C-3″)，80.15，82.07(C-2，C-2″)，95.38，95.10(C-8，C-8″)，96.37，96.16(C-6，C-6″)，103.02，104.07(C-10，C-10″)，115.39，115.65(C-3′，C-3″′)，127.51，127.78(C-1′，C-1″′)，127.89，129.21(C-2′，C-2″′)，157.63，157.93(C-4′，C-4″′)，162.17，164.05(C-9，C-9″)，166.97，166.76(C-7，C-7″)，195.37，197.49(C-4，C-4″)。
Referring to Fig. 3, HPLC collection of illustrative plates: eluent CH
3OH/H
2O (V/V) 47: 5, WatersALC/JPC-201 high pressure liquid chromatograph, pillar are Nova.Pak C18,150mm * 4mm (i.d), particle diameter 4.5 μ m, flow velocity 0.7mlmin
-1, UV-detector detects wavelength 296nm.
Claims (1)
1, the extraction and separation method of new stellerin B in a kind of Stellera chamaejasme L. is characterized in that comprising following operation steps:
(1) chameajasme is pulverized, according to chameajasme grain weight amount kg and 1: 4～1: 10 ratio of solvent volume L, adopt the intermittent type ultrasonic extraction, extract 30 ℃～55 ℃ of temperature, every batch of starting material adopt the mixture of ethyl acetate or acetone or ethyl acetate and acetone to extract 3 times continuously, and each extraction time is 30～50min, and ultrasonic power is 1.8W, each ultrasonic time is 6s, and twice timed interval between ultrasonic is 4s;
(2) after each extraction finishes, adopt centrifuging, collect filtrate, No. 3 extracting solutions are merged, and negative pressure gets crude extract after steaming and desolventizing, recovered solvent can use repeatedly, total extraction yield is different and different according to solvent types, is generally 7%～21%, and the content of new stellerin B is 5%～25% in the crude extract;
(3) with acetone or methyl alcohol or the mixture of the two dissolving crude extract, be made into the solution of mass concentration about 20%, under constantly stirring, add the 200 purpose column chromatography silica gels that are equivalent to 3～7 times of quality of crude extract, the silica gel of mixing behind the sample is dried at normal temperatures, be added to the top of silicagel column, carry out dry chromatography, adopt chloroform, ethyl acetate to carry out wash-out successively, collect ethyl acetate stream part, negative pressure gets a rough segmentation thing after steaming and desolventizing, and the new stellerin B content in this rough segmentation thing is 40%～50%;
(4) a rough segmentation thing employing and the similar method of step 3 are carried out column chromatography, different is to adopt the mixed solvent of 7: 3 volume ratios of chloroform-acetone as eluent, with new stellerin B standard substance is contrast, adopt TLC method or HPLC method that each stream part is detected, merge stream part of containing new stellerin B, negative pressure gets secondary rough segmentation thing after steaming and desolventizing, and the new stellerin B content in this rough segmentation thing is 80%～90%;
(5) with dissolve with methanol secondary rough segmentation thing, last dextran LH-20 post carries out purifying, collects stream part of containing new stellerin B, and negative pressure gets new stellerin B elaboration after steaming and desolventizing, and content is 90%～95%.
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| CN102060827A (en) * | 2010-12-30 | 2011-05-18 | 苏州瑞蓝博中药技术开发有限公司 | Method for extracting new chamaejasmine B from stellera chamaejasme. L |
| CN103183596B (en) * | 2012-11-20 | 2015-05-06 | 北京农学院 | Novel aliphatic ketone compound having acaricidal activity |
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| CN104610214B (en) * | 2013-11-04 | 2017-02-08 | 中国科学院大连化学物理研究所 | Method for rapidly preparing six compounds in Stellera chamaejasme L. |
| CN103858877B (en) * | 2014-03-17 | 2016-02-10 | 赵伟 | Biological bactericide neochamaejasmine B water dispersible granules and preparation method thereof |
| CN105315118A (en) * | 2015-07-10 | 2016-02-10 | 李玉山 | Integrated extracting and separating method for active ingredients of Chinese stellera roots |
| CN107114414A (en) * | 2017-05-25 | 2017-09-01 | 中国科学院西北高原生物研究所 | The application of the anti-Wolfberry Aphid of The Leaves And Stems of Stellera Chamaejasme extract |
| CN107787991A (en) * | 2017-09-29 | 2018-03-13 | 山西德威本草生物科技有限公司 | A kind of matrine and chamaejasmine compound synergistic bactericidal agent, preparation method and applications |
| 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 |
| CN113475534B (en) * | 2021-07-26 | 2022-11-22 | 海南师范大学 | Morinda citrifolia sterilizing preparation and preparation method thereof |
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| CN1410424A (en) * | 2002-09-18 | 2003-04-16 | 张杰克 | Extraction technology of new stellerin A |
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