CN107056644A - A kind of method and its application that 2 phenyl acetamide compounds are extracted from lepidii,semen - Google Patents
A kind of method and its application that 2 phenyl acetamide compounds are extracted from lepidii,semen Download PDFInfo
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- CN107056644A CN107056644A CN201710382069.9A CN201710382069A CN107056644A CN 107056644 A CN107056644 A CN 107056644A CN 201710382069 A CN201710382069 A CN 201710382069A CN 107056644 A CN107056644 A CN 107056644A
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- A61K31/00—Medicinal preparations containing organic active ingredients
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- A61K31/165—Amides, e.g. hydroxamic acids having aromatic rings, e.g. colchicine, atenolol, progabide
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Abstract
The present invention relates to the method and its application that 2 phenyl acetamide compounds are extracted from lepidii,semen, effectively solve to extract 2 phenyl acetamide compounds from lepidii,semen and its preparing the pharmaceutical problems for the treatment of estrogen deficiency, method is, the water of 10 times of weight is added to extract three times by lepidii,semen is fried, merge No. three extract solutions, it is concentrated under reduced pressure into medicinal extract, medicinal extract ethanol alcohol precipitation, abandon precipitation, by supernatant centrifugal filtration, it is concentrated into no alcohol taste, the upper posts of Dianion HP 20, water is used successively, 20% ethanol, 40% ethanol elution, collect 40% alcohol elution, with the discrete dissolving of water, centrifugal filtration, concentration, cross the chromatographic columns of Toyopearl HW 40, eluted successively with water and 10% methanol aqueous solution, collect 10% methanol aqueous solution elution fraction, dissolved with methanol, stand 24h, separate out colourless crystallization, dry, obtain 2 phenyl acetamides, the inventive method novel and unique, it is easy to operate, medicine effective for preparing treatment estrogen deficiency, the medical value and commercial value of lepidii,semen are opened up.
Description
Technical field
The present invention relates to medicine, it is particularly a kind of from lepidii,semen extract 2- phenyl acetamide compounds method and its should
With.
Background technology
Phytoestrogen is derived from plant, has similar structure to the beta estradiol of steroid hormone -17 of mammal
Polyol.Natural phytoestrogen is compared to the estrogen of synthesis, and its estrogenic activity is low, but caused
The side effect such as breast cancer, carcinoma of endometrium it is also less, using can be safer.Therefore to the research containing phytoestrogen gradually
As focus.
Lepidium seed is parts of generic medicinal plants, first recorded in《Sheng Nong's herbal classic》, low-grades are classified as, the flavour of a drug are pungent, hardship, in property Great Cold, return
Lung and bladder warp, have effects that to lead off relieving asthma, line water detumescence.2015 editions《Chinese Pharmacopoeia》" lepidium seed " included have north and south it
Point, wherein crucifer Lepidium apetalum LepidiumapetalumWilld. dry mature seed, which is practised, claims " lepidii,semen ",
And Descurainia sophia Descurainiasophia (L.) WebbexPrantl. dry mature seed is practised and claims " descurainiae,semen ".Although southern
Lepidii,semen all does certified products lepidium seed use, but its plant origin, appearance character and pharmacological activity difference.It is not related to
The open report that 2- phenyl acetamides compound is extracted from lepidii,semen and its is applied in estrogenic is prepared.
The content of the invention
For above-mentioned situation, to overcome the defect of prior art, the purpose of the present invention is just to provide one kind from lepidii,semen
The method and its application of middle extraction 2- phenyl acetamide compounds, can effectively solve to extract 2- phenyl acetamide chemical combination from lepidii,semen
Thing and its pharmaceutical problems in preparation treatment estrogen deficiency.
The technical scheme that the present invention is solved is, it is a kind of 2- phenyl acetamide compounds are extracted from lepidii,semen method be,
Lepidii,semen 7.5-8.5kg will be fried, adds the water of 10 times of weight to extract every time three times, each 1.5h merges No. three extract solutions, decompression
Be concentrated into 260-280g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 19-21L alcohol precipitation 2h, abandons precipitation, by supernatant from
The heart is filtered, and is concentrated into no alcohol taste (about 1000ml), the upper Dianion HP-20 posts (absorption of highly porous styrene/desorption tree
Fat), successively with water 20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h collects 40% alcohol elution,
With the discrete dissolving of water, centrifugal filtration is concentrated into 30-40ml, Toyopearl HW-40 chromatographic columns is crossed, successively with water 3L and volume
The methanol aqueous solution 3L of concentration 10% is eluted, and flow velocity 8mL/min, the methanol aqueous solution elution fraction of collected volume concentration 10% uses first
Alcohol is dissolved, and stands 24h, separates out colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and is dissolved again with methanol, is stood
24h, so repeatedly 5 times, it is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
Prepared product 2- phenyl acetamides can be effectively used for preparing the medicine for the treatment of estrogen deficiency, realize 2- phenyl acetamides
It is used as application of the sole active agent in treatment estrogen deficiency disease drug is prepared.
The inventive method novel and unique, it is easy to operate, it can be effectively used for preparing 2- phenyl acetamides from lepidii,semen, and effectively
Medicine for preparing treatment estrogen deficiency, has opened up the new way for the treatment of estrogen deficiency, has opened up lepidii,semen
Medical value and commercial value, have good economic and social benefit.
Embodiment
The embodiment to the present invention elaborates with reference to embodiments.
Embodiment 1
The present invention is in specific implementation, and a kind of method that 2- phenyl acetamide compounds are extracted from lepidii,semen is to fry
Lepidii,semen 8kg, adds the water of 10 times of weight to extract three times every time, and each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into 270g
Medicinal extract, medicinal extract volumetric concentration be 80% ethanol 20L alcohol precipitation 2h, abandon precipitation, supernatant centrifugal filtration be concentrated into
1000ml (no alcohol taste), upper Dianion HP-20 posts (absorption of highly porous styrene/desorption resin), successively with water 20L,
20% ethanol 60L, 40% ethanol 60L are eluted, flow velocity 20L/24h, collect 40% alcohol elution, with the discrete dissolving of water, from
The heart is filtered, and is concentrated into 35ml, Toyopearl HW-40 chromatographic columns is crossed, successively with water 3L and the methanol aqueous solution of volumetric concentration 10%
3L is eluted, and flow velocity 8mL/min, the methanol aqueous solution elution fraction of collected volume concentration 10% is dissolved with methanol, stands 24h, is separated out
Colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and is dissolved again with methanol, is stood 24h, so repeatedly 5 times, is obtained nothing
Color crystallization is 2- phenyl acetamides, and mass content reaches more than 95%.
Embodiment 2
The present invention is in specific implementation, and a kind of method that 2- phenyl acetamide compounds are extracted from lepidii,semen is to fry
Lepidii,semen 7.5kg, adds the water of 10 times of weight to extract three times every time, and each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into
260g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 19L alcohol precipitation 2h, abandons precipitation, supernatant centrifugal filtration is concentrated into
Without alcohol taste, upper Dianion HP-20 posts (absorption of highly porous styrene/desorption resin), successively with water 20L, 20% ethanol
60L, 40% ethanol 60L are eluted, flow velocity 20L/24h, collect 40% alcohol elution, with the discrete dissolving of water, centrifugal filtration is dense
30ml is reduced to, Toyopearl HW-40 chromatographic columns are crossed, is eluted successively with the water 3L and methanol aqueous solution 3L of volumetric concentration 10%, stream
Fast 8mL/min, the methanol aqueous solution elution fraction of collected volume concentration 10%, is dissolved with methanol, stands 24h, separates out colourless crystallization,
Upper solution is suctioned out, colourless crystallization is dried, and is dissolved again with methanol, stand 24h, so repeatedly 5 times, obtaining colourless crystallization is
2- phenyl acetamides, mass content reaches more than 95%.
Embodiment 3
The present invention is in specific implementation, and a kind of method that 2- phenyl acetamide compounds are extracted from lepidii,semen is to fry
Lepidii,semen 8.5kg, adds the water of 10 times of weight to extract three times every time, and each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into
280g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 21L alcohol precipitation 2h, abandons precipitation, supernatant centrifugal filtration is concentrated into
Without alcohol taste (about 1000ml), upper Dianion HP-20 posts (absorption of highly porous styrene/desorption resin) use water successively
20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h collect 40% alcohol elution, discrete molten with water
Solution, centrifugal filtration is concentrated into 40ml, Toyopearl HW-40 chromatographic columns is crossed, successively with water 3L and the methanol-water of volumetric concentration 10%
Solution 3L is eluted, and flow velocity 8mL/min, the methanol aqueous solution elution fraction of collected volume concentration 10% is dissolved with methanol, stands 24h,
Separate out colourless crystallization, upper solution is suctioned out, colourless crystallization dry, dissolved again with methanol, stand 24h, so repeatedly 5 times,
It is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
Colourless crystallization prepared by embodiment 1-3, through liquid chromatography for measuring, is accredited as 2- phenyl acetamides, and through experiment,
With estrogen-like action, obtain fully proving effective for preparing treatment estrogen deficiency disease drug, and through experiment, it is relevant
Data is as follows：
1 instrument and material
Nuclear magnetic resonance is used with the NMRs of Bruker AVANCE III 500 (TMS internal standards) (Bruker), infrared spectrum
The Microscope Spectrometer of Nicolet is 10 (Thermo Scientific, USA), high resolution mass spectrum is used
Bruker maxis HD mass spectrometer, ultraviolet spectra Shimadzu UV-2401PC apparatus, efficiently
Phase chromatography-use Waters Alliance 2695 efficient liquid phase systems of series, are equipped with 2998 type PDADs,
Empower3 Data Processing in Chromatography Workstation, LC50 type high pressure preparative liquid chromatographs, [match spectrum is sharp to think (north to UV200 types UV-detector
Capital) Science and Technology Ltd.], YMC-PackODS-A chromatographic columns (250 × 10mm.D.S-5mm, 12mm) (YMC Co., Ltds), its
It is remaining to have N-1100 types Rotary Evaporators (Shanghai Ai Lang Instrument Ltd), A-1000S type current air exhauster (Shanghai Ai Lang instruments
Co., Ltd), N-1111 types freezing water circle device (Shanghai Ai Lang Instrument Ltd), FDU-2110 type freeze driers
(Shanghai Ai Lang Instrument Ltd), DFZ-60508 types vacuum drying chamber (Shanghai Yiheng Scientific Instruments Co., Ltd), AB204-
N a ten thousandths analytical precision balances (METTLER TOLEDO), iMARK type ELIASAs (U.S. BIO-RAD), carbon dioxide culture
Case (Shanghai STIK), superclean bench (Su Jing groups), the super combined Superpure water machines (SARTORIUS) of Arium 611VF are fallen
Put microscope (Nikon), PB-10 acidometers (German Sai Duolisi groups).
Column chromatography filler Diaion HP-20, MCI Gel CHP-20 (Mitsubishi chemical company), Toyopearl HW-
40 (Japanese TOSOH companies), Sephadex LH-20 (Parmacia Biotech companies), column chromatography used silica gel H (160-
200 mesh) produced for Haiyang Chemical Plant, Qingdao, culture dish, 96 well culture plates, cell cryopreservation tube (Corning companies), chromatogram used
The friendly fine chemicals Co., Ltd production of pure reagent position α Cygni, AR used is that Beijing Chemical Plant and Tianjin the 3rd are changed
Learn chemical reagent work's production.Remove estrogen hyclone (Guangzhou Chinese holly)；Without phenol red DMEM high glucose mediums, glucan-activated carbon
Remove hormone hyclone (Hyclone)；17 beta estradiols (17 β-estrogen, E2), ampicillin, Tris alkali (Sigma)；
Estradiol valerate tablet (Bayer medicine)；EDTA, MTT and DMSO (Amresco)；E2, FSH, LH ELISA kit (R＆D).
Cleaning grade Kunming mouse, female, birth 21 days (just ablactation), 9~12g of body weight is purchased from Beijing dimension tonneau China real
Test zoo technical Co., Ltd (credit number：SCXK (capital) 2016-0011).Human breast cancer cell (MCF-7) is purchased from middle traditional Chinese medical science
Subject institute Institute of Basic Medical Sciences's cell resource center.
Lepidii,semen picked up from Nanyang, henan in 2014, was identified through Henan College Of Traditional Chinese Medicine professor Chen Suiqing and professor Dong Chengming
For crucifer Lepidium apetalum LepidiumapetalumWilld. dry mature seed.
2 Experimental agents
The 2- phenyl acetamides that the inventive method is prepared from lepidii,semen is fried.
3 experimental methods
The weightening experiment of 3.1 Mouse Uterus
By mouse by the balanced and random principle packet of body weight, it is administered continuously 7 days.The daily distilled water 0.02mL/g of normal group
Gavage；The positive controls next day gavage Estradiol Valerate (0.33mg/kg/d) gavage；2- phenyl acetamides are extracted in lepidii,semen to press
0.5mg/10g/d, is made into suspension, and 0.02mL/g gavages are pressed daily.After last time administration 24h, pluck eyeball and take blood, take off cervical vertebra
Mouse is put to death, uterus is won immediately and is weighed, Uterine coefficient (uterine wet weight × (body weight) is calculated-1× 100%).Test parallel repetition
Three times.As a result compared with normal group, P values are calculated, investigation has not statistically significant.
3.2 MCF-7 cell proliferation experiments
MCF-7 cells through containing 5% go estrogen hyclone without phenol red DMEM medium cultures 1 week after, choose logarithm
Growth period cell, PBS is washed twice, after 0.05% Trypsin Induced, is added without the piping and druming of phenol red DMEM culture mediums uniformly, with 2
×104Individual/mL concentration is inoculated in 96 orifice plates, and per hole, culture cumulative volume is 200 μ L.24h is cultivated after after cell attachment, is changed to
Continue to cultivate containing (10 μM) of 2- phenyl acetamides nutrient solution is extracted in lepidii,semen.37 DEG C, 5%CO2Cultivate after 48h, added per hole
The μ L of MTT solution (5mg/mL) 20,37 DEG C are continued to cultivate 4h, and carefully exhausted nutrient solution, and 150 μ LDMSO are added per hole, shakes 5-
10min, is completely dissolved purple crystal.Each hole absorbance (A) is determined under 490nm with ELIASA, average A-value is calculated and thin
Born of the same parents' vigor.Experiment is parallel in triplicate.
Cell viability=each group OD values/normal group OD values
3.3 ELISA method detection blood serum E2s, LH, FSH
Mouse plucks eyeball and takes blood, and blood is stored at room temperature after 1h, and 3000 leave heart 10min, take supernatant.According to ELISA reagents
Box specification is carefully operated.
4 statistical dispositions
Experimental data withRepresent, with the statistical software processing datas of SPSS 20.0, using one-way analysis of variance
(One-Way ANOVA) carries out the comparison of group difference, with P<0.05 is that difference has significant, with P<0.01 has for difference
Pole significant.
5 experimental results
Influence of the 2- phenyl acetamides to sex immature female mice Uterine coefficient is extracted in 5.1 lepidii,semens
Sex immature female mice uterus system can significantly be induced by extracting 2- phenyl acetamides compared with normal group, in lepidii,semen
Several increase (P<0.05).Point out to extract 2- phenyl acetamides in lepidii,semen in vivo with estrogen-like action.It is shown in Table 1.
Influence of the 2- phenyl acetamides to sex immature female mice Uterine coefficient is extracted in the lepidii,semen of table 1
Note:Compared with normal group, represent P<0.05, represent P<0.01.
2- phenyl acetamides are extracted in 5.2 lepidii,semens to MCF-7 cell proliferations
Extracted in lepidii,semen 2- phenyl acetamides at 10 μM with normal group ratio, have to MCF-7 cells and significant promote propagation
Act on (P<0.05).Point out to extract 2- phenyl acetamides in lepidii,semen in vitro with estrogen-like action.It is shown in Table 2.
The influence that 2- phenyl acetamides are bred to MCF-7 cells is extracted in the lepidii,semen of table 2
Influence of the 2- phenyl acetamides to blood serum E2, LH, FSH is extracted in 5.3 lepidii,semens
Mice serum E2, LH level can be dramatically increased by extracting 2- phenyl acetamides compared with normal group, in lepidii,semen, but
Have substantially no effect on the level (P of serum FSH<0.05).Extract 2- phenyl acetamides in prompting lepidii,semen has estrogen-like in body
Effect, may increase internal E2 with it and LH level is relevant.It is shown in Table 3.
Influence of the 2- phenyl acetamides to blood serum E2, LH, FSH is extracted in the lepidii,semen of table 3
Note:Compared with normal group, represent P<0.05, represent P<0.01.
Contain substantial amounts of ERs (ERs) in uterus, estrogenic chemicalses can induce son by being combined with this receptor
The increase of palace target protein (IPs) content, shows as uterine tissue hyperplasia etc., thus can by determine exogenous hormone to property not into
Ripe Mouse Uterus growth facilitation action evaluates the estrogenic activity of medicine.This experiment is wet using sex immature female mice uterus
The ratio between weight and body weight (Uterine coefficient) are used as the index for evaluating estrogenic activity.Test result indicates that, carried from lepidii,semen
2- phenyl acetamides compound is taken to dramatically increase sex immature Mouse Uterus coefficient, and lepidii,semen health product can not dramatically increasing property
Prematurity Mouse Uterus coefficient.Point out to extract 2- phenyl acetamides in lepidii,semen in vivo with estrogen-like action.
MCF-7 cells are the Breast cancer lines of estrogen receptor positive, can be specifically by estrogen or estrogen-like
Active material is adjusted and bred, and is the cell line of the most frequently used detection estrogenic activity.Experimental result is found, in lepidii,semen
Extract 2- phenyl acetamides has significant proliferation when concentration is 10 μM to MCF-7 cells.Point out to extract in lepidii,semen
2- phenyl acetamides have certain estrogen-like action in vivo, in vitro.
Estradiol is a kind of natural estrogen mainly secreted in vivo by ovary maturity folliculus, can promote and adjust women
The normal development of organ and secondary sex character.A kind of hormone that interstitialcellstimulating hormone (ICSH) is produced by hypophysis is in women moderate stimulation ovarian secretion
Female estrogen.Follicular stimulating hormone be anterior pituitary basophil cell secretion a kind of hormone, main function for promote ovarian follicle into
It is ripe, promote whole ovary to grow up.Research finds that 2- phenyl acetamides are extracted in lepidii,semen can be with conspicuousness increase prematurity female
The blood serum E2 of mouse and LH level, but the influence to FSH is little.Speculate that 2- phenyl acetamides are extracted in lepidii,semen increases small
Mouse Uterine coefficient performance estrogenic activity may increase internal E2 with it and LH level is relevant.
It is demonstrated experimentally that extracting 2- phenyl acetamides compound from lepidii,semen as sole active agent effective for preparing
Estrogenic, realizes application of the 2- phenyl acetamides as sole active agent in estrogenic is prepared, has opened up preparation
The new way of estrogen drugs, improves the medical value and commercial value of lepidii,semen, there is good economy and society's effect
Benefit.
Claims (5)
1. a kind of method that 2- phenyl acetamide compounds are extracted from lepidii,semen, it is characterised in that lepidii,semen 7.5- will be fried
8.5kg, adds the water of 10 times of weight to extract three times every time, and each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into 260-280g's
Medicinal extract, medicinal extract volumetric concentration is 80% ethanol 19-21L alcohol precipitation 2h, abandons precipitation, by supernatant centrifugal filtration, is concentrated into no alcohol
Taste, upper Dianion HP-20 posts, successively with water 20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h is collected
40% alcohol elution, with the discrete dissolving of water, centrifugal filtration is concentrated into 30-40ml, crosses Toyopearl HW-40 chromatographic columns,
Eluted successively with the water 3L and methanol aqueous solution 3L of volumetric concentration 10%, flow velocity 8mL/min, the methanol aqueous solution of collected volume concentration 10%
Elution fraction, is dissolved with methanol, stands 24h, separates out colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and first is used again
Alcohol dissolves, and stands 24h, so repeatedly 5 times, it is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
2. the method according to claim 1 that 2- phenyl acetamide compounds are extracted from lepidii,semen, it is characterised in that will
Lepidii,semen 8kg is fried, adds the water of 10 times of weight to extract every time three times, each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into
270g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 20L alcohol precipitation 2h, abandons precipitation, supernatant centrifugal filtration is concentrated into
1000 ml, upper Dianion HP-20 posts, successively with water 20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h,
40% alcohol elution is collected, with the discrete dissolving of water, centrifugal filtration is concentrated into 35ml, crosses Toyopearl HW-40 chromatographic columns,
Eluted successively with the water 3L and methanol aqueous solution 3L of volumetric concentration 10%, flow velocity 8mL/min, the methanol aqueous solution of collected volume concentration 10%
Elution fraction, is dissolved with methanol, stands 24h, separates out colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and first is used again
Alcohol dissolves, and stands 24h, so repeatedly 5 times, it is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
3. the method according to claim 1 that 2- phenyl acetamide compounds are extracted from lepidii,semen, it is characterised in that will
Lepidii,semen 7.5kg is fried, adds the water of 10 times of weight to extract every time three times, each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into
260g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 19L alcohol precipitation 2h, abandons precipitation, supernatant centrifugal filtration is concentrated into
Without alcohol taste, upper Dianion HP-20 posts, successively with water 20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h is received
Collect 40% alcohol elution, with the discrete dissolving of water, centrifugal filtration is concentrated into 30ml, crosses Toyopearl HW-40 chromatographic columns, according to
The secondary use water 3L and methanol aqueous solution 3L of volumetric concentration 10% elutions, flow velocity 8mL/min, the methanol aqueous solution of collected volume concentration 10% is washed
De- part, is dissolved with methanol, stands 24h, separates out colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and methanol is used again
Dissolving, stands 24h, so repeatedly 5 times, it is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
4. the method according to claim 1 that 2- phenyl acetamide compounds are extracted from lepidii,semen, it is characterised in that will
Lepidii,semen 8.5kg is fried, adds the water of 10 times of weight to extract every time three times, each 1.5h merges No. three extract solutions, is concentrated under reduced pressure into
280g medicinal extract, medicinal extract volumetric concentration is 80% ethanol 21L alcohol precipitation 2h, abandons precipitation, supernatant centrifugal filtration is concentrated into
Without alcohol taste, upper Dianion HP-20 posts, successively with water 20L, 20% ethanol 60L, 40% ethanol 60L elutions, flow velocity 20L/24h is received
Collect 40% alcohol elution, with the discrete dissolving of water, centrifugal filtration is concentrated into 40ml, crosses Toyopearl HW-40 chromatographic columns, according to
The secondary use water 3L and methanol aqueous solution 3L of volumetric concentration 10% elutions, flow velocity 8mL/min, the methanol aqueous solution of collected volume concentration 10% is washed
De- part, is dissolved with methanol, stands 24h, separates out colourless crystallization, upper solution is suctioned out, and colourless crystallization is dried, and methanol is used again
Dissolving, stands 24h, so repeatedly 5 times, it is 2- phenyl acetamides to obtain colourless crystallization, and mass content reaches more than 95%.
5. 2- phenyl acetamides compound prepared by any one of claim 1 or 2-4 methods described is as sole active agent in system
Application in standby treatment estrogen deficiency disease drug.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105168301A (en) * | 2015-10-23 | 2015-12-23 | 河南中医学院 | Application of semen lepidii water extract in preparation of estrogen medicines |
| CN107353315A (en) * | 2017-07-29 | 2017-11-17 | 河南中医药大学 | A kind of method and its application that the new alkali A compounds of northern Roripa are extracted from lepidii,semen |
-
2017
- 2017-05-26 CN CN201710382069.9A patent/CN107056644A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105168301A (en) * | 2015-10-23 | 2015-12-23 | 河南中医学院 | Application of semen lepidii water extract in preparation of estrogen medicines |
| CN107353315A (en) * | 2017-07-29 | 2017-11-17 | 河南中医药大学 | A kind of method and its application that the new alkali A compounds of northern Roripa are extracted from lepidii,semen |
Non-Patent Citations (2)
| Title |
|---|
| 冯卫生 等: "北葶苈子化学成分研究", 《中国药学杂志》 * |
| 李孟 等: "从北葶苈子中分离到的一个新苯乙酰胺类化合物", 《药学学报》 * |
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