CN106138284A - A kind of extraction process of Semen Ziziphi Spinosae effective site - Google Patents
A kind of extraction process of Semen Ziziphi Spinosae effective site Download PDFInfo
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- CN106138284A CN106138284A CN201510137286.2A CN201510137286A CN106138284A CN 106138284 A CN106138284 A CN 106138284A CN 201510137286 A CN201510137286 A CN 201510137286A CN 106138284 A CN106138284 A CN 106138284A
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- ziziphi spinosae
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Abstract
The present invention relates to a kind of method extracting effective site from Chinese crude drug Semen Ziziphi Spinosae, step is as follows: is cleaned by Semen Ziziphi Spinosae medical material, dry, pulverize into coarse powder；Adding reflux, extract, in 0-90% ethanol, filter, filtrate passes through absorption with macroporous adsorbent resin, the most colourless to effluent with distilled water and 10% alcohol flushing resin post, using 2-6 times amount 50-70% ethanol elution instead, reclaim ethanol, drying processes and i.e. obtains Semen Ziziphi Spinosae effective site.It is high that the Semen Ziziphi Spinosae effective site using the inventive method to prepare has yield, and purity is high, the advantage that production cost is low.
Description
Technical field
The present invention relates to Chinese crude drug effective site extraction process technology field, a kind of method extracting effective site from Semen Ziziphi Spinosae.
Background technology
Semen Ziziphi Spinosae is Rhamnaceae plant Ziziphi Spinosae
The dry mature seed of [Ziziphus jujuba Mill.Var.spinosa (Bunge) Hu ex H.F.Chou], the time of the year when autumn changes into winter gathers mature fruit, removes sarcocarp and nucleocapsid, collect seed, dry.Jujube nucleus begins to be loaded in Shennong's Herbal, is classified as top grade." Mingyi Bielu " three people three cloud: " the raw east of a river, in pool, is adopted reality, dried in the shade August." " Newly Revised Canon of Materia Medica " say: " and this be jujube also, tree is big such as Fructus Jujubae, real impermanence shape, but in Fructus Jujubae, sour in the mouth person is." " Kaibao Bencao " record: " this is that spine is real, his thing more non-.If meaning is Fructus Jujubae sour in the mouth person, Quan Feiye.It is grown at tailo or dry poor soil, is commonly formed bushes.Main product in Hebei, Shanxi, Liaoning, Henan, the ground such as Shandong.Its property is sweet, sour, flat.Enter liver, gallbladder, heart channel.There is the tonifying liver that nourishes heart, mind tranquilizing and the heart calming, arresting sweating, the effect promoted the production of body fluid, cure mainly restlessness of asrhenia type and insomnia, dreaminess of palpitating with fear, body void hyperhidrosis, Tianjin wound is thirsty.Sedative is commonly used for the traditional Chinese medical science.
nullBegin to the chemical composition of Semen Ziziphi Spinosae is studied from the beginning of the eighties，Until within nearly 10 years, achieving great achievement: alkaloid: Semen Ziziphi Spinosae alkali (sanjoinine) A、B、D、E、F、G1、G2、Ia、Ib、K，Wherein alkali A is exactly frangufoline (frangu-foline)，Alkali E is exactly nuciferine (nuciferine)，Alkali Ia is exactly miltanthin (nornu-ciferine)，Alkali Ib is exactly norisocorydine (norisocorydine)，Alkali K is exactly the coclaurine (coclaurine) of dextrorotation，N-methyl asimilobine (N-methylasimilo-bine)，Acid Lee's alkali (zizyphusine)，5-hydroxyl-6-methoxyl group nor-aporphine (caaver-ine，5-hydroxy-6-methoxynoraporphine)，Amphibin D (amphibine) D.Also (sanjoinenine) Han Semen Ziziphi Spinosae cyclic peptide.Also containing triterpenes: betulic acid (betulinic acid), betulin (betulin), ceanothic acid (ceanothic acid), alphitolic acid (alphitolic acid), Jujuboside (jujuboside) A, B, and daucosterol (daucosterol).nullAgain containing flavonoid: spinosin (spinosin)，It is i.e. 2 "-O-β-D-glucopyranosyl swertisin (2 "-O-β-D-glucopyrano-sylswertisin)，Ziziphi Spinosae flavin (zivulgarin)，6 ＇ ＇ ＇-Semen Sinapis acyl spinosin (6 ＇ ＇ ＇-sinapoylspinosin)，6 ＇ ＇ ＇-Resina Ferulae acyl spinosin (6 ＇ ＇ ＇-feruloylspinosin)，6 ＇ ＇ ＇-to coumaric acyl spinosin (6 ＇ ＇ ＇-p-coumaroylspinosin)，Swertisin (swer-tisin)，6，8-bis--C-glucosyl group apigenin (vicenin II)，Apigenin-6-C-[(6-O-para hydroxybenzene formyl)-β-D-glucopyranosyl (1 → 2)]-β-D-pyranglucoside [apigenin-6-C-[(6-O-p-hydroxybenzoyl)-β-D-glucopyranosyl(1 → 2)]-β-D-glucopyranoside] etc..Also (threonine) Han threonine, valine (valine), methionine (methionine), leucine (leucine), isoleucine (isoleucine), lysine (lysine), the Determination of multiple metal elements such as 17 kinds of aminoacid and potassium, sodium, calcium, zinc, ferrum, copper, manganese such as phenylalanine (phenylalanine).(ferulic acid) Han ferulic acid again, vitamin C and plant sterol, cyclic adenosine monophosphate (cyclic adenosine 3 ＇, 5 ＇-monophosphate) etc..
The most constantly the modern pharmacology effect to Semen Ziziphi Spinosae is studied, find multiple biological activity, as to the effect of nervus centralis (sedative-hypnotic effect, convulsion, antidepressant and the effect in terms of improving learning and memory etc.), to the effect of cardiovascular system (hypotensive effect, prevent and treat the effect of arteriosclerosis and blood fat reducing), immunological enhancement, antimutagenic, the effect of anti-curing cancers, antiinflammatory action, anti-ageing wait for a long time in terms of effect.In sum, Semen Ziziphi Spinosae has fabulous DEVELOPMENT PROSPECT, but still lacks a kind of industrialized production preparation method that can extract plurality of active ingredients in Semen Ziziphi Spinosae at present.
Summary of the invention
The technical problem to be solved in the present invention is: provide that a kind of technological process is short, energy-saving and emission-reduction, the preparation method of Semen Ziziphi Spinosae effective site that purity is high.
The present invention solves the technical scheme of technical problem: with Semen Ziziphi Spinosae as raw material, is cleaned by Semen Ziziphi Spinosae medical material, dry, pulverize into coarse powder；Adding reflux, extract, in 0-90% ethanol, filter, filtrate passes through absorption with macroporous adsorbent resin, the most colourless to effluent with distilled water and 10% alcohol flushing resin post, using 2-6 times amount 50-70% ethanol elution instead, reclaim ethanol, drying processes and i.e. obtains Semen Ziziphi Spinosae effective site.
Semen Ziziphi Spinosae raw material used in the present invention, can first extract with after petroleum ether degreasing, it is also possible to not defat extracting directly again.
Currently preferred resin model is HPD100 type macroporous adsorbent resin.First with 95% soak with ethanol 24 hours, wet method dress post before using, it is further continued for use 95% alcohol flushing, adds 5 times of distilled water occur without muddiness until collecting alcohol washing liquid, finally extremely standby without alcohol with distilled water flushing.
The invention have the advantage that present invention ethanol extraction Semen Ziziphi Spinosae effective site, with HPD100 type (Cangzhou Bon Adsorption Material Science and Technology Co., Ltd) general macroporous adsorbent resin, Semen Ziziphi Spinosae is extracted extractum and carry out edulcoration purification effective site, make Semen Ziziphi Spinosae effective site extraction rate reached 1%, extracting the rate of transform and reach more than 90%, (HPLC method mensuration) content reaches more than 60%.The technological process of employing HPD100 type macroporous adsorbent resin extraction Semen Ziziphi Spinosae effective site is short, pollution-free, utilization rate of equipment and installations is high, and Semen Ziziphi Spinosae effective site yield is high, and purity is high, and production cost is low.
The Semen Ziziphi Spinosae effective site using the inventive method to prepare, may be used for preparing medicine or health food.
Detailed description of the invention
In conjunction with embodiment as described below, the present invention is further described:
Embodiment 1
With 1kg Semen Ziziphi Spinosae as raw material, it is ground into coarse powder, it is added to the water Semen Ziziphi Spinosae to boil and carries 3 times, amount of water 10 times every time, extraction time is 2 hours, united extraction liquid, filter, filtrate is concentrated into proportion and is about the survey of 1.10(heat), the extractum that will be cooled to room temperature is added on the macroporous adsorbent resin HPD100 post that pretreatment is good, priority distilled water and 10% ethanol are eluted to colourless, 60% ethanol elution of 4 times of column volumes again, collect alcohol washing liquid, concentrate drying, obtain Semen Ziziphi Spinosae effective site raw material about 11.3g, wherein total saponin content is 30.6%, general flavone content is 38.4%.
Embodiment 2
With 1kg Semen Ziziphi Spinosae as raw material, it is ground into coarse powder, first use petroleum ether degreasing twice, petroleum ether addition is 8 times every time, extraction time is 1 hour, obtain defat medicinal residues and add 30% alcohol reflux 3 times, each 50% ethanol consumption is 10 times, reflux extracting time is 1.5 hours, united extraction liquid, filter, filtrate is concentrated into without alcohol, it is diluted with water to ratio and weighs about the survey of 1.10(heat), it is cooled to room temperature be added on the macroporous adsorbent resin HPD100 post that pretreatment is good, priority distilled water and 10% ethanol are eluted to colourless, 60% ethanol elution of 4 times of column volumes again, collect alcohol washing liquid, concentrate drying, obtain Semen Ziziphi Spinosae effective site raw material about 12.1g, wherein total saponin content is 32.0%, general flavone content is 39.9%.
Embodiment 3
With 1kg Semen Ziziphi Spinosae as raw material, it is ground into coarse powder, first use petroleum ether degreasing twice, petroleum ether addition is 8 times every time, extraction time is 1 hour, obtain defat medicinal residues and add 50% alcohol reflux 3 times, each 50% ethanol consumption is 10 times, reflux extracting time is 1.5 hours, united extraction liquid, filter, filtrate is concentrated into without alcohol, it is diluted with water to ratio and weighs about the survey of 1.10(heat), it is cooled to room temperature be added on the macroporous adsorbent resin HPD100 post that pretreatment is good, priority distilled water and 10% ethanol are eluted to colourless, 70% ethanol elution of 4 times of column volumes again, collect alcohol washing liquid, concentrate drying, obtain Semen Ziziphi Spinosae effective site raw material about 11.3g, wherein total saponin content is 32.6%, general flavone content is 40.7%.
Embodiment 4
With 1kg Semen Ziziphi Spinosae as raw material, it is ground into coarse powder, first use petroleum ether degreasing twice, petroleum ether addition is 8 times every time, extraction time is 1 hour, obtain defat medicinal residues and add 90% alcohol reflux 3 times, each 50% ethanol consumption is 10 times, reflux extracting time is 1.5 hours, united extraction liquid, filter, filtrate is concentrated into without alcohol, it is diluted with water to ratio and weighs about the survey of 1.10(heat), it is cooled to room temperature be added on the macroporous adsorbent resin HPD100 post that pretreatment is good, priority distilled water and 10% ethanol are eluted to colourless, 70% ethanol elution of 4 times of column volumes again, collect alcohol washing liquid, concentrate drying, obtain Semen Ziziphi Spinosae effective site raw material about 10.8g, wherein total saponin content is 34.7%, general flavone content is 42.1%.
Claims (3)
1. an extraction process for Chinese crude drug Semen Ziziphi Spinosae effective site, is characterized in that: with Semen Ziziphi Spinosae as raw material, is cleaned by Semen Ziziphi Spinosae medical material, dry, pulverize into coarse powder；Adding reflux, extract, in 0-90% ethanol, filter, filtrate passes through absorption with macroporous adsorbent resin, the most colourless to effluent with distilled water and 10% alcohol flushing resin post, using 2-6 times amount 50-70% ethanol elution instead, reclaim ethanol, drying processes and i.e. obtains Semen Ziziphi Spinosae effective site raw material.
Technique the most according to claim 1, it is characterised in that Semen Ziziphi Spinosae raw material can first extract with after petroleum ether degreasing again.
Technique the most according to claim 1, it is characterised in that described macroreticular resin is HPD100 type macroporous adsorbent resin.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510137286.2A CN106138284A (en) | 2015-03-27 | 2015-03-27 | A kind of extraction process of Semen Ziziphi Spinosae effective site |
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| CN201510137286.2A CN106138284A (en) | 2015-03-27 | 2015-03-27 | A kind of extraction process of Semen Ziziphi Spinosae effective site |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401643A (en) * | 2002-09-13 | 2003-03-12 | 中国药科大学 | Process for preparing total jujuboflavone with calmative and hypnosis action |
| CN101401855A (en) * | 2008-11-17 | 2009-04-08 | 河南中医学院 | Method for extracting antianxity substance from spina date seed |
| KR20100046968A (en) * | 2008-10-28 | 2010-05-07 | 박준홍 | Soap containing the extracts of zizyphus jujube seed and manufacturing method of it |
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2015
- 2015-03-27 CN CN201510137286.2A patent/CN106138284A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401643A (en) * | 2002-09-13 | 2003-03-12 | 中国药科大学 | Process for preparing total jujuboflavone with calmative and hypnosis action |
| KR20100046968A (en) * | 2008-10-28 | 2010-05-07 | 박준홍 | Soap containing the extracts of zizyphus jujube seed and manufacturing method of it |
| CN101401855A (en) * | 2008-11-17 | 2009-04-08 | 河南中医学院 | Method for extracting antianxity substance from spina date seed |
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