CN102391327A - Separation and preparation method for acteoside - Google Patents
Separation and preparation method for acteoside Download PDFInfo
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- CN102391327A CN102391327A CN2011102100551A CN201110210055A CN102391327A CN 102391327 A CN102391327 A CN 102391327A CN 2011102100551 A CN2011102100551 A CN 2011102100551A CN 201110210055 A CN201110210055 A CN 201110210055A CN 102391327 A CN102391327 A CN 102391327A
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Abstract
The invention relates to separation of natural medicaments, in particular to a separation and preparation method for acteoside. The method comprises the following steps of: smashing the ground part of Arab speedwell; leaching with boiling water for three times, every time for 1-2 hours; combining leaching solutions; performing macroporous resin chromatography; eluting with ethanol water; concentrating the collected liquid and recovering ethanol; feeding the concentrated solution into a high-speed centrifuge for filtering; separating the filtrate with a membrane separator to obtain a component, and separating and preparing with an efficient industrial chromatographic column; gradually eluting with a water-alcohol system; combining eluents which are rich in acteoside; and concentrating and performing freeze drying to obtain acteoside. The method has the advantages of high product purity and stable process, and is particularly suitable for separating and preparing a high-purity acteoside compound from Arab speedwell.
Description
Technical field
The present invention relates to the separation of natural drug, specifically a kind of preparation method who separates acteoside through membrane sepn and preparative high performance liquid chromatography technology from Arabic veronica over-ground part.
Background technology
Arabic veronica (
Veronica persicaPoir.) being the scrophulariaceae herbage, being born in field, roadside, is East China common weed in early spring, also is common instruction plant, aboundresources.But the herb hyoscine of plant can be treated diseases such as rheumatic arthralgia, lumbago due to renal deficiency, outer malaria.Arabic veronica over-ground part contains Arabic veronica glycosides, acteoside, galactitol isoreactivity composition.
Acteoside is the plain constituents of phenylpropyl alcohol, dissolves in the alcohols organic reagent, and water-soluble, polarity is big.Modern pharmacological research shows that acteoside has multiple liveliness proof: anti-oxidant, antiviral, protect the liver, anti metastasis, anti-inflammatory, reducing blood-fat, antibiotic, neuroprotective, hypotensive and cardiovascular protection etc.Sun Weidong etc. can promote apoptosis through discovering acteoside, and ultrastructure is improved significantly, and can suppress the prostatitis hyperplasia.
The relevant report of not seeing acteoside industrial separation preparation method as yet at present.
Summary of the invention
The purpose of this invention is to provide a kind of environment friendly and pollution-free, product purity is high, the method for separating and preparing of acteoside that can scale operation.
In order to achieve the above object, the present invention adopts technical scheme to be:
A kind of method for separating and preparing of acteoside is characterized in that:
(1) extract: take by weighing Arabic veronica dry aerial parts, add 8-12 times of boiling water lixiviate 3 times, each 1-2h merges vat liquor;
(2) macroporous resin column chromatography: vat liquor is splined on the non-polar macroporous resin post, uses zero(ppm) water and 45-65% ethanol elution respectively, collect elutriant;
(3) membrane sepn: with the concentrated ethanol of removing of elutriant; Through the centrifugal clear liquid that obtains of supercentrifuge; Micro-filtration weisspiessglanz ceramic membrane filter through 0.10 micron in aperture; Filtrating is 1000 tubular fibre membrane sepn again through molecular weight cut-off, obtains seeing through liquid, and concentrate drying promptly obtains the membrane sepn component;
(4) preparative high performance liquid chromatography separates: with the silica gel bonded stationary phase of anti-phase C18 is chromatographic column filler, is moving phase with methyl alcohol-water, gradient elution, and target component is collected in the on-line ultraviolet monitoring, and concentrated frozen is drying to obtain acteoside.
Methyl alcohol-water volume ratio is 10-55% described in the step (4).
The monitoring of on-line ultraviolet described in the step (4) wavelength is 227nm.
The present invention has the following advantages:
(1) products obtained therefrom purity is high.The present invention has adopted advanced preparative high performance liquid chromatography stripping technique, has high score from ability, can guarantee that product purity reaches more than 98%.
(2) organic residual few.The present invention has abandoned technologies such as traditional SX, silica gel column chromatography, has adopted water to carry with membrane sepn etc. and need not method with an organic solvent.
(3) environment friendly and pollution-free.It is all recyclable that the present invention prepares the organic solvent that uses in the process, the waste water of the environment that do not exert an influence.
(4) can realize scale operation.
Embodiment
Embodiment 1
Arabic veronica dry aerial parts are pulverized, and take by weighing 0.5kg, add 10 times of boiling water lixiviates 3 times; Each 1.5h filters, and merges vat liquor; Vat liquor is splined on D101 type macroporous resin column, uses zero(ppm) water and 65% ethanol elution respectively, collects alcohol eluen; Concentrate and remove ethanol, through the centrifugal clear liquid that obtains of supercentrifuge, through the micro-filtration weisspiessglanz ceramic membrane filter in 0.10 micron in aperture; Filtrating is 1000 tubular fibre membrane sepn again through molecular weight cut-off, obtains seeing through liquid, and concentrate drying promptly obtains the membrane sepn component;
With the silica gel bonded stationary phase of anti-phase C18 is chromatographic column filler, is moving phase with 10-55% methyl alcohol-water, gradient elution; The membrane sepn component is dissolved sample introduction, on-line ultraviolet monitoring with the 10ml anhydrous methanol; Wavelength is 227nm, collects target component, and concentrated frozen is drying to obtain acteoside.
Embodiment 2
Arabic veronica dry aerial parts are pulverized, and take by weighing 1kg, add 12 times of boiling water lixiviates 3 times; Each 2h filters, and merges vat liquor; Vat liquor is splined on D101 type macroporous resin column, uses zero(ppm) water and 45% ethanol elution respectively, collects alcohol eluen; Concentrate and remove ethanol, through the centrifugal clear liquid that obtains of supercentrifuge, through the micro-filtration weisspiessglanz ceramic membrane filter in 0.10 micron in aperture; Filtrating is 1000 tubular fibre membrane sepn again through molecular weight cut-off, obtains seeing through liquid, and concentrate drying promptly obtains the membrane sepn component;
With the silica gel bonded stationary phase of anti-phase C18 is chromatographic column filler, is moving phase with 10-55% methyl alcohol-water, gradient elution; The membrane sepn component is dissolved sample introduction, on-line ultraviolet monitoring with the 10ml anhydrous methanol; Wavelength is 227nm, collects target component, and concentrated frozen is drying to obtain acteoside.
Embodiment 3
Arabic veronica dry aerial parts are pulverized, and take by weighing 2kg, add 12 times of boiling water lixiviates 3 times; Each 1h filters, and merges vat liquor; Vat liquor is splined on D101 type macroporous resin column, uses zero(ppm) water and 50% ethanol elution respectively, collects alcohol eluen; Concentrate and remove ethanol, through the centrifugal clear liquid that obtains of supercentrifuge, through the micro-filtration weisspiessglanz ceramic membrane filter in 0.10 micron in aperture; Filtrating is 1000 tubular fibre membrane sepn again through molecular weight cut-off, obtains seeing through liquid, and concentrate drying promptly obtains the membrane sepn component;
With the silica gel bonded stationary phase of anti-phase C18 is chromatographic column filler, is moving phase with 10-55% methyl alcohol-water, gradient elution; The membrane sepn component is dissolved sample introduction, on-line ultraviolet monitoring with the 10ml anhydrous methanol; Wavelength is 227nm, collects target component, and concentrated frozen is drying to obtain acteoside.
Claims (3)
1. the method for separating and preparing of an acteoside is characterized in that:
(1) extract: take by weighing Arabic veronica dry aerial parts, add 8-12 times of boiling water lixiviate 3 times, each 1-2h merges vat liquor;
(2) macroporous resin column chromatography: vat liquor is splined on the non-polar macroporous resin post, uses zero(ppm) water and 45-65% ethanol elution respectively, collect elutriant;
(3) membrane sepn: with the concentrated ethanol of removing of elutriant; Through the centrifugal clear liquid that obtains of supercentrifuge; Micro-filtration weisspiessglanz ceramic membrane filter through 0.10 micron in aperture; Filtrating is 1000 tubular fibre membrane sepn again through molecular weight cut-off, obtains seeing through liquid, and concentrate drying promptly obtains the membrane sepn component;
(4) preparative high performance liquid chromatography separates: with the silica gel bonded stationary phase of anti-phase C18 is chromatographic column filler, is moving phase with methyl alcohol-water, gradient elution, and target component is collected in the on-line ultraviolet monitoring, and concentrated frozen is drying to obtain acteoside.
2. according to the method for separating and preparing of the said acteoside of claim 1, it is characterized in that methyl alcohol-water volume ratio is 10-55% described in the step (4).
3. according to the method for separating and preparing of the said acteoside of claim 1, it is characterized in that the monitoring of on-line ultraviolet described in the step (4) wavelength is 227nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011102100551A CN102391327A (en) | 2011-07-26 | 2011-07-26 | Separation and preparation method for acteoside |
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| CN2011102100551A CN102391327A (en) | 2011-07-26 | 2011-07-26 | Separation and preparation method for acteoside |
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| CN102391327A true CN102391327A (en) | 2012-03-28 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131056A (en) * | 2015-10-15 | 2015-12-09 | 厦门华侨亚热带植物引种园 | Acteoside and separating preparation method thereof |
| CN107474556A (en) * | 2017-09-07 | 2017-12-15 | 华南师范大学 | A kind of edible packing membrane and its production and use |
| CN107880084A (en) * | 2017-11-02 | 2018-04-06 | 中国人民解放军第九七医院 | The method that middle extraction preparation high-purity acteoside is spent from platymiscium of reaching the clouds |
| CN108675939A (en) * | 2018-07-10 | 2018-10-19 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting dencichine from Radix Notoginseng |
| CN112294726A (en) * | 2020-11-24 | 2021-02-02 | 东莞波顿香料有限公司 | Herba Veronicae Didyma extract and its preparation method and application |
Citations (3)
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| CN1931868A (en) * | 2006-09-29 | 2007-03-21 | 张惠东 | Figwort total phenyl glycoside and its prepn process and application |
| CN101194934A (en) * | 2007-12-28 | 2008-06-11 | 中山大学 | Method for abstracting active compound rich in echinacoside and feltwort glycoside |
| CN101723998A (en) * | 2008-10-17 | 2010-06-09 | 中国科学院大连化学物理研究所 | Preparation method of flavonoid glycosides in scutellaria baicalensis |
-
2011
- 2011-07-26 CN CN2011102100551A patent/CN102391327A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931868A (en) * | 2006-09-29 | 2007-03-21 | 张惠东 | Figwort total phenyl glycoside and its prepn process and application |
| CN101194934A (en) * | 2007-12-28 | 2008-06-11 | 中山大学 | Method for abstracting active compound rich in echinacoside and feltwort glycoside |
| CN101723998A (en) * | 2008-10-17 | 2010-06-09 | 中国科学院大连化学物理研究所 | Preparation method of flavonoid glycosides in scutellaria baicalensis |
Non-Patent Citations (1)
| Title |
|---|
| U.SEBNEM HARPUT: "Phenylethanoid and Iridoid Glycosides from Veronica persica", 《CHEM.PHARM.BULL》, vol. 50, no. 6, 30 June 2002 (2002-06-30), pages 869, XP001183389, DOI: doi:10.1248/cpb.50.869 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131056A (en) * | 2015-10-15 | 2015-12-09 | 厦门华侨亚热带植物引种园 | Acteoside and separating preparation method thereof |
| CN105131056B (en) * | 2015-10-15 | 2018-02-16 | 厦门华侨亚热带植物引种园 | A kind of acteoside and its method for separating and preparing |
| CN107474556A (en) * | 2017-09-07 | 2017-12-15 | 华南师范大学 | A kind of edible packing membrane and its production and use |
| CN107880084A (en) * | 2017-11-02 | 2018-04-06 | 中国人民解放军第九七医院 | The method that middle extraction preparation high-purity acteoside is spent from platymiscium of reaching the clouds |
| CN108675939A (en) * | 2018-07-10 | 2018-10-19 | 山东端信堂大禹药业有限公司 | A kind of device and its extracting method extracting dencichine from Radix Notoginseng |
| CN112294726A (en) * | 2020-11-24 | 2021-02-02 | 东莞波顿香料有限公司 | Herba Veronicae Didyma extract and its preparation method and application |
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Application publication date: 20120328 |