CN101744879B - Method for decoloring salvia-soluble extract - Google Patents
Method for decoloring salvia-soluble extract Download PDFInfo
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- CN101744879B CN101744879B CN 200810153792 CN200810153792A CN101744879B CN 101744879 B CN101744879 B CN 101744879B CN 200810153792 CN200810153792 CN 200810153792 CN 200810153792 A CN200810153792 A CN 200810153792A CN 101744879 B CN101744879 B CN 101744879B
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Abstract
The invention discloses a method for decoloring salvia-soluble extract, which is characterized in that an anion exchange resin is taken as a decoloring medium. The method for decoloring the salvia-soluble extract has obvious decoloring effect and is easy for industrialized production.
Description
Technical field
The present invention relates to the purification process field of Chinese medicine, particularly the purification process of Radix Salviae Miltiorrhizae extract.
Background technology
Radix Salviae Miltiorrhizae is the dry root and rhizome of labiate Radix Salviae Miltiorrhizae (Salvia miltiorrhiza Bunge), is one of traditional activating blood herbs, and long-term clinical practice basis is arranged.Water-soluble extract of red sage root is the common drug for the treatment of coronary heart disease, angina pectoris, myocardial infarction, cerebral infarction etc. clinically.Salvianolic acid class wherein is the main effective site of water solublity, has the effect of obvious suppression platelet aggregation, anticoagulant, molten fibre and anti peroxidation of lipid, is the main component of Radix Salviae Miltiorrhizae activating blood circulation to dissipate blood stasis.This compounds mainly contains catechu aldehyde, protocatechuic acid, danshensu, salvianolic acid A, B, C, E, rosmarinic acid etc.
The existence of pigment can have a strong impact on product quality in the Radix Salviae Miltiorrhizae extraction with aqueous solution composition injection.The pigment material is most of to belong to acidic materials, and water-soluble extract of red sage root is main component with the Radix Salviae Miltiorrhizae total phenolic acids, and effective ingredient and acidic dye character approach, and is very difficult when acid impurities such as removal pigment.
Summary of the invention
The invention provides a kind of method for decoloring salvia-soluble extract, this method is decoloring medium with the anion exchange resin.
The preparation method of the extracting method of a lot of salvia-soluble compositions is disclosed in the prior art, for example water extraction, circumfluence method, countercurrent extraction method, percolation, ultrasonic extraction etc. can also further separate and/or macroporous adsorption resin chromatography separation (Chinese patent 02117923.9) with polyamide chromatography post after the extraction.Preferably, water-soluble extract of red sage root of the present invention can adopt the method preparation that may further comprise the steps: (1) red rooted salvia extracts through water or aqueous methanol, alcoholic solution; (2) extracting solution carries out purification with macroporous adsorbent resin and/or polyamide or precipitate with ethanol or extracting process.
Discoloration method of the present invention, wherein used anion exchange resin can be acid or alkaline anion exchange resin, the preferred anionic exchanger resin, for example strong-base anion-exchange resin such as D201, D290, D296R etc. also can be weak-base anion-exchange resin such as D301T, D371, D392, D380, D382 etc.
The present invention preferably adopts and may further comprise the steps ground technical scheme enforcement:
(1) water-soluble extract of red sage root is regulated the pH value of its aqueous solution to 3-9;
(2) through ion-exchange chromatography;
(3) water or volumn concentration are that the alcoholic solution of the C1-C5 of 10-95% is washed post, discard cleaning mixture;
(4) be that the volumn concentration of 1-3 is the aqueous solution eluting of alcohol of the C1-C5 of 20-95% with pH value, collect eluent.
Discoloration method of the present invention, wherein preferably also contain the inorganic alkaline metal salt that weight percentage is 0.05-0.5% in the eluent of step (4), wherein said inorganic alkaline metal salt can be conventional or commonly used inorganic alkaline metal salt, particular certain cancers or potassium salt of this area.
Method of the present invention, the alcohol of wherein said C1-C5 are selected from the alcohol of C1-C5 this area routine or commonly used, include but not limited to methanol, ethanol, isopropyl alcohol, n-butyl alcohol etc., particular methanol or ethanol.
Method of the present invention can use method commonly used or routine to regulate the pH value of eluent, for example adds mineral acid or organic acid such as formic acid, acetic acid such as hydrochloric acid, sulphuric acid, phosphoric acid, nitric acid.
The inventive method, decolorizing effect is obvious, and the finger printing of effective ingredient shows before and after the decolouring, and this method does not influence content of effective, and is easy to industrialized great production.
Concrete enforcement
Further describe flesh and blood of the present invention below in conjunction with embodiments of the invention, this embodiment only is used for explanation the present invention and the present invention is not limited.
Embodiment 1
Get Radix Salviae Miltiorrhizae 100 grams, 500ml water reflux, extract, three times is concentrated to about 100ml, by 150 gram AB-8 macroporous resins, and the 300ml washing, 300ml 60% ethanol elution, eluent are concentrated to no ethanol flavor, upper prop.Resin column is the D371 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 20% washed with methanol.60% methanol solution eluting of 3 times of column volume 0.5% sodium chloride is collected eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Embodiment 2
Get Radix Salviae Miltiorrhizae 100 grams, 500ml 50% alcohol reflux three times, being concentrated to does not have the alcohol flavor, by 100 gram polyamide, the 300ml washing, 300ml95% ethanol elution, eluent are concentrated to no ethanol flavor, upper prop.Resin column is the D380 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 20% alcohol flushings.60% alcoholic solution eluting of 3 times of column volume 0.5% sodium chloride is collected eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Embodiment 3
Get Radix Salviae Miltiorrhizae 100 grams, 5000ml 50% ethanol percolate extraction, being concentrated to does not have pure flavor, by 100 gram polyamide, the 300ml washing, 300ml 95% ethanol elution, eluent are concentrated to no ethanol flavor, use the hydrochloric acid adjust pH to 6 upper props.Resin column is the D392 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 40% n-butyl alcohol flushings.3 times of column volumes contain 60% butanol solution eluting of 0.1% hydrochloric acid, collect eluent, concentrate, be drying to obtain.Extract is light yellow.
Embodiment 4
Get Radix Salviae Miltiorrhizae 100 grams, the extraction of 5000ml watery vomiting stream is extracted, and extracting solution is concentrated to 100ml, with hydrochloric acid adjust pH to 1, filters upper prop.Resin column is the D296R anion exchange resin.With 3 times of column volume washings, 2 times of column volume 30% alcohol flushings.3 times of column volumes contain 50% alcoholic solution eluting of 1% acetic acid and 0.2% sodium chloride, collect eluent, are de-inking solution.Be concentrated to about 50ml, transfer pH value 2.3, ethyl acetate extraction 3 times, each 30ml, combining extraction liquid, concentrated, dry, namely.Extract is white.
Embodiment 5
Get Radix Salviae Miltiorrhizae 100 grams, 5000ml 75% methanol percolation extracts, and is concentrated to nothing alcohol, by 100 gram polyamide, and the 300ml washing, 300ml95% ethanol elution, eluent are concentrated to no ethanol flavor, use the hydrochloric acid adjust pH to 10 upper props.Resin column is the D301T anion exchange resin.With 3 times of column volume washings, 2 times of column volume 40% n-butyl alcohol flushings.3 times of column volumes contain 60% butanol solution eluting of 0.1% sulphuric acid, collect eluent, concentrate, be drying to obtain.Extract is light yellow.
Embodiment 6
Get Radix Salviae Miltiorrhizae 100 grams, 5000ml 75% methanol percolation extracts, and is concentrated to nothing alcohol, by 100 gram D101 resins, and the 300ml washing, 300ml75% ethanol elution, eluent are concentrated to no ethanol flavor, use the hydrochloric acid adjust pH to 3 upper props.Resin column is the D201 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 40% alcohol flushings.3 times of column volumes contain 60% alcoholic solution eluting of 0.1% formic acid, collect eluent, concentrate, be drying to obtain.Extract is off-white color.
Embodiment 7
Get Radix Salviae Miltiorrhizae 100 grams, 5000ml 75% methanol percolation extracts, being concentrated to does not have alcohol, by 100 gram polyamide, 700ml washing, 350ml0.3% sodium bicarbonate eluting, eluent transfers PH3.8 by 200 gram D101 resins, 600ml washing, 1000ml75% ethanol elution, eluent is concentrated to no ethanol flavor, uses the hydrochloric acid adjust pH to 3 upper props.Resin column is the D201 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 40% alcohol flushings.3 times of column volumes contain 60% alcoholic solution eluting of 0.1% phosphoric acid, collect eluent, concentrate, be drying to obtain.Extract is off-white color.
Embodiment 8
Get Radix Salviae Miltiorrhizae 100 gram, 500ml 75% reflux, extract, three times is concentrated to about 100ml, transfers pH value 1.8, filters, and filtrate adds ethyl acetate extraction three times, each 70ml, and combining extraction liquid is concentrated, and thin up is to 50ml, upper prop.Resin column is the D371 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 20% washed with methanol.60% methanol solution eluting of 3 times of column volume 0.5% sodium chloride is collected eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Embodiment 9
Get Radix Salviae Miltiorrhizae 100 gram, 500ml water reflux, extract, three times is concentrated to about 100ml, adds 95% ethanol and measures 70% to containing alcohol, is concentrated into proportion 1.15 (60 ℃), and thin up is to 100ml, upper prop.Resin column is the D371 anion exchange resin.With 3 times of column volume washings, 2 times of column volume 20% washed with methanol.60% methanol solution eluting of 3 times of column volume 0.5% sodium chloride is collected eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Embodiment 10
Get Radix Salviae Miltiorrhizae 100 grams, 500ml 50% alcohol reflux three times, being concentrated to does not have the alcohol flavor, by 100 gram polyamide, the 300ml washing, 300ml95% ethanol elution, eluent are concentrated to no ethanol flavor, upper prop.Resin column is the D380 anion exchange resin.With 3 times of column volume washings, 1 times of column volume 10% alcohol flushing.95% alcoholic solution eluting of 1 times of column volume 0.05% sodium chloride is collected eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Embodiment 11
Get Radix Salviae Miltiorrhizae 100 grams, 500ml 50% alcohol reflux three times, being concentrated to does not have the alcohol flavor, by 100 gram polyamide, the 300ml washing, 300ml95% ethanol elution, eluent are concentrated to no ethanol flavor, upper prop.Resin column is the D380 anion exchange resin.With 3 times of column volume washings, 1 times of column volume 10% alcohol flushing.The pH of 1 times of column volume 0.05% sodium chloride is 1 20% alcoholic solution eluting, collects eluent, is de-inking solution.Concentrated, dry, namely.Extract is off-white color.
Claims (1)
1. method for decoloring salvia-soluble extract is characterized in that step is as follows:
(1) get Radix Salviae Miltiorrhizae 100 grams, 500ml50% alcohol reflux three times, being concentrated to does not have the alcohol flavor;
(2) concentrated solution is by 100 gram polyamide, 300ml washing, 300ml95% ethanol elution, eluent be concentrated to no ethanol distinguish the flavor of the eluting concentrated solution;
(3) get the eluting concentrated solution and cross the D380 anion-exchange resin column, respectively with 3 times of column volumes washings, 1 times of column volume 10% alcohol flushing, 95% alcoholic solution eluting of 1 times of column volume 0.05% sodium chloride is collected eluent, is de-inking solution.
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| CN 200810153792 CN101744879B (en) | 2008-12-05 | 2008-12-05 | Method for decoloring salvia-soluble extract |
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| CN 200810153792 CN101744879B (en) | 2008-12-05 | 2008-12-05 | Method for decoloring salvia-soluble extract |
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| CN101744879B true CN101744879B (en) | 2013-08-21 |
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| CN103630500A (en) * | 2013-11-29 | 2014-03-12 | 广西医科大学 | Method for determining activity of alpha-amylase inhibitor by colorimetric method via resin de-coloring |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1349818A (en) * | 2001-10-24 | 2002-05-22 | 沈阳药科大学 | Effective part group in red sage mixture and its delayed release prepn. medicinal use and prepn process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1349818A (en) * | 2001-10-24 | 2002-05-22 | 沈阳药科大学 | Effective part group in red sage mixture and its delayed release prepn. medicinal use and prepn process |
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