CN1436553A - Method of extracting effective component in red sage - Google Patents

Method of extracting effective component in red sage Download PDF

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Publication number
CN1436553A
CN1436553A CN 02110817 CN02110817A CN1436553A CN 1436553 A CN1436553 A CN 1436553A CN 02110817 CN02110817 CN 02110817 CN 02110817 A CN02110817 A CN 02110817A CN 1436553 A CN1436553 A CN 1436553A
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China
Prior art keywords
radix salviae
salviae miltiorrhizae
extracting
extract
red sage
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CN 02110817
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Chinese (zh)
Inventor
余琛
朱大元
张慧
蒋山好
蔡永葆
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Individual
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Individual
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Priority to CN 02110817 priority Critical patent/CN1436553A/en
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Abstract

The present invention relates to the method of extracting effective component in red sage. The extracting process features the liposoluble component extraction with ethanol as extracting medium, water soluble component extraction with water as extracting medium, ultrasonic treatment to raise extracting efficiency, controlling extracting temperature below 60 deg.c and may be isolating air in some degree. The extracted solution may be further purified with macroporous resin or through adsorption, chromatographic method or other physical and chemical method, or the extracted solution is concentrated and dried to eliminate solvent and to obtain red sage extractive powder, granular or extractive.

Description

A kind of extracting method of effective component in red sage
Technical field
The present invention relates to the extracting method of Chinese medicine, more specifically to the method for utilizing ultrasonic technology that the effective ingredient in the salviamiltiorrhizabung is extracted.
Background technology
Salviamiltiorrhizabung is dry root and the rhizome of labiate Radix Salviae Miltiorrhizae Salvia miliiorrhiza Bge., and traditional traditional Chinese medical science thinks that Radix Salviae Miltiorrhizae has stasis-dispelling and pain-killing, promoting blood circulation to restore menstrual flow, the effect of the relieving restlessness that clears away heart-fire.Modern medicine discovers that Radix Salviae Miltiorrhizae all has therapeutical effect for multiple cardiovascular and cerebrovascular disease and chronic hepatopathy, nephritis, renal failure, peptic ulcer etc.The main effective ingredient of Radix Salviae Miltiorrhizae is broadly divided into fat-soluble tanshinone (is representative with Tanshinone I I-A) and water miscible salvianolic acid class (is representative with salvianolic acid B, danshensu and protocatechualdehyde).
In present effective component in red sage extracts, adopt traditional decocting mostly after methods such as precipitate with ethanol or acid, alkali liquor processing.But adopt traditional decocting method to heat for a long time, and tend to destroy its some effective ingredient and increase trouble for further extraction separation to crude drug; Simultaneously, also exist energy resource consumption big, influence problem of environment.Our experiment at present confirms that tangible degraded can take place Radix Salviae Miltiorrhizae crude drug its some effective ingredient after long-time high temperature decocts, and its extraction recovery is had bigger influence.
The extraction of the effective ingredient in the Radix Salviae Miltiorrhizae can be divided into the extraction of (1) liposoluble substance, the extraction of (2) water-soluble substances.Fat-soluble effective ingredient in the Radix Salviae Miltiorrhizae is mainly tanshinone, as Tanshinone I I-A, cryptotanshinone etc., can adopt alcohol (as ethanol, methanol etc.) and ethyl acetate for extract medium to fat-soluble be that main composition extracts.And the aqueous soluble active constituent in the Radix Salviae Miltiorrhizae is mainly phenolic acid, and as salvianolic acid B, danshensu and protocatechualdehyde class material, can adopt water or contain pure aqueous solution is that main composition extracts as extracting medium to water solublity.
Summary of the invention
The purpose of this invention is to provide a kind of yield of extraction active ingredient in the Radix Salviae Miltiorrhizae and method of purity of improving.
The present invention adopts ultrasonic Treatment and control to extract method of temperature effective ingredient in the Radix Salviae Miltiorrhizae is extracted.Ultrasonic Treatment can make the various compositions that comprise tanshinone and salvianolic acid class in the Radix Salviae Miltiorrhizae crude drug contact with extracting medium widely, and constantly is added in the extraction medium.Frequency of ultrasonic and power will be decided on the degree of sample pulverizing and the quantity of sample, and frequency can be 20-80kHz, and power can be 200-6000W.In the process of extracting, need avoid high temperature (<60 ℃), to avoid part effective ingredient decomposes.Simultaneously, if can be in extraction secluding air relatively, then can reduce the oxidation Decomposition of part effective ingredient.
Can carry out purification as various physico-chemical methods such as macroporous resin adsorption, silica gel column chromatographies further with conventional method with the resulting Radix Salviae Miltiorrhizae extract of the present invention, use for clinical treatment and research to obtain comparatively purified component or monomer.Simultaneously, this extracting solution also can directly remove solvent, dehydration via methods such as cryoconcentration, dialysis ultrafiltration, lyophilization or spray dryinges, with dry powder, granule and the extractum hyoscine of preparation Radix Salviae Miltiorrhizae extract.The present invention has bigger potentiality aspect the preparation of Radix Salviae Miltiorrhizae single granule.
Compare with traditional decocting method, the present invention have energy resource consumption few, to the relative features of smaller of the influence of environment.Simultaneously, owing to adopt the ripple processing-extract at low temperature of overfulfiling a production target, avoided the destruction of high temperature to effective ingredient preferably, the content and the quality of the tanshinone in the extracting solution of use the inventive method gained and the material of salvianolic acid effective constituents will be better than traditional decocting method.
The specific embodiment
A: the Radix Salviae Miltiorrhizae crude drug is through pulverizing and cross 30 mesh sieves; Get the 0.1kg powder, add 5-10 times of volume of ethanol and soaked 2-4 hour; Handled 0.5-1 hour with ultrasound wave (frequency is 40kHz, and power is 500W), extract temperature and be controlled at about 4-10 ℃, solid-liquid is separated, obtain alcohol extract based on fat-soluble class material through centrifugal; Can repeat in case of necessity to extract repeatedly.Merge extractive liquid, low temperature is removed organic solvent, gets tanshinone compound by the routine operation that extracts such material with macroporous resin or silica gel column chromatography separation and purification then.
The Radix Salviae Miltiorrhizae crude drug powder after the alcohol extraction of learning from else's experience adds water logging bubble 4-8 hour of 5-10 times of volume, ultrasound wave (frequency is 40kHz, and power is 500W) was handled 0.5-1 hour, extracted temperature and was controlled at about 4-10 ℃, through centrifugal solid-liquid is separated, obtain aqueous extract based on water solublity class material; Can repeat in case of necessity to extract repeatedly.Operational approach (should note avoiding high temperature) routinely behind macroporous resin or the silica gel column chromatography on the merge extractive liquid,, separation and purification gets pressure differential self.
B: get Radix Salviae Miltiorrhizae crude drug coarse powder (5-10 order) portion, the water logging that adds 5 times of volumes was steeped 12 hours, (frequency is 40kHz to ultrasound wave, power is 500W) handled 1-2 hour, nitrogen is filled in the part, constantly add an amount of ice block cooling during ultrasonic Treatment, solid-liquid is separated, obtaining and including salvia-soluble class material is main aqueous extract.Can repeat in case of necessity to extract repeatedly.Merge aqueous extract, remove solvent, dehydration, get the lyophilized powder or the extract powder of Radix Salviae Miltiorrhizae extract through methods such as lyophilization or spray dryinges.

Claims (4)

1. one kind is extracted the method for Radix Salviae Miltiorrhizae ester dissolubility or water solublity active ingredient with organic solvent or water logging bubble, it is characterized in that handling through ultrasonic low temperature in the leaching process, isolated down extract relative with oxygen, the gained extracting solution through macroporous resin, silica gel column chromatography be further purified or directly cryoconcentration, dialyse ultrafiltration, lyophilization, dewater Radix Salviae Miltiorrhizae extract.
2. according to the method for the described extraction Radix Salviae Miltiorrhizae of claim ester dissolubility or aqueous soluble active constituent, it is characterized in that the ultrasonic Treatment frequency is 20-80KHz, power is 200-6000W.
3. according to the method for the described extraction Radix Salviae Miltiorrhizae of claim ester dissolubility or aqueous soluble active constituent, it is characterized in that leaching process is carrying out less than 60 ℃.
4. according to the method for the described extraction Radix Salviae Miltiorrhizae of claim ester dissolubility or aqueous soluble active constituent, it is characterized in that leaching process carries out under completely cut off relative with oxygen, best inert gas is to carry out under the nitrogen current.
CN 02110817 2002-02-08 2002-02-08 Method of extracting effective component in red sage Pending CN1436553A (en)

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CN 02110817 CN1436553A (en) 2002-02-08 2002-02-08 Method of extracting effective component in red sage

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Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1303052C (en) * 2004-03-18 2007-03-07 中国科学院大连化学物理研究所 Process for preparing Danshensu
WO2007068143A1 (en) * 2005-12-13 2007-06-21 Lanqin Yang Preparation of plant oil, crude protein and fiber by water extraction
CN100393709C (en) * 2004-03-17 2008-06-11 天津天士力现代中药资源有限公司 Process for extracting tanshinone
CN100425160C (en) * 2006-04-07 2008-10-15 谭金镜 Danshi food and preparing method
CN101007057B (en) * 2007-01-17 2010-05-19 华南理工大学 Extraction method of water soluble components from salvia miltiorrhiza by ultrasonic continuous countercurrent gradient
CN1813893B (en) * 2004-12-06 2011-05-18 百愈生物医药有限公司 Method for extracting effective portion of polyphenol acid
CN102274283A (en) * 2011-09-05 2011-12-14 邵明川 Preparation method of red-rooted salvia root active fraction
CN102351819A (en) * 2011-10-27 2012-02-15 广州汉方现代中药研究开发有限公司 Extraction, purification and preparation method of high-purity salvianolic acid B
CN102526188A (en) * 2012-02-15 2012-07-04 苏州卫生职业技术学院 Process for processing root of red-rooted salvia with vinegar
CN102772487A (en) * 2012-08-01 2012-11-14 辽宁盛生医药集团有限公司 Preparation method of Salvia miltiorrhiza soft capsule
CN102836210A (en) * 2011-06-22 2012-12-26 四川农业大学 Vinegar-frying preparation method of traditional Chinese medicine salvia miltiorrhiza
CN102579460B (en) * 2003-12-30 2015-04-29 麦仁斯有限公司 Obesity and metabolic syndrome treatment with tanshinone derivatives which increase metabolic activity
CN105085266A (en) * 2014-05-14 2015-11-25 南京虹桥医药技术研究所 Method for preparing salvianolic acid A from a plurality of salvia plants
CN109350644A (en) * 2018-12-28 2019-02-19 青岛海隆达生物科技有限公司 Auxiliary hyperglycemic tablet
CN110563677A (en) * 2019-08-23 2019-12-13 惠州市九惠制药股份有限公司 Salvianolic acid B and powder inhalation capsule thereof and preparation method

Cited By (17)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102579460B (en) * 2003-12-30 2015-04-29 麦仁斯有限公司 Obesity and metabolic syndrome treatment with tanshinone derivatives which increase metabolic activity
CN100393709C (en) * 2004-03-17 2008-06-11 天津天士力现代中药资源有限公司 Process for extracting tanshinone
CN1303052C (en) * 2004-03-18 2007-03-07 中国科学院大连化学物理研究所 Process for preparing Danshensu
CN1813893B (en) * 2004-12-06 2011-05-18 百愈生物医药有限公司 Method for extracting effective portion of polyphenol acid
WO2007068143A1 (en) * 2005-12-13 2007-06-21 Lanqin Yang Preparation of plant oil, crude protein and fiber by water extraction
CN100425160C (en) * 2006-04-07 2008-10-15 谭金镜 Danshi food and preparing method
CN101007057B (en) * 2007-01-17 2010-05-19 华南理工大学 Extraction method of water soluble components from salvia miltiorrhiza by ultrasonic continuous countercurrent gradient
CN102836210A (en) * 2011-06-22 2012-12-26 四川农业大学 Vinegar-frying preparation method of traditional Chinese medicine salvia miltiorrhiza
CN102274283A (en) * 2011-09-05 2011-12-14 邵明川 Preparation method of red-rooted salvia root active fraction
CN102274283B (en) * 2011-09-05 2013-04-17 邵明川 Preparation method of red-rooted salvia root active fraction
CN102351819B (en) * 2011-10-27 2014-05-14 广州白云山汉方现代药业有限公司 Extraction, purification and preparation method of high-purity salvianolic acid B
CN102351819A (en) * 2011-10-27 2012-02-15 广州汉方现代中药研究开发有限公司 Extraction, purification and preparation method of high-purity salvianolic acid B
CN102526188A (en) * 2012-02-15 2012-07-04 苏州卫生职业技术学院 Process for processing root of red-rooted salvia with vinegar
CN102772487A (en) * 2012-08-01 2012-11-14 辽宁盛生医药集团有限公司 Preparation method of Salvia miltiorrhiza soft capsule
CN105085266A (en) * 2014-05-14 2015-11-25 南京虹桥医药技术研究所 Method for preparing salvianolic acid A from a plurality of salvia plants
CN109350644A (en) * 2018-12-28 2019-02-19 青岛海隆达生物科技有限公司 Auxiliary hyperglycemic tablet
CN110563677A (en) * 2019-08-23 2019-12-13 惠州市九惠制药股份有限公司 Salvianolic acid B and powder inhalation capsule thereof and preparation method

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