CN102100736A - Method for simultaneously extracting water-soluble and lipid-soluble effective components in traditional Chinese medicine salvia miltiorrhiza bunge - Google Patents
Method for simultaneously extracting water-soluble and lipid-soluble effective components in traditional Chinese medicine salvia miltiorrhiza bunge Download PDFInfo
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- CN102100736A CN102100736A CN 200910201558 CN200910201558A CN102100736A CN 102100736 A CN102100736 A CN 102100736A CN 200910201558 CN200910201558 CN 200910201558 CN 200910201558 A CN200910201558 A CN 200910201558A CN 102100736 A CN102100736 A CN 102100736A
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Abstract
The invention belongs to the field of analysis chemistry, and relates to a method for simultaneously extracting water-soluble and lipid-soluble effective components from traditional Chinese medicine salvia miltiorrhiza bunge by using an infrared radiation auxiliary technology. The method comprises the following steps of: pulverizing salvia miltiorrhiza bunge medicinal materials to obtain a powder sample; adding certain quantity of extraction solvent; and carrying out the infrared radiation auxiliary technology and simultaneously extracting the water-soluble and lipid-soluble effective components in the salvia miltiorrhiza bunge. Combined with the effective liquid-phase chromatograph, the content of the eight effective components, i.e. salvianolic acids, tanshinone II A and the like, in the salvia miltiorrhiza bunge can be correctly tested so as to evaluate the quality of the traditional Chinese medicine salvia miltiorrhiza bunge from a more comprehensive angle. The method has the advantages of convenience, quickness, less sample dosage, high extraction efficiency, good reproducibility and high recycling ratio.
Description
Technical field
The invention belongs to the analytical chemistry field, the method that relates to pharmaceutically active ingredient in the extraction, be specifically related to a kind of method of extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously, relate in particular to a kind of method of utilizing the infra-red radiation ancillary technique from salviamiltiorrhizabung, to extract water solublity and fat-soluble effective ingredient simultaneously.
Background technology
Radix Salviae Miltiorrhizae is the dry root and rhizome of labiate Radix Salviae Miltiorrhizae (Salvia miltiorrhiza Bge.).Its bitter in the mouth is slightly cold, GUIXIN, Liver Channel.Has the silt of dispelling pain relieving, promoting blood circulation to restore menstrual flow, the effect of the relieving restlessness that clears away heart-fire.Prior art discloses that chemical constituent mainly comprises following two big constituents in the Radix Salviae Miltiorrhizae: phenolic acids water soluble ingredient and Diterpenes liposoluble constituent.Wherein, fat-soluble chemical constituent mainly comprises Tanshinone I, Tanshinone I I A, cryptotanshinone, dihydrotanshinone and iso tanshinone I, iso tanshinone II etc., it is reported, described fat-soluble chemical constituent all has the function of protection myocardial ischemia-anoxemia, anticoagulant, also has obvious antineoplastic; Its water-soluble components is mainly pressure differential self such as salvianolic acid A, B, C, D, E, F, G, danshensu, protocatechualdehyde, protocatechuic acid, and pharmacological research shows that liposoluble ingredient has effects such as antiplatelet aggregation, antithrombotic formation, microcirculation improvement, anti-oxidative damage and myocardial preservation in the Radix Salviae Miltiorrhizae.Version in 2005 " has been set up the method for measuring water soluble ingredient salvianolic acid B and liposoluble constituent Tanshinone I I A in the Radix Salviae Miltiorrhizae respectively in the Chinese pharmacopoeia.But will control the quality of salviamiltiorrhizabung all sidedly, only above-mentioned 2 compositions of measuring wherein are far from being enough, and educational circles is thought, controls the quality of salviamiltiorrhizabung all sidedly and should measure the effective component group that wherein can represent the Radix Salviae Miltiorrhizae effect.
At present, being used for of existing report extracts the water solublity of Radix Salviae Miltiorrhizae simultaneously and the method for liposoluble constituent has the water-bath circumfluence method, ultrasonic extraction, microwave-assisted extraction method etc., but all there is following defective in these methods: consumption of organic solvent is big, extraction time is long, the more high shortcoming of extraction cost, therefore, this area need be set up one fast, and is simple, economic, efficient, reliable extracting method is convenient to simultaneously water solublity in the Radix Salviae Miltiorrhizae and liposoluble constituent be carried out compartment analysis.
Studies show that ultrared wavelength is 0.75 μ m-1000 μ m, between electromagnetic wave and visible light, outwards propagates with radiating form.When the absorbing wavelength of the wavelength of radiation source and heating object was consistent, this material was easy to absorb infrared ray.Material molecule can make the energy of photon be transformed into the vibration or the rotational energy of molecule fully after absorbing infrared energy; The rotational energy of molecule is changed.Infra-red radiation enters in the material body, will strengthen the motion of its component molecule, does the time spent to the constraint that is enough to break away from heating object by force when the component molecular motion, and then component is extracted out.Similar to microwave, infra-red radiation propagates into the heating object surface with the speed of light, and has partial radiation to penetrate interior of articles just to be absorbed, and having to conduct heat fast and object surfaces externally and internally characteristics such as have a narrow range of temperature.Research shows that also infrared ray bulb can change the input electric energy more than 75% into infra-red radiation, and the infra-red radiation more than the 5000nm that gives off because of infrared lamp is all absorbed by glass shell, so infrared lamp can be used as near-infrared and mid-infrared light source.With supersound extraction and microwave-assisted extract phase ratio, utilize the infra-red radiation assisted extraction more economically and safety.
Summary of the invention
The object of the present invention is to provide a kind of new method of extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously, relate in particular to a kind of method of utilizing the infra-red radiation ancillary technique from salviamiltiorrhizabung, to extract water solublity and fat-soluble effective ingredient simultaneously.
The present invention utilizes the infra-red radiation auxiliary extraction technology, extracts water solublity and fat-soluble effective ingredient from salviamiltiorrhizabung simultaneously, and this method is easy, fast, and economy, extraction efficiency height, favorable reproducibility, response rate height.This law combines with high performance liquid chromatography, can be used for accurately measuring the content of 8 kinds of chemical compounds such as salvianolic acid B in the salviamiltiorrhizabung, Tanshinone I I A, can estimate the quality of different places of production Radix Salviae Miltiorrhizae from angle more fully.
In the inventive method, choose the red sage root water soluble ingredient of following structure and the index that the representation compound in the liposoluble constituent is investigated as method, described chemical compound is respectively, water soluble ingredient: danshensu, protocatechuic acid, protocatechualdehyde, salvianolic acid B; Liposoluble constituent: hydrogen TANSHINONES, cryptotanshinone, Tanshinone I and Tanshinone I I A.
The inventive method comprises the steps:
Red rooted salvia is pulverized the back cross 40 mesh sieves, get a certain amount of Danshen Root sample, place round-bottomed flask, after adding a certain amount of extraction solvent, place it on the infra-red radiation, after selecting certain extraction time, utilize the infra-red radiation heat release to extract water solublity and fat-soluble effective ingredient in the Radix Salviae Miltiorrhizae simultaneously, it is centrifugal to extract the back, take out supernatant, danshensu, protocatechuic acid, protocatechualdehyde, salvianolic acid B in the Radix Salviae Miltiorrhizae, hydrogen TANSHINONES, cryptotanshinone, Tanshinone I and Tanshinone I I A content of effective are measured with efficient liquid phase chromatographic analysis in the dilution back.
Among the present invention, its radiation source of described infra-red radiation is hard infrared ray bulb or infrared lamp and infrared electric filament lamp etc.;
In the method for water solublity and fat-soluble effective ingredient, the Radix Salviae Miltiorrhizae sample of adding must sieve after crushed to guarantee certain uniformity in the said extracted Radix Salviae Miltiorrhizae, and sample volume is 0.1-0.5g.
In the method for water solublity and fat-soluble effective ingredient, the extraction solvent of adding is the mixed solvent that water and organic solvent are formed in the said extracted Radix Salviae Miltiorrhizae, and consumption is 5-20mL, and organic solvent content is 50%-90%.This organic solvent can be alcohols such as methanol, ethanol.
In the method for water solublity and fat-soluble effective ingredient, the extraction time of using is 5-20 minute in the said extracted Radix Salviae Miltiorrhizae.
The present invention extracts the method for 8 kinds of water solublity and fat-soluble effective ingredient in the infra-red radiation assisted extraction red rooted salvia, and this method is easy, accurate, reliable, and fast, amount of samples is few, and extraction efficiency is higher, and extraction time is short, favorable reproducibility, response rate height.This law combines with high performance liquid chromatography, can be used for accurately measuring 8 kinds of water solublity and fat-soluble content of effective such as salvianolic acid B in the red rooted salvia, Tanshinone I I A, estimates the quality of red rooted salvia from more comprehensive angle.
Description of drawings
Fig. 1 is 8 kinds of effective ingredient chromatograms in infra-red radiation assisted extraction-high performance liquid chromatography extraction and analysis Radix Salviae Miltiorrhizae.
Fig. 2 is 8 kinds of content of effective disparity map such as salvianolic acid B, Tanshinone I I A in the Radix Salviae Miltiorrhizae of the different places of production.
The specific embodiment
Embodiment 1: 8 kinds of content of effective in the infra-red radiation assisted extraction high-efficient liquid phase chromatogram technique analysis Radix Salviae Miltiorrhizae
Instrument and material:
Instrument: Tianjin, island CL-10 type chromatograph of liquid (comprising SPD-10A UV-detector and CTO-10A column oven, 20 μ L hand sampling systems, chromatographic work station), An Disheng board hard infra-red radiation, Millipore Direct-Q pure water generator.
Material: Radix Salviae Miltiorrhizae (Shandong, the place of production, lot number: 091117,090923; Henan, the place of production, lot number: 090314; Jiangsu, the place of production, lot number: 081207).Acetonitrile (the world, chromatographically pure), the formic acid analytical pure, the deionization pure water is made by Millipore Direct-Q pure water generator, and danshensu, protocatechuic acid, protocatechualdehyde, salvianolic acid B, dihydrotanshinone, cryptotanshinone, Tanshinone I and Tanshinone I I A are accurate, and product derive from Nat'l Pharmaceutical ﹠ Biological Products Control Institute.
Sample pre-treatments:
Red rooted salvia is pulverized the back cross 40 mesh sieves, respectively get the 0.1g Danshen Root then in the 50mL round-bottomed flask, add the 15mL70% methanol aqueous solution, adopt hard infrared ray bulb or infrared electric filament lamp to extract, infrared extraction is after 15 minutes, mend heavy back centrifuging and taking supernatant liquid filtering, danshensu, protocatechuic acid, protocatechualdehyde, salvianolic acid B in the Radix Salviae Miltiorrhizae, hydrogen TANSHINONES, cryptotanshinone, Tanshinone I and Tanshinone I I A content of effective are measured with efficient liquid phase chromatographic analysis in the dilution back.
Embodiment 2: 8 kinds of content of effective in the infra-red radiation assisted extraction high-efficient liquid phase chromatogram technique analysis Radix Salviae Miltiorrhizae
Instrument and material are with embodiment 1
Sample pre-treatments:
Red rooted salvia is pulverized the back cross 40 mesh sieves, respectively get the 0.5g Danshen Root then in the 50mL round-bottomed flask, add the 20mL70% ethanol water, adopt infrared lamp or infrared electric filament lamp to carry out infrared extraction, infrared extraction is after 10 minutes, mend heavy back centrifuging and taking supernatant liquid filtering, danshensu, protocatechuic acid, protocatechualdehyde, salvianolic acid B in the Radix Salviae Miltiorrhizae, hydrogen TANSHINONES, cryptotanshinone, Tanshinone I and Tanshinone I I A content of effective are measured with efficient liquid phase chromatographic analysis in the dilution back.
Claims (7)
1. a method of extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously is characterized in that, utilizes the infra-red radiation ancillary technique, extracts water solublity and fat-soluble effective ingredient from salviamiltiorrhizabung simultaneously, and it comprises the steps:
Red rooted salvia is pulverized the back cross 40 mesh sieves, get quantitative Danshen Root sample, place round-bottomed flask, after adding quantitative extraction solvent, place it on the infra-red radiation, after selected extraction time, extract water solublity and fat-soluble effective ingredient in the Radix Salviae Miltiorrhizae simultaneously, the extraction back is centrifugal, takes out supernatant, dilutes the content of back with the representation compound in water soluble ingredient and the liposoluble constituent in the efficient liquid phase chromatographic analysis mensuration Radix Salviae Miltiorrhizae.
2. the method for extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously according to claim 1, it is characterized in that the representation compound in the described Radix Salviae Miltiorrhizae in water soluble ingredient and the liposoluble constituent is: water soluble ingredient is danshensu, protocatechuic acid, protocatechualdehyde and salvianolic acid B; Liposoluble constituent is hydrogen TANSHINONES, cryptotanshinone, Tanshinone I and Tanshinone I I A.
3. the method for extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously according to claim 1 is characterized in that the described source of infrared radiation is selected from hard infrared ray bulb or infrared lamp or infrared electric filament lamp.
4. the method for extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously according to claim 1 is characterized in that described sample volume is 0.1-0.5g.
5. the method for extracting water solublity and fat-soluble effective ingredient in the salviamiltiorrhizabung simultaneously according to claim 1 is characterized in that described extraction solvent is the mixed solvent of water and organic solvent, and volume is 5-20mL.
6. method according to claim 6 is characterized in that, described organic solvent is methanol or ethanol, and organic solvent content is 50%-90%.
7. method according to claim 1 is characterized in that, the time of described infra-red radiation is 5-20 minute.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103070446A (en) * | 2013-02-26 | 2013-05-01 | 薛秀云 | Red ginseng liquid and production method thereof |
| CN103512981A (en) * | 2012-06-19 | 2014-01-15 | 复旦大学 | Method for ion liquid-infrared assisted extraction of effective components of traditional Chinese medicine |
| CN104849379A (en) * | 2014-02-13 | 2015-08-19 | 天士力制药集团股份有限公司 | Method for measuring danshensu, m-methyl-danshensu, protocatechualdehyde, and protocatechuic acid in human blood plasma |
| CN108148028A (en) * | 2016-12-06 | 2018-06-12 | 复旦大学 | A kind of method of tanshin polyphenolic acid B ingredient in extraction salviamiltiorrhizabung |
| CN109320486A (en) * | 2017-08-01 | 2019-02-12 | 复旦大学 | A kind of method of amentoflavone in infrared extraction Selaginella tamariscina |
| CN111426634A (en) * | 2019-11-21 | 2020-07-17 | 四川省中医药科学院 | Method for detecting content of main chemical components of salvia miltiorrhiza medicinal material powder according to color of salvia miltiorrhiza medicinal material powder |
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2009
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103512981A (en) * | 2012-06-19 | 2014-01-15 | 复旦大学 | Method for ion liquid-infrared assisted extraction of effective components of traditional Chinese medicine |
| CN103070446A (en) * | 2013-02-26 | 2013-05-01 | 薛秀云 | Red ginseng liquid and production method thereof |
| CN104849379A (en) * | 2014-02-13 | 2015-08-19 | 天士力制药集团股份有限公司 | Method for measuring danshensu, m-methyl-danshensu, protocatechualdehyde, and protocatechuic acid in human blood plasma |
| CN104849379B (en) * | 2014-02-13 | 2017-10-31 | 天士力制药集团股份有限公司 | The method of danshensu in one kind measure human plasma, meta methyl danshensu, protocatechualdehyde and protocatechuic acid |
| CN108148028A (en) * | 2016-12-06 | 2018-06-12 | 复旦大学 | A kind of method of tanshin polyphenolic acid B ingredient in extraction salviamiltiorrhizabung |
| CN109320486A (en) * | 2017-08-01 | 2019-02-12 | 复旦大学 | A kind of method of amentoflavone in infrared extraction Selaginella tamariscina |
| CN111426634A (en) * | 2019-11-21 | 2020-07-17 | 四川省中医药科学院 | Method for detecting content of main chemical components of salvia miltiorrhiza medicinal material powder according to color of salvia miltiorrhiza medicinal material powder |
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