CN103044424B - A kind of method of matrine in enriching and purifying kuh-seng - Google Patents
A kind of method of matrine in enriching and purifying kuh-seng Download PDFInfo
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- CN103044424B CN103044424B CN201210595624.3A CN201210595624A CN103044424B CN 103044424 B CN103044424 B CN 103044424B CN 201210595624 A CN201210595624 A CN 201210595624A CN 103044424 B CN103044424 B CN 103044424B
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Abstract
The invention belongs to field of natural organic chemistry, relate to a kind of purification process of matrine, particularly relate to a kind of preparation method utilizing matrine in ultrasonic extraction one high speed adverse current chromatogram partition method enriching and purifying kuh-seng.Advantage of the present invention is: 1, adopt ultrasonic extraction matrine to have and extract completely, simple to operate, time saving advantage; 2, high speed adverse current chromatogram partition method is utilized to obtain the matrine of 98% purity through twice purifying from natural phant kuh-seng vat liquor.This law is applicable to the various natural phant containing matrine, and the extract of natural phant is that highly purified matrine prepared by raw material.Be applicable to adopt the counter current chromatograph of various model to be separated and prepare matrine, with high-speed countercurrent chromatography prepare matrine can continuously, efficiently, fast liquid liquid distribution chromatography be separated, have that fractional dose is large, sample nondestructive loses, the rate of recovery is high, isolating environment relaxes, save the features such as solvent.
Description
Technical field:
The invention belongs to field of natural organic chemistry, relate to a kind of purification process of matrine, particularly relate to a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng.
Background technology:
Kuh-seng: be the root of perennial fallen leaves semishrub plant kuh-seng, containing multiple alkaloid and multiple flavonoid compound, with matrine (Matrine) in alkaloid, Oxymatyine (Oxymatrine) is main, still has Iosmatrine (Isomatrine), sophocarpine (Sophocarpine), different sophocarpine (Isosopho-carpine), sophoramine (Sophoramine), Sophocarpidin (Noxysophocarpine), the d-Sophoranol (d-Sophoranole) of trace, I-rhombinin (I-Anagyrine), I-methylcytisine (I-Methylcytisine), counterfeit indigo leaf alkali (Bapti-foline), I-sophocarpines (I-Sophocarpine) etc., have picrol C (kushenolC) in flavonoid compound, picrol G (KushenolG), Vexibidin (Isokurarinone), kuh-seng alcohol (Kurannol), neokurarinol (Neokurannol), kuh-seng alcohol (Norkurannol) falls, neochanin (Formononetin), Kuraridine alcohol (Kuraridinol), kurarinone (Kurarinone), secondary kurarinones (Kurandin) etc., have obvious restraining effect to heart, can anti-heart disorder, and reduce blood pressure, and have resisting pathogenic microbes, relieving asthma and eliminate the phlegm, the effects such as leukocyte increasing.
Matrine is a kind of natural active matter human health being had to remarkable health-care effect, caused the common concern of international community: prove through scientific research and clinical application, matrine had antitumor, leukocyte increasing, relieving asthma eliminate the phlegm, ease pain, antianaphylaxis and immunosuppressive action.In recent years, it is found that, containing a large amount of matrines in natural phant kuh-seng, therefrom extract matrine and achieve encouraging progress, because its raw material kuh-seng is Chinese medicine, raw material sources are wider.Name is called in the patent application of " method extracting matrine from kuh-seng " just to disclose extracts matrine technical process by kuh-seng through solvent extration optimization.Matrine extraction process in above-mentioned patent documentation is mainly through solvent extraction, and adsorption resin column carries out the processing step extractions such as purifying and forms, and its separating effect is nothing like the separating effect of high speed adverse current chromatogram partition method.
Summary of the invention:
The object of the invention is to overcome the shortcomings such as routine techniques extraction yield is relatively low, DNA purity is low, a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng is provided.For achieving the above object, the technical solution used in the present invention is: a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng.Its step is as follows:
(1) pulverized by dry kuh-seng, carry out ultrasonic extraction with the acetone soln that concentration is 70%, Extracting temperature is 50 ~ 60 DEG C, extracts frequency 80 ~ 100Hz, 1 ~ 2 hour extraction time, extracts 3 times;
(2) Radix Sophorae Flavescentis extractive liquid (1) processed filters, and merges No. three extracting solutions, after boiling off acetone, obtains primary extract;
(3) preliminary purification of matrine: primary extract high speed adverse current chromatogram partition method is carried out initial gross separation, collects the component containing matrine, solvent evaporated;
(4) kuh-seng is refining: the matrine sterling again (3) obtained component high speed adverse current chromatogram partition method being made high purity more than 98%:
High-speed countercurrent chromatography carries out preliminary purification to kuh-seng, and available solvent system mainly contains three.All above is stationary phase mutually, and lower is moving phase mutually, and the flow velocity of moving phase is 2.0ml/min.A solvent system is made up of three components, and A1 component can select the fatty lipids such as ethyl acetate, acetic acid lactone, isopropyl acetate, n-butyl acetate; B1 component can select the fatty alcohol such as propyl carbinol, isopropylcarbinol, the trimethyl carbinol; C1 component is water; Ethyl acetate-tertiary butanol and water system, A1, B1, C1 volume ratio is 0.5-2: 2-10: 2-10.No. two solvent systems are made up of four components, and A2 component can select the ester fatty ester classes such as ethyl acetate, propyl acetate, isopropyl acetate, n-butyl acetate; B2, C2 component can select fatty alcohol or the aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, Virahol, acetone, propyl carbinol, isopropylcarbinol, the trimethyl carbinol; D2 component is water; The ethyl acetate trimethyl carbinol-acetone-water system, A2, B2, C2, D2 volume ratio is 0.5-5: 10-100: 0.5-5: 10-100.Number solvent system is made up of two components, and A3 component can select the fatty alcohol such as propyl carbinol, isopropylcarbinol, the trimethyl carbinol; B3 component is water; Preferred tertiary fourth alcohol-water system, A3, B3 volume ratio is 1-100: 1-100.
High speed adverse current chromatogram partition method mainly contains two to matrine refining solvent system.All above is stationary phase mutually, and lower is moving phase mutually, and the flow velocity of moving phase is 2.0ml/min.No. four solvent systems are made up of two components, and A4 component can select the halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin; B4 component can select fatty alcohol or the aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, acetone; C4 component is water, preferred dichloromethane-ethanol-aqueous systems; A4, B4, C4 volume ratio is 2-10: 2-15: 1-10.No. five solvent systems are made up of four components, and A5 component can select the halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin; B5, C5 component can select fatty alcohol or the aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, Virahol, acetone, propyl carbinol, isopropylcarbinol, the trimethyl carbinol; D5 component is water; Preferred chloroform-isopropanol-methanol-water solution, A5, B5, C5, D5 volume ratio is 1-10: 0.5-5: 1-10: 0.5-10.No. six solvent systems are made up of five components, and A6, C6 component can select the halohydrocarbon such as chloroform, methylene dichloride, tetracol phenixin; B6, D6 component can select fatty alcohol or the aliphatic ketones such as methyl alcohol, ethanol, propyl alcohol, Virahol, acetone, propyl carbinol, isopropylcarbinol, the trimethyl carbinol; E6 component is water; Preferred methylene dichloride-Virahol-chloroform-methanol-aqueous systems, A6, B6, C6, D6, E6 volume ratio is 0.5-2: 0.5-2: 1-10: 2-10: 1-10.
In described step (1), kuh-seng crosses 60 ~ 80 mesh sieves after pulverizing.
In described step (1), the volume adding ethanol is 6 ~ 8 times that pulverize volume.
It is carry out at 15-30 DEG C that experiment is applicable to room temperature.
The matrine purity prepared by this law can reach more than 98%.This law is applicable to the various natural phant containing matrine, and the extract of natural phant is that highly purified matrine prepared by raw material.Be applicable to adopt the counter current chromatograph of various model to be separated and prepare matrine, utilize ultrasonic extraction matrine to have and extract completely, simple to operate, save time; Utilize high-speed countercurrent chromatography prepare matrine can continuously, efficiently, fast liquid liquid distribution chromatography be separated, there is fractional dose people, sample nondestructive lose, high, the isolating environment of the rate of recovery relaxes, save the features such as solvent
Embodiment:
Case study on implementation 1: a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng, its step is as follows:
(1) cross 60 mesh sieves after being pulverized by dry for 100g kuh-seng, carry out ultrasonic extraction with the acetone soln that concentration is 70%, solid-liquid ratio is 6 times that pulverize volume, and Extracting temperature is 50 DEG C, extracts frequency 80Hz, 1 hour extraction time, extracts 3 times;
(2) Radix Sophorae Flavescentis extractive liquid (1) processed filters, and merges No. three extracting solutions, after boiling off acetone, obtains primary extract;
(3) preliminary purification of matrine: primary extract high speed adverse current chromatogram partition method is carried out initial gross separation, collects the component containing matrine, steams solvent;
(4) kuh-seng is refining: again (3) obtained component high speed adverse current chromatogram partition method is made high purity 98.2% matrine sterling;
Ethyl acetate-tertiary butanol and water and chloroform-isopropanol-methanol-water two solvent system is adopted to prepare the matrine of purity high fourth 98%; Use semi-preparative high-speed counter-current chromatograph, be furnished with NS-1007 pump, 20ml sampling valve, tetrafluoroethylene post, the volume of post is 2-10ml, 8823A-UV UV-detector Yokogawa3057 Portable type recorder.Before sample introduction, first be full of whole pillar with stationary phase, adjustment engine speed is 800rpm, with the flow velocity of 2.0ml/min, moving phase is pumped in post, after whole Establishing running balance, by sampling valve sample introduction, then according to detector uv-spectrogram, the preparation of receiving target composition matrine is carried out in two steps: (1) by volume ratio be 1: 3: 5 ethyl acetate-tertiary butanol and water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, lower floor's solution (lower phase) for moving phase with 1: 1 the crude extract 100mg that obtains of upper and lower phase mixed solution 20ml dissolving be separated, collect the component containing matrine, evaporate to dryness (2) by volume ratio be 5: 0.5: 5: 4 chloroform-isopropanol-methanol-water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, and lower floor's solution (lower phase) is moving phase.Upper and lower phase mixed solution 2ml with 1: 1 dissolves (1) gained sample and is separated, and collects the component peaks containing matrine, lyophilize.Obtain white matrine solid, analyze through HPLC, its purity reaches 98.2%.
Case study on implementation 2: a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng, its step is as follows:
(1) cross 70 mesh sieves after being pulverized by dry for 100g kuh-seng, carry out ultrasonic extraction with the acetone soln that concentration is 70%, solid-liquid ratio is 7 times that pulverize volume, and Extracting temperature is 55 DEG C, extracts frequency 90Hz, 1.5 hours extraction times, extracts 3 times;
(2) Radix Sophorae Flavescentis extractive liquid (1) processed filters, and merges No. three extracting solutions, after boiling off acetone, obtains primary extract;
(3) preliminary purification of matrine: primary extract high speed adverse current chromatogram partition method is carried out initial gross separation, collects the component containing matrine, steams solvent;
(4) kuh-seng is refining: again (3) obtained component high speed adverse current chromatogram partition method is made high purity 98.33% matrine sterling;
Adopt the ethyl acetate-trimethyl carbinol-acetone-water and dichloromethane-ethanol-water two solvent system prepare purity higher than 98% matrine: use semi-preparative high-speed counter-current chromatograph, is furnished with NS-1007 pump, 20ml sampling valve, tetrafluoroethylene post, the volume of post is 210ml, 8823A-UV UV-detector Yokogawa3057 Portable type recorder.Before sample introduction, be first full of whole pillar with stationary phase, adjustment engine speed is 800rpm, with the flow velocity of 2.0ml/min, moving phase is pumped in post, after whole Establishing running balance, by sampling valve sample introduction, then according to detector uv-spectrogram, receiving target composition.The preparation of matrine is carried out in two steps: (1) by volume ratio be 5: 50: 1: 60 ethyl acetate-trimethyl carbinol acetone-water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, and lower floor's solution (lower phase) is moving phase.The crude extract 200mg that upper and lower phase mixed solution 20ml dissolving with 1: 1 obtains is separated, and collects the component containing matrine, evaporate to dryness.(2) by volume ratio be 8: 15: 8 dichloromethane-ethanol-water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, and lower floor's solution (lower phase) is moving phase.Upper and lower phase mixed solution 2ml with 1: 1 dissolves (1) gained sample and is separated, and collects the component peaks containing matrine, lyophilize.Obtain white matrine solid, analyze through HPLC, its purity reaches on 98.33%.
Case study on implementation 3: a kind of preparation method utilizing matrine in ultrasonic extraction-high speed adverse current chromatogram partition method enriching and purifying kuh-seng, its step is as follows:
(1) cross 80 mesh sieves after being pulverized by dry for 100g kuh-seng, carry out ultrasonic extraction with the acetone soln that concentration is 70%, solid-liquid ratio is 8 times that pulverize volume, and Extracting temperature is 60 DEG C, extracts frequency 100Hz, 2 hours extraction times, extracts 3 times;
(2) Radix Sophorae Flavescentis extractive liquid (1) processed filters, and merges No. three extracting solutions, after boiling off acetone, obtains primary extract;
(3) preliminary purification of matrine: primary extract high speed adverse current chromatogram partition method is carried out initial gross separation, collects the component containing matrine, solvent evaporated;
(4) kuh-seng is refining: again (3) obtained component high speed adverse current chromatogram partition method is made the matrine sterling that high purity is 98.12%;
Adopt tertiary butanol and water and methylene dichloride-Virahol-chloroform-methanol-water two solvent system prepare purity higher than 98% matrine: use semi-preparative high-speed counter-current chromatograph, is furnished with NS-1007 pump, 20ml sampling valve, tetrafluoroethylene post, the volume of post is 210ml, 8823AUV UV-detector Yokogawa3057 Portable type recorder.Before sample introduction, be first full of whole pillar with stationary phase, adjustment engine speed is 800rpm, with the flow velocity of 2.0ml/min, moving phase is pumped in post, after whole Establishing running balance, by sampling valve sample introduction, then according to detector uv-spectrogram, receiving target composition.The preparation of matrine is carried out in two steps: (1) by volume ratio be 13: 55 tertiary butanol and water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, and lower floor's solution (lower phase) is moving phase.The crude extract 150mg that upper and lower phase mixed solution 20ml dissolving with 1: 1 obtains is separated, and collects the component of matrine, evaporate to dryness.(2) by volume ratio be 1: 1: 5: 8: 6 methylene dichloride-Virahol-chloroform-methanol-water miscible in separating funnel, shake up rear static layering.Getting its upper solution (upper phase) is stationary phase, and lower floor's solution (lower phase) is moving phase.Upper and lower phase mixed solution 2ml with 1: 1 dissolves (1) gained sample and is separated, and collects the component peaks containing matrine, lyophilize.Obtain white matrine solid, analyze through HPLC, its purity reaches 98.12%.
Claims (5)
1. utilize a method for matrine in ultrasonic extraction-high-speed countercurrent chromatography enriching and purifying kuh-seng, its step is as follows:
(1) pulverized by dry kuh-seng, carry out ultrasonic extraction with the acetone soln that concentration is 70%, Extracting temperature is 50 ~ 60 DEG C, extracts frequency 80 ~ 100Hz, 1 ~ 2 hour extraction time, extracts 3 times;
(2) Radix Sophorae Flavescentis extractive liquid (1) processed filters, and merges No. three extracting solutions, after boiling off acetone, obtains primary extract;
(3) preliminary purification of matrine: primary extract high speed adverse current chromatogram partition method is carried out initial gross separation, collects the component containing matrine, solvent evaporated;
(4) kuh-seng is refining: the matrine sterling again (3) obtained component high speed adverse current chromatogram partition method being made high purity more than 98%;
In described step (3) and (4), high speed adverse current chromatogram partition method is in matrine initial gross separation and treating process, and all above is stationary phase mutually, and lower is moving phase mutually, and the flow velocity of moving phase is 2.0ml/min.
2. a kind of method utilizing matrine in ultrasonic extraction-high-speed countercurrent chromatography enriching and purifying kuh-seng according to claim 1, is characterized in that: in described step (1), and kuh-seng crosses 60 ~ 80 mesh sieves after pulverizing.
3. a kind of method utilizing matrine in ultrasonic extraction-high-speed countercurrent chromatography enriching and purifying kuh-seng according to claim 2, is characterized in that: in described step (1), and solid-liquid ratio is 6 ~ 8 times that pulverize volume.
4. a kind of method utilizing matrine in ultrasonic extraction-high-speed countercurrent chromatography enriching and purifying kuh-seng according to claim 3, it is characterized in that: by high speed adverse current chromatogram partition method, preliminary purification is carried out to matrine, optional solvent system is made up of three individual system, a solvent system preferential ethyl acetate-tertiary butanol and water system, volume ratio is 0.5-2: 2-10: 2-10; No. two solvent system ethyl acetate-trimethyl carbinol-acetone-water system, volume ratio is 0.5-5: 10-100: 0.5-5: 10-100; No. three solvent system preferred tertiary fourth alcohol-water systems, volume ratio is 1-100: 1-100.
5. a kind of method utilizing matrine in ultrasonic extraction-high-speed countercurrent chromatography enriching and purifying kuh-seng according to claim 4, it is characterized in that: by high speed adverse current chromatogram partition method, matrine refining solvent system is made up of three components, No. four preferred dichloromethane-ethanol-aqueous systems of solvent system, volume ratio is 2-10: 2-15: 1-10; No. five preferred chloroform-isopropanol-methanol-water solution of solvent system, volume ratio is 1-10: 0.5-5: 1-10: 0.5-10; No. six preferred methylene dichloride-Virahol-chloroform-methanol-aqueous systems of solvent system, volume ratio is 0.5-2: 0.5-2: 1-10: 2-10: 1-10.
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| CN106565714A (en) * | 2016-11-08 | 2017-04-19 | 南安创友日化有限公司 | Method for separating oxymatrine from sophora tonkinensis |
| CN109331061B (en) * | 2018-11-13 | 2021-09-14 | 南京中医药大学 | Kuh-seng flavonoid effective part with tyrosinase inhibitory activity and antibacterial activity, preparation method and application thereof |
| CN115624577A (en) * | 2022-09-09 | 2023-01-20 | 厦门海关技术中心 | Sophora flavescens alkaloids, extraction and purification method thereof, and method for detecting Sophora flavescens alkaloids |
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