CN102772499B - Effective parts obtained by alcohol extraction of raw materials of Relingqing granules as well as preparation method and applications thereof - Google Patents
Effective parts obtained by alcohol extraction of raw materials of Relingqing granules as well as preparation method and applications thereof Download PDFInfo
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Abstract
The invention relates to effective parts obtained by alcohol extraction of raw materials of Relingqing granules as well as a preparation method and applications thereof, and particularly relates to extracts of Polygonum capitatum Buch-Ham ex D.Don. The preparation method comprises the following steps of: (1) adding 50-90% alcohol in Polygonum capitatum Buch-Ham ex D.Don overground part fresh product or dried product, carrying out reflux extraction for 1-3 times, filtering, and concentrating and drying filtrate to obtain alcoholic extract, wherein the amount of the added alcohol is 5-15 times that of the Polygonum capitatum Buch-Ham ex D.Don overground part fresh product or dried product; (2) suspending the alcoholic extract in methanol, ultrasonically treating for 0.5-5 hours, centrifuging, and loading supernate on an MCI macroporous resin column; and (3) performing gradient eluting successively by using water and 10-100% methanol, collecting all eluents, recovering solvents, drying parts obtained after elution of different solvents to obtain methanol eluates with any concentration interval or concentration point in the range of 30-50% or the mixtures of the methanol eluates, thus obtaining the effective parts namely extracts of Polygonum capitatum Buch-Ham ex D.Don. The extracts of Polygonum capitatum Buch-Ham ex D.Don disclosed by the invention have the beneficial effects as described in the specification.
Description
Technical field
The invention belongs to the field of Chinese medicines, is the extract of medicinal material Polygonum capitatum for the preparation of the raw material of the clear granule of Chinese medicine pyretic stranguria.Particularly, the present invention relates to the raw material clear by pyretic stranguria and be the effective site that the alcohol extract of medicinal material Polygonum capitatum obtains, and the preparation method of this effective site and purposes.
Background technology
Herba Polygoni Capitati (Polygonum capitatum Buch-Ham ex D.Don) is Polygonaceae Polygonum herbaceos perennial.Effect with clearing away heat-damp and promoting diuresis, inducing diuresis for treating stranguria syndrome, treating clinically urinary system infection has significant effect.Its Chinese patent medicine preparation made as raw material " the clear granule of pyretic stranguria " of take enters national basic medical insurance catalogue in 2004, within 2012, enters Guizhou Province's essential drug list.
Herba Polygoni Capitati is the common medicine of minority area, is mainly used in the diseases such as pyelonephritis, urinary tract infection, inducing diuresis for treating stranguria syndrome.Relevant pharmaceutical research is rare, and several pieces of reports such as Ren Guangyou are only arranged at present.Ren Guangyou adopts rat bacterial pyelonephritis model to be tested, and the WBC in Herba Polygoni Capitati water extract group rat urine and BLD and the apparent in view minimizing of matched group as a result shows that the Herba Polygoni Capitati water extract has certain antiinflammatory action to pyelonephritis.Ren Guangyou etc. observe dead mouse situation in 5 days with mouse peritoneal Escherichia Coli Injection bacterium liquid, and the matched group mortality rate is 100% as a result, and Herba Polygoni Capitati group mortality rate is respectively 20% and 50%, show that the Herba Polygoni Capitati water extract can resist the infection that escherichia coli cause.Ren Guangyou etc. give rabbit with Herba Polygoni Capitati water extract gastric infusion, result, Herba Polygoni Capitati water extract group and matched group relatively, body temperature there was no significant difference, but can reduce the heating body temperature of the rabbit that the intravenous injection TAB causes.Ren Guangyou etc., with Herba Polygoni Capitati water extract respectively gastric infusion rabbit, rat, with blank group and furosemide matched group urine amount relatively.Result show the Herba Polygoni Capitati water extract to rabbit and rat without obvious diuresis.The people such as the Xu Yingchun In Vitro Bacteriostatic of Herba Polygoni Capitati to 10 strain Neisseria gonorrhoeae (gonococcus) that adopted agar dilution to detect, Herba Polygoni Capitati has bacteriostatic activity to gonococcus as a result.It is 8 ~ 32g/L to the gonococcal minimal inhibitory concentration scope of 10 strain, and meansigma methods is 11.2g/L.
Chinese patent application prospectus CN1054899A discloses a kind of miganling instant herbal medicine, syrup production technology in (Chinese Patent Application No. 90107810.7, open day on October 2nd, 1991).This production technology is to take four seasons grass as raw material water decoction 30-60 minute, extracting liquid filtering is concentrated, its supernatant concentrating under reduced pressure is become to cream, use again the 60-70% ethanol extraction, by the ethanol extract vacuum drying, Herba Polygoni Capitati extractum, further be mixed with electuary or syrup, it is believed that it has removing toxic substances, dissipating blood stasis, diuresis, treating stranguria effect.
Recorded the Chinese patent medicine preparation of " the clear granule of pyretic stranguria " by name in Ministry of Health of the People's Republic of China's " drug standard-Traditional Chinese medicine historical preparation " (the 17) that Ministry of Health of the People's Republic of China's committee of pharmacopeia is compiled in 1998, it is made by Herba Polygoni Capitati being decocted with water to twice rear filtering and concentrating.
CN1481832A (Chinese Patent Application No. 02129686.3, disclosed day on March 17th, 2004) and CN1483466A (Chinese Patent Application No. 03146381.9, open day on March 24th, 2004) Herba Polygoni Capitati extract is disclosed, it is prepared by following steps basically: a. is by the fresh goods of Herba Polygoni Capitati herb or the dry product water decocts at twice or divide reflux, extract, two to three times with alcohol-water mixture, each 1-2 hour, merge decoction liquor, relative density during filtering and concentrating to 20 ℃ is 1.2, and spray drying or drying under reduced pressure obtain; Perhaps, b. is obtained through carbon dioxide supercritical fluid extraction by Herba Polygoni Capitati herb and water extraction medicinal residues thereof.It is believed that this extract can be used for antibiotic, antiinflammatory, analgesia, diuresis, treatment urinary system calculus, treatment pyelonephritis and prostatitis.
Although have at present many about preparing the report of Herba Polygoni Capitati extract, yet those skilled in the art still expect to obtain more efficiently product from Herba Polygoni Capitati.
Summary of the invention
The present invention seeks to expect to obtain a kind of effective product from Herba Polygoni Capitati.The inventor finds, uses the alcohol extraction Herba Polygoni Capitati, the eluate that the extract obtained obtains through specific macroporous resin eluting, and it has the effect of desirable aspect biological activity.The present invention is based on this discovery and be accomplished.
For this reason, first aspect present invention provides a kind of Herba Polygoni Capitati extract, and it is prepared by the method comprised the following steps basically:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 5-15 and doubly measure that (for example 5-12 doubly measures, for example 6-10 doubly measures) 50 ~ 90% (for example 60 ~ 80%, for example 65 ~ 75%, for example approximately 70%) alcohol reflux 1-3 time (for example 2 times), each 1-3 hour (for example approximately 1.5 hours), filter, make filtrate concentrated, dry, obtain pure extractum;
(2) pure extractum is suspended in methanol, supersound process 0.5 ~ 5 hour (for example 0.5 ~ 3 hour, for example 1 ~ 2 hour, for example approximately 1.5 hours), centrifugal, supernatant (for example is loaded into to the MCI macroporous resin column, it is the 0.5-4 liter that every 100g extractum is used the amount of resin, 1-3 liter for example, 1.5-2.5 liter for example, for example 2 liters) on;
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out successively gradient elution (for example every kind of solvent load is 0.5 ~ 5 times of column volume, 0.5 ~ 2.5 times of column volume for example, 0.5 ~ 2 times of column volume for example, 1 times of column volume for example), collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtain the methanol-eluted fractions thing of any concentration interval between 30%-50% or concentration point, perhaps their mixture, obtain.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 30% methanol-eluted fractions thing (in the present invention can referred to as: position A).
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 35%-40% methanol-eluted fractions thing (in the present invention can referred to as: position B).
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40% methanol-eluted fractions thing (in the present invention can referred to as: position C).
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40%-50% methanol-eluted fractions thing (in the present invention can referred to as: position D).
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein step (3) gained methanol-eluted fractions thing be methanol-eluted fractions thing between 30%-50% mixture (in the present invention can referred to as: position X).In the present invention, this position X can be the mixture of position A to position D dry product, can also be that 30%-50% methanol-eluted fractions gained mixed liquor is through desolventizing dried dry product.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein in the A of position, contain for example digalloylglucose of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein in the B of position, contain for example trigalloylglucose of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein in the C of position, contain hydrolysable tannin and/or procyanidin.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein in the D of position, contain for example hydrolysable tannin davidiin of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of first aspect present invention, wherein in the X of position, contain hydrolysable tannin and/or procyanidin, for example digalloylglucose, trigalloylglucose, procyanidin and/or hydrolysable tannin davidiin.
According to the Herba Polygoni Capitati extract of first aspect present invention, it is measured according to Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method (in the present invention can referred to as UPLC-TOF-MS), result:
(a) show the chromatographic peak of hydrolysable tannin (for example digalloylglucose) between retention time 1-3min;
(b) between retention time 3.4-4.4min for example, between (about 3.9min place) and retention time 4.8-5.8min (for example about 5.3min place) show the chromatographic peak of hydrolysable tannin (for example trigalloylglucose);
(c) between retention time 3.4-4.4min for example, between (about 3.9min place), retention time 4.8-5.8min for example, between (about 5.3min place), retention time 8.2-9.2min for example, between (about 8.7min place), retention time 12.0-13.0min (for example about 12.5min place) show the chromatographic peak of hydrolysable tannin, and/or for example, for example, for example, at the chromatographic peak of (about 9.1min place) demonstration procyanidin between (about 8.6min place), retention time 8.6-9.6min between (about 6.7min place), retention time 8.1-9.1min between retention time 6.2-7.2min;
(d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min; And/or
(x) show arbitrary or whole chromatographic peak shown in above (a) to (d);
Wherein, the assay method of UPLC-TOF-MS is as follows:
(i) test liquid preparation: take appropriate Herba Polygoni Capitati extract powder, add 70% methanol to make the suspension of the about 5mg/ml of concentration, ultrasonic making dissolved as far as possible, and 10 times of suspension dilutions, filter, and sample introduction 2 μ l make Mass Spectrometer Method;
(ii) chromatograph and mass spectral analysis condition:
Chromatographic column: Acquity BEH C18 post (2.1 * 100mm, 1.7 μ m), column temperature: 40 ℃; Flow velocity: 0.35ml/min; Sample size: 2 μ l; Mass spectrum condition: ion source: ESI source; Dry gas temperature: 180 ℃; Capillary voltage: 4500eV; Detecting pattern: negative ion mode; Atomisation pressure: 2.5bar; Dry gas (N2) flow velocity: 8L/min; Sweep limits: 100-2000amu; Collision energy: 10ev; Take 0.1% aqueous formic acid as mobile phase A, and 0.1% formic acid acetonitrile solution is Mobile phase B, and the according to the form below regulated procedure is carried out gradient elution:
| Time (min) | A(%) | B(%) |
| 0 | 95 | 5 |
| 0.5 | 95 | 5 |
| 20 | 81.5 | 18.5 |
| 28 | 0 | 100 |
| 30 | 0 | 100 |
| 30.1 | 95 | 5 |
| 32 | 95 | 5 |
Herba Polygoni Capitati extract according to first aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: the chromatographic peak that (a) between retention time 1-3min, shows hydrolysable tannin (for example digalloylglucose).
Herba Polygoni Capitati extract according to first aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (b) for example, for example, for example, at the chromatographic peak of (about 5.3min place) demonstration hydrolysable tannin (trigalloylglucose) between (about 3.9min place) and retention time 4.8-5.8min between retention time 3.4-4.4min.
Herba Polygoni Capitati extract according to first aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (c) between retention time 3.4-4.4min (for example about 3.9min place), for example, between retention time 4.8-5.8min (about 5.3min place), for example, between retention time 8.2-9.2min (about 8.7min place), between retention time 12.0-13.0min, (for example about 12.5min place) shows the chromatographic peak of hydrolysable tannin, and/or for example, between retention time 6.2-7.2min (about 6.7min place), for example, between retention time 8.1-9.1min (about 8.6min place), between retention time 8.6-9.6min, (for example about 9.1min place) shows the chromatographic peak of procyanidin.
Herba Polygoni Capitati extract according to first aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min.
According to the Herba Polygoni Capitati extract of first aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result:
(a) show the chromatographic peak of hydrolysable tannin (for example digalloylglucose) between retention time 1-3min;
(b) between retention time 3.4-4.4min for example, between (about 3.9min place) and retention time 4.8-5.8min (for example about 5.3min place) show the chromatographic peak of hydrolysable tannin (for example trigalloylglucose);
(c) between retention time 3.4-4.4min for example, between (about 3.9min place), retention time 4.8-5.8min for example, between (about 5.3min place), retention time 8.2-9.2min for example, between (about 8.7min place), retention time 12.0-13.0min (for example about 12.5min place) show the chromatographic peak of hydrolysable tannin, and/or for example, for example, for example, at the chromatographic peak of (about 9.1min place) demonstration procyanidin between (about 8.6min place), retention time 8.6-9.6min between (about 6.7min place), retention time 8.1-9.1min between retention time 6.2-7.2min; And/or
(d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min.
According to the Herba Polygoni Capitati extract of first aspect present invention, it has the described feature of the arbitrary embodiment of second aspect present invention.
Second aspect present invention provides a kind of Herba Polygoni Capitati extract, and it is measured according to Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method (in the present invention can referred to as UPLC-TOF-MS), result:
(a) show the chromatographic peak of hydrolysable tannin (for example digalloylglucose) between retention time 1-3min;
(b) between retention time 3.4-4.4min for example, between (about 3.9min place) and retention time 4.8-5.8min (for example about 5.3min place) show the chromatographic peak of hydrolysable tannin (for example trigalloylglucose);
(c) between retention time 3.4-4.4min for example, between (about 3.9min place), retention time 4.8-5.8min for example, between (about 5.3min place), retention time 8.2-9.2min for example, between (about 8.7min place), retention time 12.0-13.0min (for example about 12.5min place) show the chromatographic peak of hydrolysable tannin, and/or for example, for example, for example, at the chromatographic peak of (about 9.1min place) demonstration procyanidin between (about 8.6min place), retention time 8.6-9.6min between (about 6.7min place), retention time 8.1-9.1min between retention time 6.2-7.2min;
(d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min; And/or
(x) show arbitrary or whole chromatographic peak shown in above (a) to (d);
Wherein, the assay method of UPLC-TOF-MS is as follows:
(i) test liquid preparation: take appropriate Herba Polygoni Capitati extract powder, add 70% methanol to make the suspension of the about 5mg/ml of concentration, ultrasonic making dissolved as far as possible, and 10 times of suspension dilutions, filter, and sample introduction 2 μ l make Mass Spectrometer Method;
(ii) chromatograph and mass spectral analysis condition:
Chromatographic column: Acquity BEH C18 post (2.1 * 100mm, 1.7 μ m), column temperature: 40 ℃; Flow velocity: 0.35ml/min; Sample size: 2 μ l; Mass spectrum condition: ion source: ESI source; Dry gas temperature: 180 ℃; Capillary voltage: 4500eV; Detecting pattern: negative ion mode; Atomisation pressure: 2.5bar; Dry gas (N2) flow velocity: 8L/min; Sweep limits: 100-2000amu; Collision energy: 10ev; Take 0.1% aqueous formic acid as mobile phase A, and 0.1% formic acid acetonitrile solution is Mobile phase B, and the according to the form below regulated procedure is carried out gradient elution:
| Time (min) | A(%) | B(%) |
| 0 | 95 | 5 |
| 0.5 | 95 | 5 |
| 20 | 81.5 | 18.5 |
| 28 | 0 | 100 |
| 30 | 0 | 100 |
| 30.1 | 95 | 5 |
| 32 | 95 | 5 |
Herba Polygoni Capitati extract according to second aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: the chromatographic peak that (a) between retention time 1-3min, shows hydrolysable tannin (for example digalloylglucose).
Herba Polygoni Capitati extract according to second aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (b) for example, for example, for example, at the chromatographic peak of (about 5.3min place) demonstration hydrolysable tannin (trigalloylglucose) between (about 3.9min place) and retention time 4.8-5.8min between retention time 3.4-4.4min.
Herba Polygoni Capitati extract according to second aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (c) between retention time 3.4-4.4min (for example about 3.9min place), for example, between retention time 4.8-5.8min (about 5.3min place), for example, between retention time 8.2-9.2min (about 8.7min place), between retention time 12.0-13.0min, (for example about 12.5min place) shows the chromatographic peak of hydrolysable tannin, and/or for example, between retention time 6.2-7.2min (about 6.7min place), for example, between retention time 8.1-9.1min (about 8.6min place), between retention time 8.6-9.6min, (for example about 9.1min place) shows the chromatographic peak of procyanidin.
Herba Polygoni Capitati extract according to second aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result: (d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min.
According to the Herba Polygoni Capitati extract of second aspect present invention, it is measured according to described Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result:
(a) show the chromatographic peak of hydrolysable tannin (for example digalloylglucose) between retention time 1-3min;
(b) between retention time 3.4-4.4min for example, between (about 3.9min place) and retention time 4.8-5.8min (for example about 5.3min place) show the chromatographic peak of hydrolysable tannin (for example trigalloylglucose);
(c) between retention time 3.4-4.4min for example, between (about 3.9min place), retention time 4.8-5.8min for example, between (about 5.3min place), retention time 8.2-9.2min for example, between (about 8.7min place), retention time 12.0-13.0min (for example about 12.5min place) show the chromatographic peak of hydrolysable tannin, and/or for example, for example, for example, at the chromatographic peak of (about 9.1min place) demonstration procyanidin between (about 8.6min place), retention time 8.6-9.6min between (about 6.7min place), retention time 8.1-9.1min between retention time 6.2-7.2min; And/or
(d) chromatographic peak of (for example about 12.5min place) demonstration hydrolysable tannin (for example davidiin) between retention time 12.0-13.0min.
According to the Herba Polygoni Capitati extract of second aspect present invention, it is prepared by the method comprised the following steps basically:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 5-15 and doubly measure that (for example 5-12 doubly measures, for example 6-10 doubly measures) 50 ~ 90% (for example 60 ~ 80%, for example 65 ~ 75%, for example approximately 70%) alcohol reflux 1-3 time (for example 2 times), each 1-3 hour (for example approximately 1.5 hours), filter, make filtrate concentrated, dry, obtain pure extractum;
(2) pure extractum is suspended in methanol, supersound process 0.5 ~ 5 hour (for example 0.5 ~ 3 hour, for example 1 ~ 2 hour, for example approximately 1.5 hours), centrifugal, supernatant (for example is loaded into to the MCI macroporous resin column, it is the 0.5-4 liter that every 100g extractum is used the amount of resin, 1-3 liter for example, 1.5-2.5 liter for example, for example 2 liters) on;
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out successively gradient elution (for example every kind of solvent load is 0.5 ~ 5 times of column volume, 0.5 ~ 2.5 times of column volume for example, 0.5 ~ 2 times of column volume for example, 1 times of column volume for example), collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtain the methanol-eluted fractions thing of any concentration interval between 30%-50% or concentration point, perhaps their mixture, obtain.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 30% methanol-eluted fractions thing (in the present invention can referred to as: position A).
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 35%-40% methanol-eluted fractions thing (in the present invention can referred to as: position B).
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40% methanol-eluted fractions thing (in the present invention can referred to as: position C).
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40%-50% methanol-eluted fractions thing (in the present invention can referred to as: position D).
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein step (3) gained methanol-eluted fractions thing be methanol-eluted fractions thing between 30%-50% mixture (in the present invention can referred to as: position X).In the present invention, this position X can be the mixture of position A to position D dry product, can also be that 30%-50% methanol-eluted fractions gained mixed liquor is through desolventizing dried dry product.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein in the A of position, contain for example digalloylglucose of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein in the B of position, contain for example trigalloylglucose of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein in the C of position, contain hydrolysable tannin and/or procyanidin.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein in the D of position, contain for example hydrolysable tannin davidiin of hydrolysable tannin.
According to the Herba Polygoni Capitati extract of second aspect present invention, wherein in the X of position, contain hydrolysable tannin and/or procyanidin, for example digalloylglucose, trigalloylglucose, procyanidin and/or hydrolysable tannin davidiin.
According to the Herba Polygoni Capitati extract of second aspect present invention, it has the described feature of the arbitrary embodiment of first aspect present invention.
Third aspect present invention provides the method for preparing first aspect present invention or the described Herba Polygoni Capitati extract of the arbitrary embodiment of second aspect, and it consists essentially of following steps:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 5-15 and doubly measure that (for example 5-12 doubly measures, for example 6-10 doubly measures) 50 ~ 90% (for example 60 ~ 80%, for example 65 ~ 75%, for example approximately 70%) alcohol reflux 1-3 time (for example 2 times), each 1-3 hour (for example approximately 1.5 hours), filter, make filtrate concentrated, dry, obtain pure extractum;
(2) pure extractum is suspended in methanol, supersound process 0.5 ~ 5 hour (for example 0.5 ~ 3 hour, for example 1 ~ 2 hour, for example approximately 1.5 hours), centrifugal, supernatant (for example is loaded into to the MCI macroporous resin column, it is the 0.5-4 liter that every 100g extractum is used the amount of resin, 1-3 liter for example, 1.5-2.5 liter for example, for example 2 liters) on;
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out successively gradient elution (for example every kind of solvent load is 0.5 ~ 5 times of column volume, 0.5 ~ 2.5 times of column volume for example, 0.5 ~ 2 times of column volume for example, 1 times of column volume for example), collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtain the methanol-eluted fractions thing of any concentration interval between 30%-50% or concentration point, perhaps their mixture, obtain.
According to the method for third aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 30% methanol-eluted fractions thing (in the present invention can referred to as: position A).
According to the method for third aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 35%-40% methanol-eluted fractions thing (in the present invention can referred to as: position B).
According to the method for third aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40% methanol-eluted fractions thing (in the present invention can referred to as: position C).
According to the method for third aspect present invention, wherein step (3) gained methanol-eluted fractions thing be 40%-50% methanol-eluted fractions thing (in the present invention can referred to as: position D).
According to the method for third aspect present invention, wherein step (3) gained methanol-eluted fractions thing be methanol-eluted fractions thing between 30%-50% mixture (in the present invention can referred to as: position X).In the present invention, this position X can be the mixture of position A to position D dry product, can also be that 30%-50% methanol-eluted fractions gained mixed liquor is through desolventizing dried dry product.
According to the method for third aspect present invention, wherein in the A of position, contain for example digalloylglucose of hydrolysable tannin.
According to the method for third aspect present invention, wherein in the B of position, contain for example trigalloylglucose of hydrolysable tannin.
According to the method for third aspect present invention, wherein in the C of position, contain hydrolysable tannin and/or procyanidin.
According to the method for third aspect present invention, wherein in the D of position, contain for example hydrolysable tannin davidiin of hydrolysable tannin.
According to the method for third aspect present invention, wherein in the X of position, contain hydrolysable tannin and/or procyanidin, for example digalloylglucose, trigalloylglucose, procyanidin and/or hydrolysable tannin davidiin.
According to the method for third aspect present invention, wherein the gained Herba Polygoni Capitati extract has first aspect present invention or the described feature of the arbitrary embodiment of second aspect.
Fourth aspect present invention provides first aspect present invention or the described Herba Polygoni Capitati extract of second aspect preparing the clearing away heat-damp and promoting diuresis medication, the inducing diuresis for treating stranguria syndrome medication, urinary system infection or calculus medication, the pyelonephritis medication, removing toxic substances, dissipating blood stasis medication, antibiotic, antiinflammatory, analgesia medication, the purposes in the medicine of prostatitis medication.
Fifth aspect present invention provides a kind of pharmaceutical composition, wherein comprises the described Herba Polygoni Capitati extract of the arbitrary embodiment of first aspect present invention or second aspect and optional pharmaceutically acceptable carrier.
According to the pharmaceutical composition of fifth aspect present invention, it is the dosage form of oral or drug administration by injection.In one embodiment, described pharmaceutical composition is the form of tablet, capsule, granule, pill, oral solutions, injection (liquid drugs injection and/or powder pin) etc.
Arbitrary embodiment of applicable equally other the arbitrary embodiment of arbitrary technical characterictic that arbitrary embodiment of either side of the present invention or this either side has or other either side, as long as they can be not conflicting, certainly, at where applicable each other, necessary words can be done suitably to modify to individual features.Below with characteristics, be further described to various aspects of the present invention.
All documents that the present invention quotes from, their full content is incorporated to this paper by reference, and if, when the expressed implication of these documents and the present invention are inconsistent, be as the criterion with statement of the present invention.In addition, various terms and phrase that the present invention uses have the general sense of well known to a person skilled in the art, nonetheless, the present invention still wishes at this, these terms and phrase to be described in more detail and to explain, the term of mentioning and phrase, if any inconsistent with known implication, are as the criterion with the implication that the present invention was explained.
In the present invention, the inventive method obtains " Herba Polygoni Capitati extract ", and this term also can be described as " Herba Polygoni Capitati active component " of the present invention or " Herba Polygoni Capitati effective site " of the present invention.
In the present invention, the MCI macroporous resin can be the MCIGEL series of being produced by MIT, MCI GEL series reverse phase separation filler designs on the Diaion of Mitsubishi Chemical and Sepabeads macroporous adsorbent resin basis, because the HPLC high pressure liquid chromatography isolation technics based on modern, less granule has higher chromatographic separation performance, is widely used for separating of natural product and tunning.The MCI macroporous resin has two kinds of fillers: polystyrene and acrylic type, and the resin particle of polystyrene type is 4 μ m-100 μ m through scope, the grain of methacrylate type resin is 4 μ m-31 μ m through scope.MCI series not only has the resin of macroporous type in addition, also has anionic and the model resin such as cationic.The anti-phase fine separation filler of MCI GEL is a kind of resinae filler, can be used for separating saponin component, generally with methanol-water or ethanol water elution.Moreover the chlorophyll that generally is used in the little composition of place to go polarity of MCI, fine to petroleum ether part and the chlorophyllous effect in chloroform part place to go.In the present invention, the MCI macroporous resin preferably used is polystyrene type, and it includes but not limited to MCI GEL CHP 10M, MCI GEL CHP 5C, MCI GEL CHP55A, MCI GEL CHP 55Y, MCI GEL CHP 20Y, MCI GEL CHP 20P, MCI GEL CHP 20SS.In addition, in the present invention, if not otherwise specified, preferably using model is MCI GEL CHP 20P(75 ~ 150 μ m) macroporous resin, it is the most widely used model.It is a kind of porous polystyrene high polymer, its shown anti-phase adsorption is extensive, except the sugar to high polarity, aminoacid do not have adsorption substantially, most of secondary metabolites are had to absorption in various degree, this makes it can effectively remove on the one hand water solublity is disturbed to sugar greatly, aminoacid, can separate dissimilar compound again on the other hand.
The object of the invention is to overcome the deficiencies in the prior art, and a kind of Herba Polygoni Capitati effective content of anti inflammation (effective site) and application of high-efficiency low-toxicity is provided.
To Herba Polygoni Capitati, drug action is focused in the present invention, understand fully that its effect characteristics are screened the drug action of Herba Polygoni Capitati the different extracted parts simultaneously, adopt the sample of Herba Polygoni Capitati the different extracted parts to carry out the screening of Herba Polygoni Capitati active component (effective site) with the drug action characteristics by antiinflammatory, analgesia, antibiotic pharmacological evaluation.
In one embodiment, invention is achieved through the following technical solutions above-mentioned purpose:
The invention provides a kind of Herba Polygoni Capitati active component (effective site), is to be obtained by following steps:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 65 ~ 75% alcohol reflux 2 times that 6-8 doubly measures, each approximately 1.5 little), filter, make filtrate concentrated, dry, obtain pure extractum;
(2) pure extractum is suspended in methanol, supersound process approximately 1.5 hours), centrifugal, supernatant is loaded on MCI macroporous resin (MCI GEL CHP 20P) post (every 100g extractum is used the amount of resin to be approximately 2 liters);
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution (for example every kind of solvent load be approximately 1 times of column volume) successively, collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtain the methanol-eluted fractions thing of any concentration interval between 30%-50% or concentration point, or their mixture, obtain.
Above step (3) gained methanol-eluted fractions thing can be 30% methanol-eluted fractions thing (position A); Above step (3) gained methanol-eluted fractions thing can be 35%-40% methanol-eluted fractions thing (position B); Above step (3) gained methanol-eluted fractions thing can be 40% methanol-eluted fractions thing (position C); Above step (3) gained methanol-eluted fractions thing can be 40%-50% methanol-eluted fractions thing (position D); Above step (3) gained methanol-eluted fractions thing can be the mixture (position X) of methanol-eluted fractions thing between 30%-50%.In the present invention, this position X can be the mixture of position A to position D dry product, can also be that 30%-50% methanol-eluted fractions gained mixed liquor is through desolventizing dried dry product.
Contain for example digalloylglucose of hydrolysable tannin in above step (3) gained position A; Contain for example trigalloylglucose of hydrolysable tannin in above step (3) gained position B; Contain hydrolysable tannin and/or procyanidin in above step (3) gained position C; Contain for example hydrolysable tannin davidiin of hydrolysable tannin in above step (3) gained position D; Contain hydrolysable tannin and/or procyanidin in above step (3) gained position X, for example digalloylglucose, trigalloylglucose, procyanidin and/or hydrolysable tannin davidiin.
Herba Polygoni Capitati active component provided by the present invention (effective site), xylol causes the impact experiment of mice ear, press 5g Herba Polygoni Capitati dry product extract obtained/kg body weight gastric infusion, continuous 5 days, after last administration 60min, test, significant antiinflammatory action is arranged, and the highest inflammation suppression ratio can reach 49% (effective site X); For the experiment of mice hot plate induced pain, can extend the mice hot plate and add foot reaction latent time (with matched group, comparing P<0.05), the highest time delay rate can reach 18.4% (effective site X).
The effective site that the inventive method obtains can make antiinflammatory action than the obvious enhancing of water extract.The extract of extract of the present invention and extraction process by water relatively, can improve its antiphlogistic effects very significantly, and its experimental result is as shown in the table:
| Group | Dosage (g/kg) | n | Inhibitory rate of intumesce (%) |
| Matched group | - | 10 | |
| The Herba Polygoni Capitati water extract | 5 | 10 | 29.4 |
| Effective site A | 2.5 | 10 | 39.9 |
| Effective site B | 2.5 | 10 | 41.4 |
| Effective site C | 2.5 | 10 | 36.8 |
| Effective site D | 2.5 | 10 | 43.8 |
| Effective site X | 2.5 | 10 | 35.4 |
In upper table, " Herba Polygoni Capitati water extract " preparation method is: the Herba Polygoni Capitati dry product is divided into to secondary with 10 times of water (W/W) and decocts, each 1.5 hours, filter, merging filtrate, when filtrate is concentrated into to 20 ℃, relative density is 1.1, the concentrated solution spray drying obtains the above fine powder of 100 order.This Herba Polygoni Capitati water extract is also for hereinafter test example reagent in contrast.
In upper table, each effective site preparation method is: (1) adds Herba Polygoni Capitati aerial parts fresh goods or dry product 70% alcohol reflux 2 times of 7 times of amounts, and each approximately 1.5 hours, filter, make filtrate concentrated, dry, obtain pure extractum; (2) pure extractum is suspended in methanol, supersound process approximately 1.5 hours, centrifugal, supernatant is loaded on MCI macroporous resin (MCI GEL CHP20P) post (every 100g extractum is used the amount of resin to be approximately 2 liters); (3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution (every kind solvent load be approximately 1 times of column volume) successively, collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtaining 30% methanol-eluted fractions thing is position A, 35%-40% methanol-eluted fractions thing is position B, 40% methanol-eluted fractions thing is position C, and 40%-50% methanol-eluted fractions thing is position D, and 30%-50% methanol-eluted fractions thing is position X.
In the present invention, while with g/kg, meaning the dosage of test, unless otherwise noted, refer to that every kg the weight of animals gives the corresponding reagent weight that (for example extract of the present invention) amounts to into the Herba Polygoni Capitati dry product.
Herba Polygoni Capitati active component of the present invention can be prepared into various common dosage forms and slow releasing agent, controlled release agent, targeting preparation etc. with acceptable auxiliary material combination in the medicine manufacture.
The accompanying drawing explanation
Fig. 1, Fig. 2, Fig. 3 and Fig. 4 are respectively the liquid chromatograms of position A, position B, position C and position D.In Fig. 1, digalloylglucose means digalloylglucose, and isomer means isomer.
The specific embodiment
In order more clearly to understand technology contents of the present invention, especially exemplified by following examples, describe in detail, but embodiments of the present invention are not limited to this.
a, extract preparation example part
preparation example 1: Herba Polygoni Capitati active component
(1) by Herba Polygoni Capitati aerial parts dry product 10Kg, add 70% alcohol reflux 2 times of 7 times of amounts, each approximately 1.5 hours, filter, make filtrate concentrated, dry, obtain pure extractum (885g), (2) pure extractum (45g) is suspended in methanol, supersound process approximately 1.5 hours, centrifugal, supernatant is loaded on MCI macroporous resin (MCI GEL CHP 20P) post (every 100g extractum is used the amount of resin to be approximately 2 liters), (3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution (every kind solvent load be approximately 1 times of column volume) successively, collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtaining 30% methanol-eluted fractions thing is position A (yield 2.1%), 35%-40% methanol-eluted fractions thing is position B (yield 3.47%), 40% methanol-eluted fractions thing is position C (yield 1.47%), 40%-50% methanol-eluted fractions thing is position D (yield 7.16%), 30%-50% methanol-eluted fractions thing is position X (yield 14.2%).
Hereinafter, unless otherwise noted, position A used, B, C, D, X sample are the products by this preparation example 1.
preparation example 2: Herba Polygoni Capitati active component
(1) by Herba Polygoni Capitati aerial parts dry product 10Kg, add 60% alcohol reflux 3 times of 6 times of amounts, each approximately 1 hour, filter, make filtrate concentrated, dry, obtain pure extractum (935g); (2) pure extractum (45g) is suspended in methanol, supersound process approximately 2 hours, centrifugal, supernatant is loaded on MCI macroporous resin (MCI GEL CHP 20Y) post (every 100g extractum is used the amount of resin to be approximately 3 liters); (3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution (every kind solvent load be approximately 2 times of column volumes) successively, collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtaining 30% methanol-eluted fractions thing is position A, 35%-40% methanol-eluted fractions thing is position B, 40% methanol-eluted fractions thing is position C, and 40%-50% methanol-eluted fractions thing is position D, and 30%-50% methanol-eluted fractions thing is position X.The yield at each position is basic identical with preparation example 1.
preparation example 3: Herba Polygoni Capitati active component
(1) by Herba Polygoni Capitati aerial parts dry product 10Kg, add 80% alcohol reflux 1 time 3 hours of 10 times of amounts, filter, make filtrate concentrated, dry, obtain pure extractum (818g); (2) pure extractum (45g) is suspended in methanol, supersound process approximately 1 hour, centrifugal, supernatant is loaded on MCI macroporous resin (MCI GEL CHP 55A) post (every 100g extractum is used the amount of resin to be approximately 1 liter); (3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution (every kind solvent load be approximately 0.5 times of column volume) successively, collect the each several part eluent, reclaim solvent, the position drying obtained by the different solvents eluting, obtaining 30% methanol-eluted fractions thing is position A, 35%-40% methanol-eluted fractions thing is position B, 40% methanol-eluted fractions thing is position C, and 40%-50% methanol-eluted fractions thing is position D, and 30%-50% methanol-eluted fractions thing is position X.The yield at each position is basic identical with preparation example 1.
b, pharmacodynamics test example part
test example 1: the experiment of mice caused by dimethylbenzene xylene ear swelling, the antiphlogistic effects of investigation Herba Polygoni Capitati extract
Animal: SPF level Kunming mouse, body weight 18～22g, male and female dual-purpose.
Reagent, dosage and medication: with above various effective site and the control sample Herba Polygoni Capitati water extract (seeing above) of " preparation example 1: Herba Polygoni Capitati active component " gained, dosage is that to give the weight that corresponding reagent amounts to into the Herba Polygoni Capitati dry product be 5g to every kg the weight of animals.Each reagent is suspended to normal saline the concentration that is equivalent to every each gastric infusion 0.4ml of animal before use, and the matched group of gavage with the volume normal saline is set simultaneously.
Test method: mice male and female dual-purpose, random packet, 10 animals of each reagent group; Successive administration 5 days, after last administration 60min, only be coated with auris dextra with dimethylbenzene 0.1ml/ and cause inflammation, puts to death mice after 30min, with the card punch of diameter 6mm, gets left and right two auricles.Use immediately scales/electronic balance weighing, using two auricle weight differences as swelling (mg), calculate the suppression ratio (%) of each reagent group with following formula:
Swelling (mg)=auris dextra sheet weight-left auricle weight wherein
Result is carried out statistical analysis.Experimental result is in Table 1.
Suppression ratio is carried out to classification, and suppression ratio is the A level lower than 10%, and suppression ratio 10 ~ 20% is the AA level, and suppression ratio 20 ~ 30% is the AAA level, and suppression ratio 30 ~ 40% is the AAAA level, and suppression ratio 40 ~ 50% is the AAAAA level, and suppression ratio is greater than 50% for the AAAAAA level.
Table 1: different Herba Polygoni Capitati sample xylol causes the impact of mice ear
| Reagent | The suppression ratio classification |
| Position A | AAA+* |
| Position B | AAAA** |
| Position C | AAAAA** |
| Position D | AAAA** |
| Position X | AAAAA** |
| The Herba Polygoni Capitati water extract | AAAA** |
Annotate: swelling (mg), compare with the solvent control animals: * P<0.05, * * P<0.01.Each position of in parallel test, using preparation example 2 and preparation example 3 is as reagent, and result is identical with table 1.
test example 2: the heat-resisting hot plate reaction experiment of mice, the analgesic effect of investigation Herba Polygoni Capitati extract
Animal, reagent, dosage and medication are identical with test example 1.
Test method: mice male and female dual-purpose, random packet, 10 animals of each reagent group; Successive administration 5 days, after last administration 60min, put into intelligent hot-plate instrument by each group mice, and the observed and recorded mice is added foot reaction latent time, and each is organized mice measurement 2 times (the about 15min of every minor tick) and gets its meansigma methods.Experimental result is in Table 2.
Carry out classification to adding foot reaction latent time, latent time was the A level lower than 6 seconds, and latent time 6 ~ 7 seconds is the AA level, and latent time 7 ~ 8 seconds is the AAA level, and latent time 8 ~ 9 seconds is the AAAA level, and it is the AAAAA level that latent time is greater than 9 seconds.
Table 2: the impact of different Herba Polygoni Capitati reagents on the heat-resisting hot plate reaction of mice
| Reagent | Add the classification of foot reaction latent time |
| Position A | AAA |
| Position B | AAAA** |
| Position C | AAA* |
| Position D | AAAA** |
| Position X | AAAA** |
| The Herba Polygoni Capitati water extract | AAAA** |
Annotate: add foot reaction latent time (second), compare with the solvent control animals: * P<0.05**P<0.01.Each position of in parallel test, using preparation example 2 and preparation example 3 is as reagent, and result is identical with table 2.
test example 3: the antibacterial experiment of different Herba Polygoni Capitati extract
Adopt conventional antibacterial test, use the MH broth bouillon to be tested bacillus pyocyaneus, escherichia coli M421C1ST, dysentery bacterium, staphylococcus aureus, Hemolytic streptococcus, using each sample of " preparation example 1 " gained above and Herba Polygoni Capitati water extract as reagent, test their sensitivity to these cells.
Result shows, position A, position B, position C, position D, each sample of position X are to the MIC of five kinds of antibacterials between 1-5mg/ml, and the MIC of Herba Polygoni Capitati water extract is between 10-25mg/ml.
c, chemical analysis example part
Use UPLC-TOF-MS method test preparation example 1 gained alcohol extract and each position.
The assay method of UPLC-TOF-MS is as follows:
(i) test liquid preparation: take appropriate Herba Polygoni Capitati extract powder, add 70% methanol to make the suspension of the about 5mg/ml of concentration, ultrasonic making dissolved as far as possible, and 10 times of suspension dilutions, filter, and sample introduction 2 μ l make Mass Spectrometer Method;
(ii) chromatograph and mass spectral analysis condition:
Chromatographic column: Acquity BEH C18 post (2.1 * 100mm, 1.7 μ m), column temperature: 40 ℃; Flow velocity: 0.35ml/min; Sample size: 2 μ l; Mass spectrum condition: ion source: ESI source; Dry gas temperature: 180 ℃; Capillary voltage: 4500eV; Detecting pattern: negative ion mode; Atomisation pressure: 2.5bar; Dry gas (N2) flow velocity: 8L/min; Sweep limits: 100-2000amu; Collision energy: 10ev; Take 0.1% aqueous formic acid as mobile phase A, and 0.1% formic acid acetonitrile solution is Mobile phase B, and the according to the form below regulated procedure is carried out gradient elution:
| Time (min) | A(%) | B(%) |
| 0 | 95 | 5 |
| 0.5 | 95 | 5 |
| 20 | 81.5 | 18.5 |
| 28 | 0 | 100 |
| 30 | 0 | 100 |
| 30.1 | 95 | 5 |
| 32 | 95 | 5 |
Result:
(a) A sample in position shows, shows the chromatographic peak of hydrolysable tannin (for example digalloylglucose) between retention time 1-3min, referring to Fig. 1;
(b) B sample in position shows, for example, at the chromatographic peak of retention time about 3.9min place and the about 5.3min of retention time place demonstration hydrolysable tannin (trigalloylglucose), referring to Fig. 2;
(c) C sample in position shows, at the about 3.9min of retention time place, the about 5.3min of retention time place, the about 8.7min of retention time place, the about 12.5min of retention time place show the chromatographic peak of hydrolysable tannin, at the about 6.7min of retention time place, the about 8.6min of retention time place, the about 9.1min of retention time place show the chromatographic peak of procyanidin, referring to Fig. 3;
(d) D sample in position shows, shows the chromatographic peak of hydrolysable tannin (for example davidiin) at the about 12.5min of retention time place, referring to Fig. 4.
Each effective site of Herba Polygoni Capitati provided by the invention, the position material and the characterization data thereof that wherein comprised see the following form:
Wherein peak 15 is Davidiin, and its chemical constitution is as follows:
。
Claims (13)
1. a Herba Polygoni Capitati extract, its method by following steps prepares:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 60～80% alcohol reflux 1-3 time that 6-10 doubly measures, each 1-3 hour, filter, and makes filtrate concentrated, dry, obtains pure extractum;
(2) pure extractum is suspended in methanol, supersound process 1～2 hour, centrifugal, supernatant is loaded on the MCI macroporous resin column;
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution successively, collects the 30%-50% meoh eluate, reclaims solvent, and drying, obtain.
2. according to the Herba Polygoni Capitati extract of claim 1, wherein, in step (2), it is the 1-3 liter that every 100g extractum is used the amount of resin.
3. according to the Herba Polygoni Capitati extract of claim 1, while wherein in step (3), carrying out eluting, every kind of solvent load is 0.5～2 times of column volume.
4. according to the Herba Polygoni Capitati extract of claim 1, wherein said MCI macroporous resin is the MCI macroporous resin that is selected from following model: MCI GEL CHP20P, MCI GEL CHP20Y, MCI GEL CHP55A.
5. according to the Herba Polygoni Capitati extract of claim 1, wherein contain hydrolysable tannin and procyanidin.
6. according to the Herba Polygoni Capitati extract of claim 1, wherein contain digalloylglucose, trigalloylglucose, procyanidin and davidiin.
7. according to the Herba Polygoni Capitati extract of claim 1, it is measured according to Ultra Performance Liquid Chromatography-time of flight mass spectrometry coupling method, result:
Showing the chromatographic peak of hydrolysable tannin between retention time 3.4-4.4min, between retention time 4.8-5.8min, between retention time 8.2-9.2min, between retention time 12.0-13.0min;
Showing the chromatographic peak of procyanidin between retention time 6.2-7.2min, between retention time 8.1-9.1min, between retention time 8.6-9.6min;
Show the chromatographic peak of hydrolysable tannin davidiin between retention time 12.0-13.0min;
Wherein, the assay method of UPLC-TOF-MS is as follows:
(i) test liquid preparation: take appropriate Herba Polygoni Capitati extract powder, add 70% methanol to make the suspension of concentration 5mg/ml, ultrasonic making dissolved as far as possible, and 10 times of suspension dilutions, filter, and sample introduction 2 μ l make Mass Spectrometer Method;
(ii) chromatograph and mass spectral analysis condition:
Chromatographic column: Acquity BEH C18 post, column temperature: 40 ℃; Flow velocity: 0.35ml/min; Sample size: 2 μ l; Mass spectrum condition: ion source: ESI source; Dry gas temperature: 180 ℃; Capillary voltage: 4500eV; Detecting pattern: negative ion mode; Atomisation pressure: 2.5bar; Drying nitrogen flow velocity: 8L/min; Sweep limits: 100-2000amu; Collision energy: 10ev; Take 0.1% aqueous formic acid as mobile phase A, and 0.1% formic acid acetonitrile solution is Mobile phase B, and the according to the form below regulated procedure is carried out gradient elution:
。
8. according to the Herba Polygoni Capitati extract of claim 7, the specification of wherein said Acquity BEH C18 post is: 2.1 * 100mm, 1.7 μ m.
9. prepare the method for the described Herba Polygoni Capitati extract of claim 1-8 any one, it is comprised of following steps:
(1) Herba Polygoni Capitati aerial parts fresh goods or dry product are added to 60～80% alcohol reflux 1-3 time that 6-10 doubly measures, each 1-3 hour, filter, and makes filtrate concentrated, dry, obtains pure extractum;
(2) pure extractum is suspended in methanol, supersound process 1～2 hour, centrifugal, supernatant is loaded on the MCI macroporous resin column;
(3) water, 10%, 20%, 30%, 35%, 40%, 45%, 50%, 60%, 70%, 80%, 100% methanol carries out gradient elution successively, collects the 30%-50% meoh eluate, reclaims solvent, and drying, obtain.
10. according to the method for claim 9, wherein, in step (2), it is the 1-3 liter that every 100g extractum is used the amount of resin.
11., according to the method for claim 9, while wherein in step (3), carrying out eluting, every kind of solvent load is 0.5～2 times of column volume.
12. the described Herba Polygoni Capitati extract of claim 1-8 any one is preparing the clearing away heat-damp and promoting diuresis medication, inducing diuresis for treating stranguria syndrome medication, urinary system infection or calculus medication, the pyelonephritis medication, removing toxic substances, dissipating blood stasis medication, antibiotic, antiinflammatory, analgesia medication, the purposes in the medicine of prostatitis medication.
13. a pharmaceutical composition, wherein consist of the described Herba Polygoni Capitati extract of claim 1-8 any one, and optional pharmaceutically acceptable carrier.
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| GB201506526D0 (en) | 2015-04-17 | 2015-06-03 | Uropharma Ltd And Synesis Llc | Medicinal composition |
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| CN106265699B (en) * | 2016-08-12 | 2019-02-15 | 孙连娜 | Three galla turcica acidic group of the β -1,6- hexahydroxy biphenyl diformyl -2,3,4--application of D-Glucose compound in medicine preparation |
| CN107625790A (en) * | 2017-09-30 | 2018-01-26 | 韩博 | Nutgall prevents and treats periodontal disease and the production method of IBD active component and application thereof |
| CN108226306B (en) * | 2017-12-27 | 2021-01-01 | 贵州威门药业股份有限公司 | Method for measuring fingerprint of ethanol extracts of polygonum capitatum with different concentrations |
| CN107870216B (en) * | 2017-12-27 | 2020-07-28 | 贵州威门药业股份有限公司 | Spectral efficiency analysis method for bacteriostasis of polygonum capitatum parts with different polarities |
| CN111198240B (en) * | 2020-01-09 | 2022-09-09 | 中国农业科学院茶叶研究所 | Method for extracting 1, 2, 6 tri-galloyl glucose from tea |
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