CN1257969C - Polygonum capilalum extract , iIts preparation method and use - Google Patents
Polygonum capilalum extract , iIts preparation method and use Download PDFInfo
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- CN1257969C CN1257969C CN 02129686 CN02129686A CN1257969C CN 1257969 C CN1257969 C CN 1257969C CN 02129686 CN02129686 CN 02129686 CN 02129686 A CN02129686 A CN 02129686A CN 1257969 C CN1257969 C CN 1257969C
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- herba polygoni
- polygoni capitati
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- Medicines Containing Plant Substances (AREA)
Abstract
The present invention relates to an extract of fresh or dry polygonum capitapum, a preparation method and functions thereof. The present invention also relates to a medicinal composition which contains the extract of polygonum capitapum. In the present invention, whole polygonum capitapum herb, overground parts thereof, leaves thereof, seeds thereof, stems thereof and roots thereof are respectively extracted in water, 75% alcohol, 95% alcohol and carbon dioxide by a supercritical extraction method, and activity study is also carried out. The extract of polygonum capitapum prepared by means of the process provided in the present invention has obvious effects on anti-bacterium, anti-inflammation, analgesia, urination promotion, treatment of pyelonephritis and prostatitis, calculus expelling, etc.
Description
The present invention relates to the field of Chinese medicines, particularly, the present invention relates to the extract and preparation method thereof of bright product of herbal medicine Herba Polygoni Capitati or dry product and this extract purposes as medicine.
Herba Polygoni Capitati (Polygonum capitatum Buch.-Ham.ex D.Don) is the polygonaceae arsesmart, is perennial herb, another name Herba Polygoni Capitati, Herba Polygoni Capitati, Polygonum capitatum Buch, water silk ball, safflower Chinese violet, completely red etc.In areas such as Chinese Guizhou, Yunnan, Guangxi, Sichuan, Tibet, Hubei, Hunan and Jiangxi distribution is arranged all, mainly be grown in hillside, mountain valley and be rich in the husky shale area in coal seam.The effect of clearing heat and detoxicating, the diffusing stasis of blood that herb has, inducing diuresis for treating stranguria syndrome.According to 1963 " Guangxi Chinese medicinal herbal " second record, Herba Polygoni Capitati is mainly used in treatment rheumatalgia; " Chinese medicine voluminous dictionary " first volume record in 1977, Herba Polygoni Capitati is mainly used in treatment dysentery, ephritis, urocystitis and lithangiuria etc.Among the people generally with Herba Polygoni Capitati with being decocted in water for oral dose, result of treatment is apparent in view, but takes inconvenience.A kind of miganling instant herbal medicine, syrup production technique are disclosed among the Chinese patent application prospectus CN1054899A, this method is through decocting after-filtration with the herbal medicine Herba Polygoni Capitati, concentrating under reduced pressure becomes paste, use extraction using alcohol 2-3 time again, vacuum concentration is made medicinal extract, again medicinal extract is made syrup or electuary respectively.Steps such as this production technique comprises decoction, concentrates, extraction, reconcentration, complex process, and also the pharmacodynamics effect of the miganling instant herbal medicine that this method obtains has much room for improvement.Our GuiZhou WeiMen Pharmacy Co., Ltd is devoted for years to the development and use research in the herbal medicine Herba Polygoni Capitati, we concentrate twice after-filtration of Herba Polygoni Capitati boiling and make the clear particle of heat pouring, said preparation is disclosed in the Ministry of Health of the People's Republic of China " drug standard--Chinese traditional patent formulation preparation " (the 17) of committee of pharmacopeia of Ministry of Health of the People's Republic of China volume in 1998, but, along with deepening continuously of research, the inventor finds, heat in the Ministry of Health of the People's Republic of China " drug standard--Chinese traditional patent formulation preparation " (the 17) of compiling in 1998 is drenched among the clear particulate preparation technology, there is defective on its extraction and the process for purification, according to this technology, 1000 gram Herba Polygoni Capitati are decocted, can not obtain 400 gram extract granules.The inventor is by carrying out long-term development research to the herbal medicine Herba Polygoni Capitati, and in conjunction with pharmacology test checking discovery, extract and process for refining by improving, the pharmacologically active of the Herba Polygoni Capitati extract that obtains obviously improves, and find that this Herba Polygoni Capitati extract has new curative effect, therefore finished the present invention.
Therefore, the extract that the purpose of this invention is to provide bright product of a kind of Herba Polygoni Capitati or dry product;
Another goal of the invention of the present invention has provided a kind of method for preparing Herba Polygoni Capitati extract;
Another goal of the invention of the present invention has provided the purposes that Herba Polygoni Capitati extract is used to prepare antibiotic, anti-inflammatory, analgesia, diuresis, treatment urinary system calculus, treatment pyelonephritis and prostatitic medicine;
Another goal of the invention of the present invention has provided the pharmaceutical composition that contains extract of the present invention.
The objective of the invention is to realize by following method.
The inventor studies the different medicinal parts of bright product of Herba Polygoni Capitati or dry product respectively, Herba Polygoni Capitati herb, Herba Polygoni Capitati over-ground part, leaf, seed, stem and root and their combination extraction and activity research have been carried out respectively, the inventor finds, the biologic activity of the leaf of Herba Polygoni Capitati, seed, stem and root portion is differentiated, and anti-inflammatory activity is best with the leaf extract; The strong and weak order of anti-microbial activity is seed＞leaf＞stem＞root.The inventor takes a hint from this discovery, and the Herba Polygoni Capitati herb that uses with the over-ground part replacement tradition of Herba Polygoni Capitati extracts, and has so both kept and improved the pharmaceutical active of extraction medicinal extract, avoids using the root of Herba Polygoni Capitati again.Because Herba Polygoni Capitati is a herbaceous plant, does not use its root, can avoid when gathering Herba Polygoni Capitati, its root being pulled up, like this, Herba Polygoni Capitati can be regenerated, and has both protected plant resources, has protected the soil vegetation again, and this is all significant to resources conseravtion and environment.
Inventor's water, 75% ethanol and 95% ethanol and CO 2 supercritical condition have been carried out extraction and activity research respectively to Herba Polygoni Capitati herb, over-ground part, leaf, seed, stem and root respectively.
Herba Polygoni Capitati extract of the present invention obtains by following method:
Embodiment 1: preparation Herba Polygoni Capitati over-ground part water extract (numbering: w-2-1)
Get Herba Polygoni Capitati over-ground part 220kg, clean, add 7 times of water gagings, heated and boiled 1.5 hours is filtered, and adds 6 times of water gagings in the dregs of a decoction, boils 1.0 hours, filters.Merging filtrate, being concentrated into relative density is that 1.2 (20 ℃) obtain medicinal extract, and spraying drying obtains extract powder 23kg, and yield is 10.45%.
Adopt the general flavone content among the spectrophotometer method mensuration w-2-1, w-2-1 extract and auxiliary material that method of the present invention prepares is evenly mixed, granulate, drying, the heat that promptly obtains the novel method preparation is drenched clear particle.
Embodiment 2: preparation Herba Polygoni Capitati herb water extract (spraying drying) (numbering: w-1-2)
According to the method identical, replace the Herba Polygoni Capitati over-ground part to extract with the Herba Polygoni Capitati herb with embodiment 1.
Get the w-1-2 extract powder by the identical method of embodiment 1, make sample (w-1-12).
The present invention compares Herba Polygoni Capitati herb and Herba Polygoni Capitati over-ground part experimental data.(seeing Table 1)
Table 1: Herba Polygoni Capitati herb water extract and Herba Polygoni Capitati over-ground part water extract experimental data
| Title | Numbering | Charging capacity (kg) | Get extract powder amount (kg) | Yield (%) | Gallic acid content (%) | General flavone content (%) |
| Herba Polygoni Capitati herb Herba Polygoni Capitati over-ground part | W-1-2 w-2-1 | 300.95 220 | 34.5 23 | 11.46 10.45 | 1.78 3.99 | 1.82 4.71 |
Find out from above result, with the over-ground part be in the extract powder of raw material gallic acid and general flavone content content apparently higher than being the extract powder of raw material with the herb.
Embodiment 3: preparation Herba Polygoni Capitati herb water extract (drying under reduced pressure) (numbering: w-1-3)
Method according to identical with embodiment 2 changes drying means into drying under reduced pressure.
Embodiment 4: preparation Herba Polygoni Capitati root 95% ethanol extraction (numbering: w-1-4)
Get Herba Polygoni Capitati root 10kg, clean, put in the stainless steel concentration tank, add 95% ethanol of 7.5 times of amounts, refluxing extraction 1.5 hours is filtered.The dregs of a decoction add 7.5 times of amount 95% ethanol, and refluxing extraction 1.0 hours is filtered.Merge filtrate twice, concentrate medicinal extract, drying under reduced pressure obtains extract 0.215kg.
Embodiment 5: preparation Herba Polygoni Capitati stem 95% ethanol extraction (numbering: w-1-5)
According to the method identical, extract with the Herba Polygoni Capitati stem with embodiment 4.
Embodiment 6: preparation Herba Polygoni Capitati leaf 95% ethanol extraction (numbering: w-1-6)
According to the method identical, extract with the Herba Polygoni Capitati leaf with embodiment 4.
Embodiment 7: preparation Herba Polygoni Capitati seed 95% ethanol extraction (numbering: w-1-7)
According to the method identical, extract with the Herba Polygoni Capitati seed with embodiment 4.
Embodiment 8: bright product 95% ethanol of preparation Herba Polygoni Capitati is put forward powder (numbering: w-1-8)
According to the method identical, extract with the bright product of Herba Polygoni Capitati with embodiment 4.
Embodiment 9: the bright product water of preparation Herba Polygoni Capitati is put forward powder (numbering: w-1-9)
According to the method identical, extract with the bright product of Herba Polygoni Capitati with embodiment 3.
Embodiment 10: preparation Herba Polygoni Capitati herb 75% ethanol extraction (numbering: W-1-10)
Get Herba Polygoni Capitati herb 10kg, clean, put in the stainless steel concentration tank, add 7-8 and doubly measure 75% ethanol, refluxing extraction 1.5 hours is filtered.The dregs of a decoction add 5 times of amount 75% ethanol, and refluxing extraction 1.0 hours is filtered.Merge filtrate twice, concentrate medicinal extract, drying under reduced pressure obtains extract 0.694kg.
Embodiment 11: preparation Herba Polygoni Capitati herb water decoction-alcohol sedimentation solution powder (W-1-14a) and Herba Polygoni Capitati herb water decoction-alcohol sedimentation precipitated powder (W-1-14b)
Get Herba Polygoni Capitati herb 10.60kg, clean, add 350kg water, heated and boiled 1.5 hours shifts supernatant liquor, adds 150kg water in the residue, boils 1.0 hours.Merge decoction liquor, filtering and concentrating to relative density is that 1.04 (24 ℃) get medicinal extract 16.1kg.Add 95% ethanol and transfer to that to contain alcohol amount be 60%, quiet to 24 hours, divide and get solution.Add 95% ethanol to precipitation and transfer to that to contain the alcohol amount be 60%, quiet to 24 hours, divide and get solution, merge solution twice, fling to ethanol, 80 ℃ of drying under reduced pressure get Herba Polygoni Capitati herb water decoction-alcohol sedimentation solution powder (W-1-14a) 0.755kg; Be deposited in 80 ℃ of drying under reduced pressure and get Herba Polygoni Capitati herb water decoction-alcohol sedimentation precipitated powder (W-1-14b) 0.465kg.
Embodiment 12: the former medicinal powder carbon dioxide upercritical fluid extraction of preparation Herba Polygoni Capitati extract (numbering: W-1-15a)
Get the former medicinal powder 10kg of Herba Polygoni Capitati, clean, drop in the supercritical extraction reactor,, basin is cooled off, when temperature reaches predetermined temperature, open CO extraction kettle and two extraction-containers heating
2Gas cylinder is supplied gas, and when pressure reached predetermined pressure, the beginning cycling extraction was regulated flow, and added entrainment agent, constant temperature and pressure extraction 2 hours.The liquid concentrating under reduced pressure that obtains is obtained medicinal extract 0.135kg.
Embodiment 13: preparation Herba Polygoni Capitati dregs of a decoction carbon dioxide upercritical fluid extraction extract (numbering: W-1-15b)
Get Herba Polygoni Capitati dregs of a decoction 10kg, clean, drop in the supercritical extraction reactor,, basin is cooled off, when temperature reaches predetermined temperature, open CO extraction kettle and two extraction-containers heating
2Gas cylinder is supplied gas, and when pressure reached predetermined pressure, the beginning cycling extraction was regulated flow, and added entrainment agent, constant temperature and pressure extraction 2 hours.The liquid concentrating under reduced pressure that obtains is obtained medicinal extract 0.119kg.
Embodiment 14: preparation Herba Polygoni Capitati over-ground part 70% ethanol extraction (numbering: W-2-2)
Get Herba Polygoni Capitati over-ground part 30kg, clean, put in the stainless steel concentration tank, add 8-9 and doubly measure 70% ethanol, refluxing extraction 1.5 hours is filtered.The dregs of a decoction add 4-5 and doubly measure 70% ethanol, and refluxing extraction 1.0 hours is filtered.The dregs of a decoction add 4-5 again and doubly measure 70% ethanol, and refluxing extraction 1.0 hours is filtered.Merge three times filtrate, concentrate medicinal extract, drying under reduced pressure obtains extract 3.75kg.
Table 2: the experimental data of different sites, Different Extraction Method sample
| Numbering | Title | Charging capacity (kg) | Get extract powder amount (kg) | Yield (%) | Gallic acid content (%) | General flavone content (%) |
| W-1-2 W-1-3 W-1-4 W-1-5 W-1-6 W-1-7 W-1-8 W-1-9 W-1-10 W-1-12 W-1-14a W-1-14b W-1-15a W-1-15b W-2-1 | The 75% ethanol extract W-1-2 that polygonum capitatum herb water extract (spray-drying) polygonum capitatum herb water extract (drying under reduced pressure) root 95% ethanol extract stem 95% ethanol extract leaf 95% ethanol extract seed 95% ethanol extract fresh goods 95% ethanol is carried powder fresh goods water extraction powder polygonum capitatum herb adds the former medicinal powder carbon dioxide supercritical extraction of the particle polygonum capitatum herb water decoction-alcohol sedimentation solution powder polygonum capitatum herb water decoction-alcohol sedimentation precipitated powder polygonum capitatum extract polygonum capitatum dregs of a decoction carbon dioxide supercritical extraction extract polygonum capitatum aerial part water extract that auxiliary material is made | 300.95 300.95 10 10 9 1.8 22 21 10 / 10.60 10.60 10 10 220 | 34.5 32.8 0.215 0.125 0.7 0.03 0.550 0.855 0.694 / 0.755 0.465 0.135 0.119 23 | 11.46 10.90 2.15 1.25 7.78 1.70 2.50 4.07 6.94 / 7.12 4.39 1.35 1.19 10.45 | 1.78 2.55 1.48 1.89 0.70 0.72 2.87 2.76 1.48 0.73 3.06 0.8 3.99 | 1.82 1.46 2.25 1.94 6.29 5.55 3.78 1.92 3.17 1.59 2.00 0.64 4.71 |
| W-2-2 | 70% ethanol extraction of over-ground part | 30 | 3.75 | 12.5 | 5.88 | 4.57 |
Annotate: because sample W-1-15a and ten fens thickness of sample W-1-15b, pre-treatment is very difficult, does not therefore measure its gallic acid content and general flavone content.
It is consistent with the method for preparing Herba Polygoni Capitati herb water decoction-alcohol sedimentation solution powder (W-1-14a) herein to prepare the method for Herba Polygoni Capitati herb extract among the Chinese invention patent prospectus CN1054899A.And sample W-1-2 actual be herb water decoction-alcohol sedimentation solution powder (W-1-14a) and herb water decoction-alcohol sedimentation precipitated powder (W-1-14b) add and.Has good activity equally through pharmacodynamic experiment proof Herba Polygoni Capitati herb water decoction-alcohol sedimentation precipitated powder (W-1-14b); Sample W-1-2 then is active the strongest (seeing Table 5) in these three samples.The method operation for preparing the Herba Polygoni Capitati herb extract among the Chinese invention patent prospectus CN1054899A is loaded down with trivial details, because of the soup of handling through alcohol precipitation during preservation is easy to generate precipitation or wall sticking phenomenon; Often viscosity is bigger for soup after alcohol precipitation reclaims ethanol, difficult concentrating.The alcohol precipitation process for producing cycle is long, the cost height.And lose part activeconstituents (being the water decoction-alcohol sedimentation precipitation part W-1-14b that throws away in the CN1054899A method).
We are to Herba Polygoni Capitati herb, over-ground part, root, stem, leaf, flower, seed and over-ground part deflorate water extract, 95% ethanol extraction, the CO of (being stem and leaf) each several part
2Supercritical extract has all carried out pharmacology test, and we find wherein best with the curative effect of Herba Polygoni Capitati over-ground part.And be raw material with the Herba Polygoni Capitati over-ground part, made a series of preparations with the ordinary method in the pharmacy field: lotion, suppository, externally used solution agent, effervescent tablet, plaster, ointment, syrup, emulsion, powder, granule, pill, capsule, aerosol, injection and slowly-releasing, controlled release preparation and targeting preparation.
The inventor has carried out the pharmacodynamic study discovery with the said extracted thing, and Herba Polygoni Capitati extract of the present invention has pharmacological activities such as good antibiotic, anti-inflammatory, analgesia, diuresis, row's stone, treatment pyelonephritis and prostatitis.
Test one: anti-inflammatory activity research
Experimental technique:,, measure the anti-inflammatory activity of the extract that different medicinal parts and different extraction processes obtain according to mice ear biological activity determination method with mouse ear Oleum Tiglii inflammatory model.The mouse mainline administration is adopted in experiment, and dosage is 40mg/kg, under Isodose, compares the anti-inflammatory activity size of each extract sample.Come different medicinal parts with this, the curative effect of different extraction process samples is made judge.
The sample compound method: make solvent with 5% propylene glycol, behind sample weighing, add earlier 0.5ml propylene glycol supersound process, treat that sample powder is uniformly dispersed after, be diluted to scale (10ml) with physiological saline again.
Experimental result:
Carry out three batches of experiments altogether, carry out under all identical at the same time experiment condition (room temperature, humidity) of the every batch of experiment.
Experimental result sees Table 3
The comparison of the different Herba Polygoni Capitati sample of table 3 anti-inflammatory activity
| Numbering | Title | Dosage (mg/kg) | Include total flavones amount (mg) | Include gallic acid amount (mg) | Experiment (n=10) for the first time | Experiment (n=10) for the second time | Experiment (n=11) for the third time | |||
| Swelling degree (mg) | Swelling rate (%) | Swelling degree (mg) | Swelling rate (%) | Swelling degree (mg) | Swelling rate (%) | |||||
| W-1-2 W-1-3 W-1-4 W-1-5 W-1-6 positive control positive control positive control | Herb water extraction (spraying) herb water extraction (decompression) root 95% alcohol extracting stem 95% alcohol extracting leaf 95% alcohol extracting hydrocortisone rutin gallic acid | 40 40 40 40 40 20 20 20 | 0.728 0.584 0.901 0.776 2.517 - 20 - | 0.864 1.098 0.592 0.480 0.305 - - 20 | 13.1±5.0 *(30.7) 13.1±4.7 *(30.7) 13.6±4.7 *(28.0) 14.1±3.5 *(25.4) 13.0±2.6 *(31.2) 6.7±2.9 **(64.6) | 77.8±36.8 * 82.6±30.9 86.1±29.9 86.4±26.0 82.1±22.7 * 45.2±20.7 ** | 10.8±2.5 *(33.7) 11.5±2.5 **{29.4} 12.2±3.2 **{25.1} 13.9±2.3 *(14.7) 8.4±3.1 **(48.5) 4.9±2.8 **(69.9) 11.4±2.7 **(30.1) 15.9±3.4(2.4) | 72.2±22.5 ** 75.1±20.3 ** 80.6±19.3 ** 96.2±16.7 * 57.9±20.4 ** 36.4±16.4 ** 74.7±17.1 ** 107.0±19.5 | 11.5±3.4 *(33.1) 11.3±2.8 **(34.3) 14.4±3.1 *(16.3) 14.5±4.5(15.7) 9.8±2.8 **(43.0) 4.7±1.6 **(72.7) 11.4±2.9 **(33.3) 15.3±2.2(11.0) | 64.0±20.2 ** 64.0±17.0 ** 84.7±24.5 * 80.5±24.7 * 59.4±17.0 ** 29.7±12.1 * 65.4±21.3 ** 96.6±18.9 |
| Model group W-1-2 W-1-8 W-1-9 W-1-15b W-1-15a positive control model group | 5% propylene glycol herb water is carried the bright product water of bright product alcohol extracting and is carried CO 2Dregs of a decoction CO 2Medicinal material hydrocortisone 5% propylene glycol | 40 40 40 40 40 20 - | 0.728 1.510 0.770 | 0.864 1.313 1.276 | 18.9±5.3 12.6±3.4 ** 13.0±2.4 *(31.2) 7.4±2.6 **(60.8) 12.1±3.3 ** 17.9±2.9 5.0±2.4 ** 20.4±2.8 | 117.2±43.1 81.1±26.5 ** 86.2±26.3 45.8±18.0 ** 77.2±19.2 ** 108.8±29.4 34.8±18.0 124.8±21.1 | 16.3±2.5 7.3±2.5 ** 13.5±3.0 *(17.2) 9.5±3.7 **(41.7) 7.6±1.6 ** 10.4±3.2 2.4±1.3 ** 13.4±3.3 | 117.8±24.0 41.7±15.4 ** 85.1±32.2 * 57.8±29.4 ** 40.7±9.7 ** 57.1±21.9 13.8±7.8 ** 73.7±20.9 | 17.2±2.8 7.8±3.4 ** 13.2±3.1 *(23.3) 8.8±2.8 **(48.8) 4.1±1.9 ** 7.1±3.9 ** 2.2±1.4 ** 12.5±4.1 | 104.4±16.6 47.3±22.2 ** 77.3±23.8 ** 55.2±22.8 ** 25.8±12.6 ** 43.8±22.7 ** 13.4±8.6 82.5±28.9 ** |
Remarks: 1. hydrocortisone, rutin, gallic acid are prepared with physiological saline, and all the other samples are prepared with 5% propylene glycol.2. the alcohol extracting powder sample that digs up the roots disperses difficult in propylene glycol and outside ultrasonic 4 hours, all the other samples were handled in all ultrasonic 10 minutes.3. "
*" "
*" represent respectively to compare P＜0.05, P＜0.01 with model group.
Draw from three interpretations:
1. the sample produced of spraying drying and drying under reduced pressure technology is from the two no significant difference of anti-inflammatory angle (40mg/kg).
2. root, stem, the leaf triol product that get sample are put forward powder anti-inflammatory action the best with leaf-alcohol, show Herba Polygoni Capitati anti-inflammatory activity composition mainly in the middle of leaf, three test-results inductive statisticses of three position alcohol extracting samples are handled seeing Table 4.
Flavones content and the statistical study of anti-inflammatory dependency in table 4 piece, stem, the leaf
| Sample number into spectrum | Title | Flavones content | Inhibitory rate of intumesce | The γ value |
| w-1-4 w-1-4 w-1-4 w-1-5 w-1-5 w-1-5 w-1-6 w-1-6 w-1-6 | Root alcohol extracting powder root alcohol extracting powder root alcohol extracting powder stem alcohol extracting powder stem alcohol extracting powder stem alcohol extracting powder leaf-alcohol is carried the powder leaf-alcohol and is carried the powder leaf-alcohol and carry powder | 22.53 22.53 22.53 19.41 19.41 19.41 62.93 62.93 62.93 | 28.0 25.1 16.3 25.4 14.7 15.7 31.2 48.5 43.0 | γ＝0.850 P＜0.01 |
This shows: the flavones content at anti-inflammatory activity and above-mentioned three positions has the positive correlation relation.
3. bright product alcohol extracting and bright product water are carried the two relatively, and the anti-inflammatory action that the water deduction divides obviously is better than the alcohol extracting composition.The anti-inflammatory action activeconstituents that shows Herba Polygoni Capitati is mainly water-soluble.
4. rutin, gallic acid dosage all reach 20mg/kg, the content in the above-mentioned Herba Polygoni Capitati sample.Experimental result only demonstrates rutin antiphlogistic effects, but action intensity fails to surpass the several times of Herba Polygoni Capitati extraction composition, illustrate that anti-inflammatory component also has other activeconstituentss to exist in the Herba Polygoni Capitati except that flavones, and gallic acid may not be the anti-inflammatory composition.
The test-results explanation:
1. Herba Polygoni Capitati root, stem, the leaf-alcohol product that get sample are put forward powder anti-inflammatory action the best with leaf-alcohol, show that Herba Polygoni Capitati anti-inflammatory activity composition mainly in leaf, removes root, and the anti-inflammatory activity of Herba Polygoni Capitati over-ground part is unaffected;
2. the anti-inflammatory action of water deduction branch obviously is better than the alcohol extracting composition, shows that the anti-inflammatory action activeconstituents of Herba Polygoni Capitati is mainly water-soluble.
Test two: inside and outside anti-microbial activity research
In-vitro antibacterial experimental technique: adopt the agar doubling dilution to measure the minimum inhibitory concentration (MIC) of the extract that different medicinal parts and different extraction processes obtain.With multiple spot inoculation instrument with microbionation in the agar plate surface that contains different pharmaceutical concentration, every some bacteria containing amount is about 10
5CFU/ml is hatched 18 hours (gonococcus hatched 48 hours) observationss for 37 ℃, is the minimum inhibitory concentration (MIC value) of medicine to this bacterium with the minimum concentration of contained drug in the no bacterial growth plate substratum.
Antimicrobial protection experimental technique in the body: laboratory animal is pressed sex; body weight is evenly divided into groups; every group of 10 mouse; male and female half and half; give mouse stomach different agents areas; the Herba Polygoni Capitati sample of different extraction processes; once a day; 0.5ml/20g mouse is heavy; continuous in advance gastric infusion 3 days; after administration in the 3rd day, respectively organize the mouse peritoneal infection and tried bacterium liquid; every mouse infection dosage is 0.5ml (1MLD), and the Norxin capsule reaches 4 hours more at once behind infectious bacteria liquid gastric infusion is once established simultaneously and infected control group and medicine control group (not infectious bacteria); record infects mouse survival number in back seven days, calculates its median effective dose (ED according to infecting back seven days animals survived numbers
50) and 95% fiducial limit or calculate to infect back seven days animals survived numbers and infect control group t test value relatively, judge and infect control group indifference is relatively arranged.
Experimental result:
(1) the in-vitro antibacterial experimental result sees Table 5.
1. gallic acid, seed alcohol extract (w-1-7) are to the examination Gram-positive, negative bacteria and Candida albicans all present certain antibiotic vigor, secondly are leaf-alcohol extract (w-1-6), Herba Polygoni Capitati 75% second alcohol extract (w-1-10), spraying drying (w-1-2) and drying under reduced pressure (w-1-3).
2.11 plant the Herba Polygoni Capitati sample the clinical separation gonococcus of try had good antibacterial activity in vitro.
3.11 kind Herba Polygoni Capitati sample is better than suis to the antibiotic vigor of clinical SEPARATION OF GOLD staphylococcus aureus, staphylococcus epidermidis in this test.
4.11 plant the Herba Polygoni Capitati sample in this test to the MIC scope of the escherichia coli of the negative bacillus that tried, Bacillus proteus, dysentery bacterium at 1.56～400mg/ml; To the MIC scope of klebsiella pneumoniae and Pseudomonas aeruginosa be 6.25～＞40mg/ml.
5.11 plant the Herba Polygoni Capitati sample to the oidiomycetic antibiotic vigor of white a little less than.
6. Herba Polygoni Capitati spray-drying powder (W-1-2) is to dermatophytes such as microsporon gypseum, gypsum tinea bacterium, and the MIC value of trichophyton is 25～100mg/ml; To the examination anerobe (as bacteroides fragilis, dyspepsiacoccus, peptostreptococcus, the MIC value of propionibacterium acnes and propionibacterium granulosum is 12.5～200mg/ml.)
(2) the antimicrobial protection experimental result sees Table 6 in the body.
1. the Herba Polygoni Capitati sample oral administration of different agents areas, different extraction processes, infection has certain therapeutic action to mouse streptococcus aureus MSSA43.Herba Polygoni Capitati drying under reduced pressure powder, Herba Polygoni Capitati spray-drying powder, root are carried pure thing, leaf and are carried pure thing, stem and carry pure thing, bright product alcohol extract, the aquatic foods product aqueous extract ED to streptococcus aureus MSSA43 infecting mouse
50Be respectively 13.62,6.87,16.14,9.14,15.29,13.62,23.47g crude drug/kg.
2. the Herba Polygoni Capitati sample oral administration of different agents areas, different extraction processes; relatively poor to escherichia coli 994 infecting mouse endogenous protective effects; when administration concentration is 1.2g/ml crude drug concentration, 0.8g/ml crude drug concentration, 0.4g/ml crude drug concentration; the mouse survival rate is all more than or equal to 60%, and infects control group relatively there are no significant difference (P＞0.05).
The in-vitro antibacterial spectrum of the different medicinal parts of table 5, different extraction, preparation technology's Herba Polygoni Capitati sample
| Bacterium (bacterium number) | (W-1-2) spraying drying (mg/ ml) | (W-1-3) drying under reduced pressure (mg/m l) | (W-1-4) root alcohol extracts (mg/ml) | (W-1-5) stem alcohol extracts (mg/ml) | (W-1-6) leaf-alcohol extracts (mg/ml) | (W-1-7) seed is carried thing (mg/ml) | (W-1-8) bright product alcohol extractings (mg/ml) | (W-1-9) bright product water is carried (mg/ml) | (W-1-10) medicine 75% second alcohol extract (mg/ml) | (W-1- 12) | The molten thing of (W-1-14a) poach alcohol precipitation (mg/ml) | (w-1-14b) water extracting alcohol hypostasis (mg/ml) | Positive control gallic acid (mg/m l) | Positive control Ciprofloxacin (μ g/ml) | Positive control ceftriaxone sodium (μ g/ml) | Positive control JIEERYIN (mg/ml) | Positive control fluconazole (μ g/ml) |
| The yellow sarcine staphylococcus aureus of shigella dysenteriae pseudomonas aeruginosa 994 Klebsiella Pneumoniaes 9938 Klebsiella Pneumoniaes 9939 EHECs 992 EHECs 993 EHEC ATCC25922 proteus 993 proteus 994 Tengs 209P staphylococcus aureus 9981 staphylococcus aureuses 9982 staphylococcus aureuses 9983 table Portugal coccuses 994 table Portugal coccuses 995 table Portugal coccus 9916 Ka Tashi coccuses 3 C group streptococcus A type hemolytic streptococcus gonococcus 1 gonococcus 2 gonococcus 3 gonococcus 4 gonococcus 5 gonococcus 6 gonococcus 7 gonococcus 8 gonococcus 9 gonococcus 10 gonococcus 11 gonococcus 12 gonococcus 13 | 100 100 25 25 25 6.25 25 25 25 12.5 6.25 12.5 12.5 12.5 6.25 12.5 6.25 400 400 400 3.12 3.12 0.05 0.2 0.1 0.025 0.025 0.39 0.025 0.025 0.1 0.39 0.05 | 50 25 50 50 25 12.5 50 50 50 12.5 6.25 6.25 25 6.25 6.25 6.25 6.25 100 100 100 0.78 0.78 0.0125 0.78 0.025 0.78 0.78 0.78 0.78 0.78 0.05 0.78 0.05 | 100 50 100 100 50 50 100 100 100 50 25 50 50 50 50 50 50 200 200 200 25 25 6.25 50 50 6.25 6.25 6.25 6.25 50 6.25 25 6.25 | 50 50 50 100 25 1.56 50 25 25 0.39 0.39 0.78 0.39 0.39 0.78 25 6.25 400 400 400 25 25 0.1 0.2 0.2 25 0.2 0.2 25 0.2 0.2 25 25 | 12.5 62.5 12.5 12.5 3.12 0.78 6.25 3.12 3.12 0.39 1.56 0.78 0.78 0.78 0.78 0.78 0.78 12.5 12.5 12.5 1.56 1.56 0.003 6.25 12.5 6.25 0.03 0.03 6.25 6.25 6.25 0.025 0.003 | 3.12 1.56 12.5 12.5 0.39 0.05 6.25 6.25 6.25 0.05 0.05 0.05 0.05 0.05 0.05 0.39 0.39 12.5 12.5 12.5 1.56 1.56 0.39 1.56 3.12 3.12 1.56 1.56 3.12 3.12 1.56 1.56 0.39 | 6.25 100 100 100 0.39 0.39 6.25 3.12 6.25 0.39 0.05 0.05 0.05 0.05 0.39 3.12 0.39 200 200 200 0.025 0.025 1.56 0.2 0.2 1.56 0.025 0.1 0.78 0.2 1.56 1.56 0.025 | 25 25 25 25 12.5 3.12 25 25 25 12.5 1.56 1.56 1.56 1.56 3.12 25 1.56 400 400 400 3.12 ＞50 3.12 0.39 0.39 1.56 0.39 3.12 0.05 1.56 12.5 6.25 0.39 | 25 12.5 25 50 0.78 0.1 12.5 6.25 6.25 0.1 0.1 0.1 0.1 0.1 0.78 0.78 1.56 25 25 25 6.25 6.25 1.56 6.25 3.12 3.12 6.25 0.1 1.56 1.56 3.12 6.25 3.12 | 200 200 400 400 100 100 200 200 200 100 25 12.5 6.25 6.25 100 100 50 400 400 400 12.5 25 3.12 1.56 1.56 12.5 1.56 1.56 3.12 3.12 3.12 3.12 1.56 | 25 25 50 50 25 12.5 12.5 25 25 12.5 1.56 12.5 1.56 1.56 3.12 25 6.25 400 400 400 3.12 3.12 0.78 ＞100 ＞100 1.56 3.12 0.78 0.2 25 0.78 0.78 0.78 | 25 100 400 400 3.12 3.12 200 50 50 1.56 0.1 0.05 0.05 0.78 6.25 3.12 0.05 200 200 200 12.5 6.25 6.25 12.5 6.25 6.25 6.25 6.25 6.25 6.25 12.5 6.25 6.25 | 12.5 12.5 12.5 6.25 3.12 3.12 6.25 12.5 12.5 12.5 12.5 12.5 6.25 6.25 12.5 12.5 6.25 12.5 12.5 12.5 1.56 0.78 0.05 0.78 0.05 0.78 0.05 0.05 0.05 0.2 0.78 0.78 0.01 | 4 4 4 4 0.5 0.5 0.5 16 16 4 0.5 4 4 0.5 8 1 1 2 0.5 2 0.78 0.78 0.015 0.78 0.78 0.39 0.0125 0.015 0.015 0.78 0.78 0.78 0.015 | ＞128 ＞128 ＞128 64 128 4 0.03 ＞128 2 4 4 8 8 8 8 ＞128 4 ＞128 ＞128 16 0.0015 6.25 0.0015 0.0015 0.0015 6.25 0.0015 0.0125 0.0015 6.25 6.25 0.39 0.0015 | Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt 8 8 8 62.5 31.5 16 16 8 4 4 1 1 2 | Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt Nt |
| Gonococcus 14 gonococcus 15 gonococcus 16 gonococcus 17 gonococcus 18 gonococcus 19 gonococcus 20 Candida albicans 011 Candida albicans 012 Candida albicans 013 Candida albicans 014 Candida albicans 015 Candida albicans 016 Candida albicans 017 Candida albicans 018 Candida albicans 019 Candida albicans 0110 Candida albicans 0111 Candida albicans 0112 Candida albicans 0113 Candida albicans 0114 Candida albicans 0115 Candida albicans 0116 Candida albicans 0117 Candida albicans 0118 Candida albicans 0119 Candida albicans 0120 | 0.025 0.025 0.1 0.1 0.05 0.39 0.05 400 400 400 400 400 200 200 200 400 400 400 400 400 200 400 400 400 400 400 400 | 0.78 0.05 0.78 0.78 0.78 0.78 0.78 200 200 200 200 200 100 100 200 200 200 200 100 200 200 100 200 200 200 200 200 | 6.25 6.25 50 6.25 6.25 6.25 25 400 400 400 400 400 200 200 400 400 400 400 400 400 400 400 400 400 400 400 400 | 0.2 0.2 25 25 0.2 0.2 0.39 200 200 200 200 200 400 400 100 200 200 200 200 200 200 200 200 200 200 200 200 | 0.39 6.25 6.25 0.025 1.56 1.56 1.56 25 25 50 50 25 12.5 25 6.25 12.5 12.5 25 12.5 12.5 25 25 25 12.5 12.5 25 25 | 1.56 1.56 1.56 1.56 0.39 1.56 1.56 25 25 50 25 25 12.5 12.5 6.25 12.5 12.5 25 25 12.5 12.5 12.5 12.5 25 12.5 12.5 12.5 | 0.25 6.56 0.2 0.2 1.56 1.56 1.56 200 400 200 200 200 200 400 100 200 200 200 400 200 200 400 200 200 200 200 200 | 0.39 0.39 12.5 3.12 3.12 0.39 6.25 400 400 400 400 400 200 400 200 400 400 400 400 400 400 400 400 400 400 400 400 | 1.56 0.2 0.78 0.78 1.25 0.78 1.56 50 50 50 100 50 25 50 100 25 50 25 100 25 25 50 25 50 25 25 50 | 3.12 6.25 3.12 6.25 1.56 1.56 3.12 ＞400 ＞400 400 400 400 ＞400 ＞400 ＞400 ＞400 400 400 ＞400 ＞400 ＞400 ＞400 ＞400 ＞400 ＞400 ＞400 ＞400 | 0.2 0.2 0.78 0.78 0.2 0.2 0.78 400 400 400 400 400 200 400 200 200 400 400 400 400 400 400 400 400 400 400 400 | 6.25 6.25 12.5 12.5 6.25 6.25 12.5 400 400 400 400 400 200 400 200 100 200 200 400 200 400 400 200 400 400 200 400 | 0.01 0.01 1.56 0.39 0.39 0.78 0.78 25 25 25 12.5 25 25 50 12.5 12.5 12.5 25 25 12.5 6.25 12.5 25 25 6.25 12.5 25 | 0.1 0.0125 0.78 0.015 0.2 0.025 0.2 64 128 128 ＞128 ＞128 128 ＞128 128 ＞128 ＞128 64 ＞128 ＞128 ＞128 128 ＞128 32 64 ＞128 ＞128 | 0.0125 0.0125 6.25 0.0015 0.125 0.05 0.39 128 ＞128 ＞128 ＞128 ＞128 ＞128 ＞128 ＞128 128 ＞128 128 ＞128 ＞128 ＞128 ＞128 ＞128 128 128 ＞128 ＞128 | 1 2 8 1 8 4 31.25 16 8 31.25 4 4 31.25 8 62.5 8 128 4 4 62.5 4 62.5 8 16 4 4 8 | Nt Nt Nt Nt Nt Nt Nt 0.03 0.06 2 2 1 2 4 0.03 0.5 0.5 0.25 0.125 0.125 0.5 8 4 8 2 0.03 0.125 |
Annotate: Nt=not tested (not test)
The endogenous protective experimental result of the different Herba Polygoni Capitati extracts of table 6
| Infection strain (bacterial strain number) (infection dosage CFU/ml) | Medicine | Numbering | ED50 (g/kg) 95% fiducial limit | The P value |
| Streptococcus aureus MSSA43 (2.5 * 10 5) EHEC 994 (3.0 * 105) | Spray dried powder drying under reduced pressure powder root alcohol extract stem alcohol extract alcohol extracts from the leaves fresh goods alcohol extracting fresh goods water extraction w-1-2 adds the particle Norfloxacin capsule spray dried powder drying under reduced pressure powder root alcohol extract stem alcohol extract alcohol extracts from the leaves fresh goods alcohol extracting fresh goods water extraction w-1-2 that auxiliary material makes and adds the particle Norfloxacin capsule that auxiliary material is made | W-1-2 w-1-3 w-1-4 w-1-5 w-1-6 w-1-8 w-1-9 w-1-12 positive control w-1-2 w-1-3 w-1-4 w-1-5 w-1-6 w-1-8 w-1-9 w-1-12 positive control | 6.87(0-1000) 13.62(0-1000) 16.14(9.11-23.12) 15.29(0-1000) 9.14(0-1000) 13.62(3.89-19.94) 23.47(17.77-33.07) ＞30 25.96(16.09-35.24)(mg/kg) ＞30 ＞30 ＞30 ＞30 ＞30 ＞30 ＞30 ＞30 57.97(43.33-78.24)(mg/kg) | P＜0.05 P＜0.05 P＜0.05 P＜0.05 P＜0.05 P＜0.05 P＜0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 P＞0.05 |
The test-results explanation:
1. the antibacterial activity in vitro intensity of different medicinal parts is followed successively by: seed＞leaf＞stem＞root.The anti-microbial activity of seed and leaf obviously is better than stem and root; And anti-microbial activity and no significant difference between seed and the leaf, between stem and the root.Seed source and gather all difficulty, and root is related to the regeneration of medicinal material and resource, environment protection, it is more suitable therefore to adopt leaf and stem or over-ground part to do medicinal material.
2. herb, bright product obviously are better than the sample of using water extraction with the antibacterial activity in vitro of the sample of 95% extraction using alcohol.
3. herb, dry product water are carried the back drying under reduced pressure, still use spraying drying, and the antibacterial activity in vitro of sample is not had obvious influence.
4. the antibacterial activity in vitro of Herba Polygoni Capitati extract powder obviously is better than sample (w-1-12).
5. bright product alcohol extract is better than bright product aqueous extract to the interior curative effect of infection of staphylococcus aureus.
6. the Herba Polygoni Capitati spray-drying powder is better than Herba Polygoni Capitati drying under reduced pressure powder to the interior curative effect of infection of staphylococcus aureus and is better than heat and drenches clear particle.
7. leaf 95% second alcohol extract is better than root 95% second alcohol extract and stem 95% second alcohol extract to the interior curative effect of infection of staphylococcus aureus.
8. the Herba Polygoni Capitati sample oral administration of different agents areas, different extraction processes, relatively poor to escherichia coli 994 infecting mouse endogenous protective effects.
Test three: analgesic activities research
Experimental technique:
Carried out the research of writhing method, hot plate method, radiant heat method three kinds of pain models with regard to W-1-2.
Experimental result:
1. the Dichlorodiphenyl Acetate mouse pain of bringing out has certain analgesic activity, and dose-effect relationship is obvious, and effective dose is 34.8g/kg.
2. radiant heat is stimulated and make the mouse pain model certain analgesic activity is arranged.
The experimental result explanation: extract of the present invention has certain analgesic activity.
Test four: diuretic activity research
Experimental technique:
Catheter collection urine method and two kinds of diuretic tests of metabolic cage method have been carried out with regard to W-1-2.
Experimental result: 17.4g/kg dosage has tangible diuretic properties to the anesthesia rabbit; 8.7g/kg dosage has tangible diuretic properties to normal rat.Dose-effect relationship is not all showed in two tests.
The test-results explanation: extract of the present invention just has certain diuretic properties.
Test five: the research of treatment pyelonephritis
Experimental technique: inoculation colon bacillus ATCC-25922 in the SD kidney of rats essence, manufacture kidney of rats nephropyelitis model.Inquired into the curative effect of Herba Polygoni Capitati extract powder (w-1-2) in the oral administration mode to pyelonephritis.
Experimental result: Herba Polygoni Capitati extract powder 6.0g/kg (amounting to the crude drug amount is 52.32g/kg) has comparatively significantly curative effect to pyelonephritis, compare with the model contrast, administration (i.g.) back can significantly be reduced the quantity of leucocyte in the urine in 3,4,5,6,7 days and be occulted blood, but to the not obviously influence of other biochemical composition of urine.
Presentation of results: the sample of present patent application has certain curative effect to pyelonephritis.
Test six: row's stone activity research
Experimental technique: the spent glycol drinking technique causes rat caoxalate urinary stone disease model, and modeling prevents to give Herba Polygoni Capitati extract powder (w-1-2) 13.1,26.2, three dosage of 52.4g crude drug in whole/kg, continuous 7 days simultaneously.
Experimental result: but Herba Polygoni Capitati extract powder 26.2g crude drug in whole/kg dosage significance reduces the content of animals urine mesoxalic acid, uric acid, and the distribution of kidney Calcium Oxalate and quantity.
Presentation of results: the Herba Polygoni Capitati extract powder has significant protective effect to rat caoxalate urinary stone disease model.
Claims (19)
1. Herba Polygoni Capitati extract is characterized in that:
A. water decocts at twice or divide refluxing extraction two to three times with alcohol-water mixture by the aquatic foods product of Herba Polygoni Capitati herb or in tasting with discrimination, and each 1-2 hour, merge decoction liquor, the relative density during filtering and concentrating to 20 ℃ is 1.2, spraying drying or drying under reduced pressure obtain, perhaps
B. carry the dregs of a decoction by Herba Polygoni Capitati herb and water thereof and obtain through carbon dioxide upercritical fluid extraction,
Alcohol-water mixture wherein is 75% aqueous ethanolic solution or 95% aqueous ethanolic solution.
2. according to the extract of claim 1, wherein Herba Polygoni Capitati is selected its over-ground part for use.
3. according to the extract of claim 2, wherein make water as extraction agent.
4. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is leaf, flower and stem.
5. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is leaf, seed and stem.
6. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is leaf and stem.
7. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is a leaf.
8. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is a stem.
9. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is colored.
10. according to the extract of one of claim 2-3, it is characterized in that the Herba Polygoni Capitati over-ground part is a seed.
11. the extract of one of claim 1-10 is used to expect the purposes of antibacterials fully.
12. according to the purposes of claim 11, wherein antibacterials are anti-gonococcus medicines.
13. the extract of one of claim 1-10 is used to prepare the purposes of anti-inflammatory drug.
14. the extract of one of claim 1-10 is used to prepare the purposes of analgesic.
15. the extract of one of claim 1-10 is used to prepare the purposes of diuretic.
16. the extract of one of claim 1-10 is used to prepare the purposes of the medicine for the treatment of urinary system calculus.
17. the extract of one of claim 1-10 is used to prepare the purposes of treatment pyelonephritis, prostatitic medicine.
18. antibiotic a, anti-inflammatory, analgesia, diuresis, treatment urinary system calculus, treatment pyelonephritis and prostatitic pharmaceutical composition, its extract and pharmaceutically acceptable auxiliaries by one of claim 1-10 is formed.
19. according to the composition of claim 18, it makes granule, pill, capsule, sprays, injection, lotion, suppository, pill, mixture, liniment, patch, film, paper preparation, suspensoid, tincture, dry syrup, effervescent tablet, plaster, ointment, syrup, emulsion, powder, slowly-releasing, controlled release preparation or targeting preparation.
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| CN102716195A (en) * | 2012-02-13 | 2012-10-10 | 李兴惠 | Polygonum capitatum composition for treating or preventing oral diseases |
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Cited By (3)
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| CN101234146B (en) * | 2008-02-29 | 2010-12-08 | 贵阳华芝宝生物研究科技有限公司 | Traditional Chinese medicine preparation for treating urinary system affection and preparation thereof |
| CN102716195A (en) * | 2012-02-13 | 2012-10-10 | 李兴惠 | Polygonum capitatum composition for treating or preventing oral diseases |
| CN102716195B (en) * | 2012-02-13 | 2014-06-18 | 张凯 | Polygonum capitatum composition for treating or preventing oral diseases |
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Denomination of invention: Polygonum capilalum extract , iIts preparation method and use Effective date of registration: 20130926 Granted publication date: 20060531 Pledgee: Agricultural Bank of China Limited by Share Ltd. Guiyang Xinhua Branch Pledgor: GUIZHOU WARMEN PHARMACEUTICAL Co.,Ltd. Registration number: 2013990000711 |
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