CN116350708A - Traditional Chinese medicine composition, preparation method thereof and application thereof in preparation of medicines for treating vaginitis - Google Patents
Traditional Chinese medicine composition, preparation method thereof and application thereof in preparation of medicines for treating vaginitis Download PDFInfo
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- 239000003814 drug Substances 0.000 title claims abstract description 152
- 239000000203 mixture Substances 0.000 title claims abstract description 91
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 206010046914 Vaginal infection Diseases 0.000 title claims abstract description 14
- 201000008100 Vaginitis Diseases 0.000 title claims abstract description 12
- 229940079593 drug Drugs 0.000 title abstract description 11
- 239000000284 extract Substances 0.000 claims abstract description 108
- 238000000605 extraction Methods 0.000 claims abstract description 40
- 240000007651 Rubus glaucus Species 0.000 claims abstract description 32
- 235000011034 Rubus glaucus Nutrition 0.000 claims abstract description 32
- 235000009122 Rubus idaeus Nutrition 0.000 claims abstract description 32
- 238000001035 drying Methods 0.000 claims abstract description 32
- 238000002791 soaking Methods 0.000 claims abstract description 21
- 241000244987 Daiswa polyphylla Species 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 4
- 239000003960 organic solvent Substances 0.000 claims description 121
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 120
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 41
- 239000000725 suspension Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 6
- 230000000635 anti-gonococcal effect Effects 0.000 claims description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 241000411851 herbal medicine Species 0.000 claims 1
- 241000588653 Neisseria Species 0.000 abstract description 27
- 230000000694 effects Effects 0.000 abstract description 27
- 229940126680 traditional chinese medicines Drugs 0.000 abstract description 8
- 239000004615 ingredient Substances 0.000 abstract description 3
- 238000011160 research Methods 0.000 abstract description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 25
- 239000000741 silica gel Substances 0.000 description 25
- 229910002027 silica gel Inorganic materials 0.000 description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 24
- 238000010828 elution Methods 0.000 description 9
- 239000012535 impurity Substances 0.000 description 7
- 230000002401 inhibitory effect Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 241000588652 Neisseria gonorrhoeae Species 0.000 description 6
- 239000003480 eluent Substances 0.000 description 6
- 239000004480 active ingredient Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011068 loading method Methods 0.000 description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 238000010898 silica gel chromatography Methods 0.000 description 3
- 229920001817 Agar Polymers 0.000 description 2
- 239000008272 agar Substances 0.000 description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 description 2
- 238000012258 culturing Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 206010000084 Abdominal pain lower Diseases 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 241000234280 Liliaceae Species 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 235000004789 Rosa xanthina Nutrition 0.000 description 1
- 241000220222 Rosaceae Species 0.000 description 1
- 241000123889 Rubus chingii Species 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000003756 cervix mucus Anatomy 0.000 description 1
- 229960003405 ciprofloxacin Drugs 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012676 herbal extract Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 208000024891 symptom Diseases 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P15/00—Drugs for genital or sexual disorders; Contraceptives
- A61P15/02—Drugs for genital or sexual disorders; Contraceptives for disorders of the vagina
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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- A61K2236/55—Liquid-liquid separation; Phase separation
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- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention relates to the technical field of traditional Chinese medicines, and in particular discloses a traditional Chinese medicine composition, a preparation method thereof and application thereof in preparing medicines for treating colpitis. The traditional Chinese medicine composition is prepared from the traditional Chinese medicines of paris polyphylla and raspberry serving as raw materials. Which comprises the following steps: mixing the Chinese medicinal materials of paris polyphylla and raspberry, adding into a solvent for soaking and extracting, concentrating and drying the extracting solution after the extraction is finished to obtain a Chinese medicinal extract, namely the Chinese medicinal composition. The traditional Chinese medicine composition is prepared from the traditional Chinese medicines of paris polyphylla and raspberry, and researches show that the traditional Chinese medicine composition has the effect of resisting gonococcus. Therefore, the traditional Chinese medicine composition provided by the invention can be used as an effective ingredient for preparing medicines with the effect of resisting gonococcus; the traditional Chinese medicine composition provided by the invention can be further used as an effective component for preparing medicines for treating gonococcal vaginitis.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicines, in particular to a traditional Chinese medicine composition, a preparation method thereof and application thereof in preparing medicines for treating colpitis.
Background
Gonococcal vaginitis refers to vaginitis caused by gonococcus (caused by gonococcus); except that it is transmitted by unclean intercourse; the infection can also be indirectly carried out through a bathtub, a toilet bowl and the like; the symptoms of the medicine are red and swollen and painful vaginal orifice, increased vaginal secretion, lower abdominal pain and the like. The gonococcus is pathogenic bacteria of gonococcal vaginitis; however, the gonococcus has a certain degree of drug resistance to antibiotics such as penicillin, tetracycline, ciprofloxacin and the like. Therefore, the development of more medicines with the anti-gonococcus has important significance for treating gonococcal vaginitis.
The rhizoma paridis is dried rhizome of Paris polyphylla or Paris polyphylla of Liliaceae. The Rubi fructus is dry fruit of Rubus chingii Hu of Rosaceae. The prior art mentions that the traditional Chinese medicines rhizoma paridis and raspberry have antibacterial effect; however, the prior art does not mention that the traditional Chinese medicines paris polyphylla and raspberry have the effect of resisting gonococcus. Therefore, the Chinese medicine paris polyphylla and raspberry are used as raw materials, and active ingredients with the function of resisting gonococcus are developed from the raw materials; in particular, the active ingredient having excellent anti-gonococcus effect has important application value.
Disclosure of Invention
In order to overcome at least one technical problem existing in the prior art, the invention provides a traditional Chinese medicine composition.
The technical problems to be solved by the invention are realized by the following technical scheme:
the invention firstly provides a traditional Chinese medicine composition which is prepared from the traditional Chinese medicines of paris polyphylla and raspberry serving as raw materials.
Preferably, the weight ratio of the paris polyphylla to the raspberry is 1:3-5.
Most preferably, the weight ratio of paris polyphylla to raspberry is 1:4.
The inventor has surprisingly found that the Chinese medicinal composition prepared by taking Chinese medicinal paris polyphylla and raspberry as raw materials has the effect of resisting gonococcus. Therefore, the traditional Chinese medicine composition provided by the invention can be used as an effective ingredient for preparing medicines with the effect of resisting gonococcus; the traditional Chinese medicine composition provided by the invention can be further used as an effective component for preparing medicines for treating gonococcal vaginitis.
The invention also provides a preparation method of the traditional Chinese medicine composition, which comprises the following steps:
mixing the Chinese medicinal materials of paris polyphylla and raspberry, adding into a solvent for soaking and extracting, concentrating and drying the extracting solution after the extraction is finished to obtain a Chinese medicinal extract, namely the Chinese medicinal composition.
Preferably, the dosage ratio of the total weight of the Chinese medicinal paris polyphylla and the raspberry to the solvent is 1 g:10-20 mL;
most preferably, the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and raspberry to the solvent is 1g to 15mL.
Preferably, the solvent is selected from ethyl acetate.
Preferably, the soaking and extracting means soaking and extracting for 2-4 d at 20-30 ℃.
Most preferably, the soaking extraction means soaking extraction at 25 ℃ for 3d.
Preferably, the preparation method further comprises an extraction step; the extraction steps are as follows:
adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the traditional Chinese medicine extract, namely the traditional Chinese medicine composition.
Further preferably, the organic solvent is selected from one or more of toluene, cyclohexane, ethyl acetate and n-butanol.
Preferably, the organic solvent consists of toluene and ethyl acetate; wherein the volume ratio of toluene to ethyl acetate is 2-3:1;
most preferably, the volume ratio of toluene to ethyl acetate is 2:1.
The traditional Chinese medicine extract is further extracted by using the organic solvent through the method disclosed by the invention, so that more effective components with the effect of resisting the gonococcus are further enriched, and further the effect of resisting the gonococcus of the prepared traditional Chinese medicine composition is further improved.
The inventors found in the study that the degree of improvement of the anti-gonococcus effect with respect to the extract of the traditional Chinese medicine was different with respect to the extract of the traditional Chinese medicine, which was extracted with different organic solvents. The inventor has surprisingly found in a large number of experiments that when the traditional Chinese medicine extract (traditional Chinese medicine composition) is obtained by adopting an organic solvent consisting of toluene and ethyl acetate for extraction, the anti-gonococcus effect is greatly improved compared with that of the traditional Chinese medicine extract; the improvement degree is far higher than that of the traditional Chinese medicine extract (traditional Chinese medicine composition) obtained by extraction with other organic solvents or the combination of other organic solvents.
Preferably, the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1 g:30-60 mL, 30-60 mL.
Most preferably, the volume ratio of the herbal extract to water and organic solvent is 1g:50mL:50 mL.
Still more preferably, the preparation method further comprises a silica gel column elution step; the silica gel column elution steps are as follows:
loading the Chinese medicinal extract onto silica gel column, eluting with mixed organic solvent A to remove impurities; then eluting with mixed organic solvent B, collecting eluent eluted from the mixed organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition.
Further preferably, the traditional Chinese medicine extract is put on a silica gel column, and eluting and impurity removing are carried out by using a mixed organic solvent A with the volume of 5-8 times of the column volume; and then eluting with 8-12 times of the column volume of the mixed organic solvent B, collecting the eluent eluted from the mixed organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition.
Still more preferably, the mixed organic solvent A is a mixed organic solvent composed of dichloromethane and acetone in a volume ratio of 100:2-4; the mixed organic solvent B is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:12-14.
Most preferably, the mixed organic solvent A is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:3; the mixed organic solvent B is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:13.
The traditional Chinese medicine extract is further subjected to silica gel column chromatography, so that more effective components with the function of resisting gonococcus are further enriched, and further the effect of resisting gonococcus of the prepared traditional Chinese medicine composition is further improved.
The inventor finds that in the silica gel column chromatography, the elution condition of the silica gel column plays a decisive role in further preparing the traditional Chinese medicine composition with more excellent anti-gonococcus effect; the traditional Chinese medicine composition prepared under the condition of silica gel column elution is not selected randomly, and compared with traditional Chinese medicine extracts, the anti-gonococcus effect of the traditional Chinese medicine composition can be improved or greatly improved; the silica gel column elution conditions are not properly selected, and even a large amount of active ingredients with the effect of resisting the gonococcus cannot be enriched, so that the effect of resisting the gonococcus of the prepared traditional Chinese medicine composition can not be improved or can not be greatly improved compared with that of the traditional Chinese medicine extract.
The inventor surprisingly found in a great deal of research that the traditional Chinese medicine extract is eluted by a mixed organic solvent consisting of dichloromethane and acetone with the volume ratio of 100:3 to remove impurities, and then the traditional Chinese medicine composition obtained by eluting by a mixed organic solvent consisting of dichloromethane and acetone with the volume ratio of 100:13 has the effect of resisting gonococcus which is further greatly improved compared with the traditional Chinese medicine extract; so that the prepared traditional Chinese medicine composition has very excellent anti-gonococcus effect.
The beneficial effects are that: the invention provides a brand new traditional Chinese medicine composition; the traditional Chinese medicine composition is prepared from the traditional Chinese medicines of paris polyphylla and raspberry, and researches show that the traditional Chinese medicine composition has the effect of resisting gonococcus. Therefore, the traditional Chinese medicine composition provided by the invention can be used as an effective ingredient for preparing medicines with the effect of resisting gonococcus; the traditional Chinese medicine composition provided by the invention can be further used as an effective component for preparing medicines for treating gonococcal vaginitis.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention in any way. All equivalents made in accordance with this disclosure are intended to fall within the scope of the invention.
EXAMPLE 1 preparation of a Chinese medicinal composition
Mixing Chinese medicinal rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for extraction for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract, namely the Chinese medicinal composition;
wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL.
EXAMPLE 2 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent is toluene.
EXAMPLE 3 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent is cyclohexane.
EXAMPLE 4 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent is ethyl acetate.
EXAMPLE 5 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent is n-butanol.
EXAMPLE 6 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and ethyl acetate in a volume ratio of 2:1.
EXAMPLE 7 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract, namely the traditional Chinese medicine composition;
in the step (2), the volume ratio of the traditional Chinese medicine extract to water to the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and n-butanol in a volume ratio of 2:1.
EXAMPLE 8 preparation of a Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract; wherein, the volume ratio of the traditional Chinese medicine extract to water and the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and ethyl acetate in a volume ratio of 2:1;
(3) Filling 200-300 mesh silica gel with 30 times of the weight of the Chinese medicinal extract into a silica gel column; loading the Chinese medicinal extract on a silica gel column, eluting with 6 times of mixed organic solvent A to remove impurities; then eluting with 10 times of the volume of the mixed organic solvent B, collecting the eluent eluted from the mixed organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition;
in the step (3), the mixed organic solvent A is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:3; the mixed organic solvent B is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:13.
Comparative example 1 preparation of Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract; wherein, the volume ratio of the traditional Chinese medicine extract to water and the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and ethyl acetate in a volume ratio of 2:1;
(3) Filling 200-300 mesh silica gel with 30 times of the weight of the Chinese medicinal extract into a silica gel column; loading the Chinese medicinal extract on a silica gel column, eluting with 6 times of mixed organic solvent A to remove impurities; then eluting with 10 times of the volume of the mixed organic solvent B, collecting the eluent eluted from the mixed organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition;
in the step (3), the mixed organic solvent A is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:15; the mixed organic solvent B is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:25.
Comparative example 2 preparation of Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract; wherein, the volume ratio of the traditional Chinese medicine extract to water and the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and ethyl acetate in a volume ratio of 2:1;
(3) Filling 200-300 mesh silica gel with 30 times of the weight of the Chinese medicinal extract into a silica gel column; loading the Chinese medicinal extract on a silica gel column, eluting with 6 times of mixed organic solvent A to remove impurities; then eluting with 10 times of the volume of the mixed organic solvent B, collecting the eluent eluted from the mixed organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition;
in the step (3), the mixed organic solvent A is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:30; the mixed organic solvent B is a mixed organic solvent consisting of dichloromethane and acetone in a volume ratio of 100:50.
Comparative example 3 preparation of Chinese medicinal composition
(1) Mixing rhizoma paridis and Rubi fructus at a weight ratio of 1:4, adding into ethyl acetate, soaking at 25deg.C for 3d, concentrating and drying the extractive solution after extraction to obtain Chinese medicinal extract; wherein the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and the raspberry to the ethyl acetate is 1g to 15mL;
(2) Adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain a traditional Chinese medicine extract; wherein, the volume ratio of the traditional Chinese medicine extract to water and the organic solvent is 1g:50mL:50mL; the organic solvent consists of toluene and ethyl acetate in a volume ratio of 2:1;
(3) Filling 200-300 mesh silica gel with 30 times of the weight of the Chinese medicinal extract into a silica gel column; loading the Chinese medicinal extract on a silica gel column, eluting with 6 times of mixed organic solvent A to remove impurities; then eluting with 10 times of the volume of the mixed organic solvent B, collecting the eluent eluted by the organic solvent B, concentrating to remove the organic solvent, and drying to obtain the traditional Chinese medicine active site, namely the traditional Chinese medicine composition;
in the step (3), the mixed organic solvent A is a mixed organic solvent consisting of petroleum ether and ethyl acetate in a volume ratio of 100:3; the mixed organic solvent B is a mixed organic solvent consisting of petroleum ether and ethyl acetate with the volume ratio of 100:13.
Experimental example 1 anti-gonococcal Activity assay
Taking a plurality of test tubes, and then adding 1ml of LB liquid medium into each test tube; inoculating the test tubes with a diplococcus gonorrhoeae; then adding the traditional Chinese medicine composition to be tested into each test tube; the final concentration of each traditional Chinese medicine composition in each test tube is set according to the concentration of the sesquidilution of 512 mug/ml, 256 mug/ml and 128 mug/ml to 0.125 mug/ml; then at 37℃5% CO 2 Culturing for 24 hours under the condition. After the culture, the bacterial liquid in each test tube is fully dipped by a sterile inoculating loop, streaked on an agar plate, and then the streaked agar plate is subjected to 5% CO at 37 DEG C 2 Culturing for 12h under the condition; determining the concentration of the growth of the gonorrhoeae-free diplococcus at the scribing site as a Minimum Inhibitory Concentration (MIC); the test results are shown in Table 1.
TABLE 1 Minimum Inhibitory Concentration (MIC) of each Chinese medicinal composition against Diplococcus gonorrhoeae
As can be seen from the experimental results in Table 1, the Chinese medicinal composition prepared in example 1 has a certain resistance to gonococcus; this shows that the Chinese medicinal composition obtained by extracting the Chinese medicinal materials paris polyphylla and raspberry with ethyl acetate has a certain anti-gonococcus.
As can be seen from the experimental results in Table 1, the minimum inhibitory concentration of the traditional Chinese medicine composition prepared in examples 2-7 on the diplococcus gonorrhoeae is further reduced compared with that in example 1; however, the reduction of the traditional Chinese medicine composition prepared by different examples is different. Wherein, the minimum inhibitory concentration of the traditional Chinese medicine composition prepared in the embodiment 6 on the diplococcus gonorrhoeae is reduced to the maximum extent compared with the embodiment 1, and the reduction is far larger than other embodiments. This illustrates: the traditional Chinese medicine extract prepared by the method of the invention in example 1 is further extracted by an organic solvent, which is helpful for further enriching and obtaining more active ingredients with the function of resisting gonococcus, and further is helpful for further improving the function of resisting gonococcus of the prepared traditional Chinese medicine composition. However, the degree of improvement in the anti-gonococcal effect of the extract (composition) of the traditional Chinese medicine obtained by extraction with different organic solvents is different from that of the extract of the traditional Chinese medicine; when the traditional Chinese medicine extract (traditional Chinese medicine composition) is extracted by adopting an organic solvent consisting of toluene and ethyl acetate, the anti-gonococcus effect of the traditional Chinese medicine extract is greatly improved compared with that of the traditional Chinese medicine extract; the improvement degree is far higher than that of the traditional Chinese medicine extract (traditional Chinese medicine composition) obtained by extraction with other organic solvents or the combination of other organic solvents.
As can be seen from the experimental results in Table 1, the minimum inhibitory concentration of the traditional Chinese medicine composition prepared in example 8 on the diplococcus gonorrhoeae is further greatly reduced compared with that of example 6; this illustrates: the traditional Chinese medicine extract is further eluted by the silica gel column elution condition to obtain the traditional Chinese medicine composition, and compared with the traditional Chinese medicine extract, the anti-gonococcus effect of the traditional Chinese medicine composition is further greatly improved; so that the prepared traditional Chinese medicine composition has very excellent anti-gonococcus effect.
As can be seen from the experimental results of table 1, the minimum inhibitory concentration of the traditional Chinese medicine compositions prepared in comparative examples 1 and 2 on the gonococcus was not reduced compared with that of example 6; the minimum inhibitory concentration of the traditional Chinese medicine composition prepared in the comparative example 3 on the diplococcus gonorrhoeae is reduced compared with that of the traditional Chinese medicine composition prepared in the example 6, but the reduction amplitude is not large; the magnitude of the decrease is much smaller than in example 8. This illustrates: in the silica gel column chromatography, the elution condition of the silica gel column plays a decisive role in further preparing the traditional Chinese medicine composition with more excellent anti-gonococcus effect; the traditional Chinese medicine composition prepared under the condition of silica gel column elution is not selected randomly, and compared with traditional Chinese medicine extracts, the anti-gonococcus effect of the traditional Chinese medicine composition can be improved or greatly improved; the silica gel column has improper elution condition and even can not enrich a large amount of active ingredients with the effect of resisting the gonococcus, so that the effect of resisting the gonococcus of the prepared traditional Chinese medicine composition is not improved or greatly improved compared with that of the traditional Chinese medicine extract. The experimental results show that: the traditional Chinese medicine extract can be further and greatly improved compared with the traditional Chinese medicine extract only by the traditional Chinese medicine composition obtained by further eluting under the condition of eluting the silica gel column; can lead the prepared traditional Chinese medicine composition to have excellent anti-gonococcus effect; compared with the traditional Chinese medicine extract, the traditional Chinese medicine composition obtained by eluting under other silica gel column eluting conditions can not be further improved or greatly improved in the action of resisting gonococcus, and the prepared traditional Chinese medicine composition does not have very excellent action of resisting gonococcus.
Claims (10)
1. A Chinese medicinal composition is characterized by being prepared from rhizoma paridis and raspberry serving as raw materials.
2. The traditional Chinese medicine composition according to claim 1, wherein the weight ratio of paris polyphylla to raspberry is 1:3-5;
most preferably, the weight ratio of paris polyphylla to raspberry is 1:4.
3. The method for preparing the traditional Chinese medicine composition according to claim 1 or 2, which is characterized by comprising the following steps:
mixing the Chinese medicinal materials of paris polyphylla and raspberry, adding into a solvent for soaking and extracting, concentrating and drying the extracting solution after the extraction is finished to obtain a Chinese medicinal extract, namely the Chinese medicinal composition.
4. The preparation method according to claim 3, wherein the ratio of the total weight of the Chinese herbal medicines rhizoma paridis and raspberry to the solvent is 1 g:10-20 mL;
most preferably, the dosage ratio of the total weight of the Chinese medicine rhizoma paridis and raspberry to the solvent is 1g to 15mL.
5. A process according to claim 3, wherein the solvent is selected from ethyl acetate.
6. The preparation method according to claim 3, wherein the soaking extraction is performed at 20-30 ℃ for 2-4 d;
most preferably, the soaking extraction means soaking extraction at 25 ℃ for 3d.
7. The method according to claim 3, further comprising an extraction step; the extraction steps are as follows:
adding the Chinese medicinal extract into water for suspension; then adding an organic solvent into the suspension for extraction to obtain an organic solvent extract; concentrating and drying the organic solvent extract to obtain the traditional Chinese medicine extract, namely the traditional Chinese medicine composition.
8. The method according to claim 7, wherein the organic solvent is one or more selected from toluene, cyclohexane, ethyl acetate and n-butanol.
9. The use of the Chinese medicinal composition according to claim 1 or 2 for preparing a medicament having an anti-gonococcal effect.
10. Use of the traditional Chinese medicine composition according to claim 1 or 2 in the preparation of a medicament for treating vaginitis;
preferably, the vaginitis is gonococcal vaginitis.
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CN103110886A (en) * | 2013-01-21 | 2013-05-22 | 宁波大学 | Traditional Chinese medicinal recipe for inhibiting streptococcus |
CN104147170A (en) * | 2014-08-28 | 2014-11-19 | 上海浦东高星生物技术研究所 | Lotion for treating pruritus vulvae |
CN106620392A (en) * | 2017-01-12 | 2017-05-10 | 张超英 | Crab louse-removing lotion |
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Title |
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