CN112641824A - Chinese medicine clinopodium polycephalum flow extraction method - Google Patents

Chinese medicine clinopodium polycephalum flow extraction method Download PDF

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CN112641824A
CN112641824A CN202011599342.1A CN202011599342A CN112641824A CN 112641824 A CN112641824 A CN 112641824A CN 202011599342 A CN202011599342 A CN 202011599342A CN 112641824 A CN112641824 A CN 112641824A
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clinopodium polycephalum
ethanol
extract
extracting
extraction
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CN112641824B (en
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刘文佳
黄光伟
黄静
胡永志
梁雪松
劳洁
李月菲
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LIUZHOU LMZ CO Ltd
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    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • 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)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30—Extraction of the material
    • A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • 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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Abstract

The invention provides a Chinese medicine clinopodium polycephalum extraction process which comprises the steps of firstly extracting with 50-85 vol.% ethanol as an extraction solvent, then decocting with water, and finally concentrating. The method can improve the content of buddlejasaponins IVb in the clinopodium polycephalum extract, has simple process and can be used for continuous production.

Description

Chinese medicine clinopodium polycephalum flow extraction method
Technical Field
The invention relates to the technical field of extraction processes of effective components of traditional Chinese medicines, in particular to a Chinese medicine clinopodium polycephalum extraction process.
Background
The Clinopodium polycephalum is dry overground part of Clinopodium chinensis (Benth) O. Kuntze and Clinopodium pdycephalum (Vaniot) C.Y. Wuet Hsuan plants in Clinopodium of Labiatae, is a common traditional Chinese medicine collected in pharmacopoeia of the people's republic of China in 2015 edition, has the effects of cooling blood and stopping bleeding, is clinically a good hemostatic medicine, and is mainly used for treating bleeding such as metrorrhagia, hematuria, epistaxis, gingival bleeding, traumatic bleeding, hysteromyoma bleeding and the like. The clinopodium polycephalum contains complex components, mainly contains buddlein IVb, melissoside, hesperidin, beta-sterol, isosakuranetin-7-rutinoside, apigenin, ursolic acid, taraxacin and the like, wherein triterpenoid saponins are main components. Modern pharmacological research and clinical tests prove that the saponin components of the medicine have the effects of treating various haemorrhages, purpura simplex, idiopathic thrombocytopenic purpura and the like, wherein buddleia saponins IVb is one of the effective components. Therefore, the buddlejasaponins IVb in the clinopodium polycephalum can be extracted to the maximum extent, and the method has important practical significance for exerting the efficacy of the extract.
The clinopodium polycephalum flow extraction process comprises a water extraction and alcohol precipitation method, an alcohol extraction method, an enzyme extraction method and the like, wherein the water extraction and alcohol precipitation method and the alcohol extraction method are commonly used, but the extraction rate of buddleia saponins IVb is not very high. The process for extracting the Chinese medicinal clinopodium polycephalum flow aims at improving the content of buddleja saponins IVb to the maximum extent so as to provide a certain theoretical basis and process reference for further development and utilization of the clinopodium polycephalum flow.
Disclosure of Invention
The invention aims to provide a Chinese medicine clinopodium polycephalum flow extraction process aiming at the defects in the prior art, has the advantage of improving the content of buddlejasaponins IVb in a clinopodium polycephalum flow extract, is simple in process and can be used for continuous production.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the Chinese medicine clinopodium polycephalum blood stream extraction method comprises the following steps:
s1, weighing the clinopodium polycephalum medicinal material, adding 50-85 vol.% of ethanol as an extraction solvent, heating, refluxing and extracting once, and separating a first ethanol extract and the clinopodium polycephalum medicinal material after extraction is finished;
s2, adding water serving as an extraction solvent into the clinopodium polycephalum medicinal material processed in the step S1, heating, decocting and extracting for one time, and separating a second water extracting solution and clinopodium polycephalum medicinal dregs after extraction is finished;
s3, concentrating the first ethanol extract, adding the second water extract into the concentrated ethanol extract, mixing and concentrating to obtain the clinopodium polycephalum extract.
Preferably, the method further comprises step S4: s4, adjusting the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract by using ethanol until the index requirements of the finished clinopodium polycephalum traditional Chinese medicine extract are met.
Preferably, in the step S1, the mass of the ethanol is 8-10 times of that of the clinopodium polycephalum.
Preferably, in the step S2, the mass of the water is 8-11 times of that of the clinopodium polycephalum herb.
Preferably, in the step S1, the extraction time is 1 to 3 hours.
Preferably, in the step S2, the extraction time is 1 to 3 hours.
Preferably, in the step S3, the first ethanol extract is concentrated by heating and decompressing at a temperature of 45 ℃ to 75 ℃ and a pressure of-0.06 to-0.085 MPa.
Preferably, in the step S3, after the second water extract is added, the mixture is concentrated under normal pressure, wherein the concentration temperature is 80-100 ℃;
or after adding the second water extracting solution, heating and concentrating under reduced pressure at the temperature of 45-75 ℃ and under the pressure of-0.06 to-0.085 Mpa, and then concentrating under normal pressure at the temperature of 80-100 ℃ for not less than 3 hours.
Preferably, the clinopodium polycephalum herb residue is heated to recover ethanol, and the ethanol recovered from the first ethanol extraction solution concentration and the ethanol recovered from the heated clinopodium polycephalum herb residue are used for the next extraction after the concentration is adjusted.
The invention further provides application of the Chinese medicinal clinopodium polycephalum flow extraction method in improving the content of buddlejasaponins IVb in the Chinese medicinal extract of the clinopodium polycephalum flow.
Compared with the prior art, the invention has the advantages that:
1. the extraction method can effectively improve the extraction rate of buddlejasaponins IVb in the clinopodium polycephalum extract, and the content of buddlejasaponins IVb in the clinopodium polycephalum extract can reach 2550 microgram/g according to the mass ratio of the clinopodium polycephalum medicinal material to the clinopodium polycephalum extract of 1: 1.
2. The method has the advantages of simple process flow, low requirement on equipment conditions, suitability for large-scale operation and industrial popularization prospect.
3. The invention adopts low-toxicity ethanol and water as extraction solvents, is green and environment-friendly, hardly has influence on the health of operators, and has no negative influence on the health of users.
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FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The present invention is further illustrated with reference to the following specific examples and fig. 1, but the scope of the present invention is not limited to the following examples.
Example 1:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 85vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding 11 times of water by mass into the clinopodium polycephalum medicinal material separated by filtration, heating and decocting for 3 hours, filtering, and collecting a second water extract. Heating and concentrating under reduced pressure the first ethanol extractive solution at 60 deg.C under-0.07 Mpa, adding the second water extractive solution, and concentrating at 80 deg.C under normal pressure for 3.5 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the above example 1, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is 1750 mug/g by adopting the high performance liquid chromatography.
Example 2:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 8 times of 70vol.% ethanol-water solution, heating and refluxing for 2 hr, filtering, and collecting the first ethanol extractive solution. Then adding 8 times of water by mass into the clinopodium polycephalum medicinal material separated by filtration, heating and decocting for 2 hours, filtering, and collecting a second water extract. Heating and concentrating under reduced pressure the first ethanol extractive solution at 45 deg.C under-0.085 Mpa, adding the second water extractive solution, and concentrating at 80 deg.C under normal pressure for 3 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the above example 2, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is 1150 mug/g by adopting the high performance liquid chromatography.
Example 3:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 50vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding water with the mass of 10 times into the clinopodium polycephalum medicinal materials separated by filtration, heating and decocting for 3 hours, filtering, and collecting a second water extract. Then heating and concentrating under reduced pressure the first ethanol extractive solution at 75 deg.C under-0.06 Mpa, adding the second water extractive solution, and concentrating at 95 deg.C under normal pressure for 4 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the above example 3, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 2550 mug/g by adopting the high performance liquid chromatography.
Example 4:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 50vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding water with the mass of 10 times into the clinopodium polycephalum medicinal materials separated by filtration, heating and decocting for 3 hours, filtering, and collecting a second water extract. Heating and concentrating under reduced pressure the first ethanol extractive solution at 75 deg.C under-0.06 Mpa, adding the second water extractive solution, concentrating under reduced pressure at 75 deg.C under-0.06 Mpa for 0.5 hr, and concentrating at 95 deg.C under normal pressure for 3 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the above example 3, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 1850 mug/g by high performance liquid chromatography.
Comparative example 1:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 50vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding 10 times of 50vol.% ethanol-water solution into the herba Clinopodii, heating and reflux extracting for 3 hr, filtering, and collecting the second ethanol extract. Then heating and concentrating under reduced pressure the first ethanol extract, adding the second ethanol extract, heating and concentrating under reduced pressure, and concentrating for 4 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the comparative example 1, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 450 mug/g by adopting the high performance liquid chromatography.
Comparative example 2:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of water, heating, refluxing, extracting for 3 hr, filtering, and collecting the first water extractive solution. Then adding 11 times of water by mass into the clinopodium polycephalum medicinal material separated by filtration, extracting for 3 hours, filtering, and collecting a second water extract. Heating, concentrating under reduced pressure, adding the second water extractive solution, and concentrating at 95 deg.C under normal pressure for 3 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the comparative example 2, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 910 mug/g by adopting the high performance liquid chromatography.
Comparative example 3:
removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 95vol.% ethanol-water solution, heating and refluxing for 3 hours, filtering, and collecting the first ethanol extract. Then adding 10 times of water by mass into the clinopodium polycephalum medicinal material separated by filtration, extracting for 3 hours, filtering, and collecting a second water extract. Then heating and concentrating the first ethanol extract under reduced pressure, adding the second water extract, and concentrating at 80 deg.C under normal pressure for 3 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the comparative example 3, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 760 microgram/g by adopting a high performance liquid chromatography.
Comparative example 4
Removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 50vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding water with the mass of 10 times into the clinopodium polycephalum medicinal materials separated by filtration, heating, decocting and extracting for 3 hours, filtering, and collecting a second water extracting solution. Heating and concentrating under reduced pressure the first ethanol extractive solution at 75 deg.C under-0.06 Mpa, adding the second water extractive solution, and concentrating under reduced pressure at 75 deg.C under-0.06 Mpa for 2.5 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the comparative example 3, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is 614 mug/g through high performance liquid chromatography.
Comparative example 5
Removing silt from herba Clinopodii, sun drying, cutting into pieces, and extracting in extraction equipment. Adding 10 times of 50vol.% ethanol-water solution, heating and refluxing for 3 hr, filtering, and collecting the first ethanol extractive solution. Then adding water with the mass of 10 times into the clinopodium polycephalum medicinal materials separated by filtration, heating, decocting and extracting for 3 hours, filtering, and collecting a second water extracting solution. Heating and concentrating under reduced pressure the first ethanol extractive solution at 75 deg.C under-0.06 Mpa, adding the second water extractive solution, concentrating under reduced pressure at 75 deg.C under-0.06 Mpa for 0.8 hr, and concentrating at 95 deg.C under normal pressure for 2.5 hr. Finally, the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract are adjusted by ethanol, and the clinopodium polycephalum extract with the mass ratio of 1:1 is prepared.
In the comparative example 5, the content of the active ingredient buddlejasaponins IVb in the clinopodium polycephalum extract is detected to be 1027 mug/g by adopting the high performance liquid chromatography.

Claims (10)

1. The Chinese medicine clinopodium polycephalum blood stream extraction method is characterized by comprising the following steps:
s1, weighing the clinopodium polycephalum medicinal material, adding 50-85 vol.% of ethanol as an extraction solvent, heating and refluxing for extraction once, and separating a first ethanol extract and the clinopodium polycephalum medicinal material after extraction is finished;
s2, adding water serving as an extraction solvent into the clinopodium polycephalum medicinal material processed in the step S1, heating, decocting and extracting for one time, and separating a second water extracting solution and clinopodium polycephalum medicinal dregs after extraction is finished;
s3, concentrating the first ethanol extract, adding the second water extract into the concentrated ethanol extract, mixing and concentrating to obtain the clinopodium polycephalum extract.
2. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
further comprising step S4: s4, adjusting the weight and the ethanol content of the clinopodium polycephalum traditional Chinese medicine extract by using ethanol until the index requirements of the finished clinopodium polycephalum traditional Chinese medicine extract are met.
3. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S1, the mass of the ethanol is 8-10 times of that of the clinopodium polycephalum medicinal material.
4. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S2, the mass of water is 8-11 times of that of the clinopodium polycephalum medicinal material.
5. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S1, the extraction time is 1-3 h.
6. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S2, the extraction time is 1-3 h.
7. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S3, the first ethanol extract is concentrated by heating and decompressing at the temperature of 45-75 ℃ and under the pressure of-0.06-0.085 MPa.
8. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
in the step S3, after the second water extracting solution is added, concentrating at normal pressure, wherein the concentration temperature is 80-100 ℃;
or after adding the second water extracting solution, heating and concentrating under reduced pressure at the temperature of 45-75 ℃ and under the pressure of-0.06 to-0.085 Mpa, and then concentrating under normal pressure at the temperature of 80-100 ℃ for not less than 3 hours.
9. The method for extracting clinopodium polycephalum of claim 1, which comprises the following steps:
heating herba Clinopodii residue to recover ethanol, concentrating the first ethanol extractive solution to recover ethanol, and adjusting the concentration of ethanol and ethanol recovered from the heated herba Clinopodii residue to obtain ethanol extract for next extraction.
10. The application of the Chinese medicinal clinopodium polycephalum flow extraction method of claims 1-9 in improving the content of buddlejaside IVb in the Chinese medicinal extract of clinopodium polycephalum flow.
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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101804092A (en) * 2010-04-27 2010-08-18 南京泽朗医药科技有限公司 Method for preparing Chinse clinopodium herb total saponins

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101804092A (en) * 2010-04-27 2010-08-18 南京泽朗医药科技有限公司 Method for preparing Chinse clinopodium herb total saponins

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
刘文佳等: "提高断血流提取物指标成分得率的工艺研究", 《口腔护理用品工业》 *
刘芳等: "断血流提取工艺的研究", 《长治医学院学报》 *

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