CN109106847A - The method that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart - Google Patents
The method that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart Download PDFInfo
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- 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)
- A61K36/73—Rosaceae (Rose family), e.g. strawberry, chokeberry, blackberry, pear or firethorn
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- A61K36/79—Schisandraceae (Schisandra family)
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- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/88—Liliopsida (monocotyledons)
- A61K36/896—Liliaceae (Lily family), e.g. daylily, plantain lily, Hyacinth or narcissus
- A61K36/8968—Ophiopogon (Lilyturf)
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- 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
- A61K2236/10—Preparation or pretreatment of starting material
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- A61K2236/30—Extraction of the material
- A61K2236/37—Extraction at elevated pressure or temperature, e.g. pressurized solvent extraction [PSE], supercritical carbon dioxide extraction or subcritical water extraction
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- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
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- 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 present invention relates to a kind of methods and products thereof that supercritical extraction extracts effective component in the easypro composition of invigorating heart, 0.3~2.0mm is crushed to more particularly to by the ginseng of recipe quantity, Radix Ophiopogonis, Schisandra chinensis, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn, and low temperature drying, individually or after mixing extracted；Using supercritical carbon dioxide as extractant, the flavones ingredient in the easypro preparation of invigorating heart is extracted, provides flavonoids effective constituent for the exploitation of novel formulation.
Description
Technical field
The present invention relates to a kind of methods that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart, belong to invigorating heart
Easypro preparation preparation technical field.
Background technique
Invigorating heart relieving capsule prescription is formed with ancient prescription " Shengmai Yin " plus taste blood-activating drug, treating both manifestation and root cause of disease." Shengmai Yin " is treatment chest
Numbness often uses square foundation, has numerous documents to be seen in report in terms of coronary heart disease clinical research with Shengmai Yin plus taste, significant in efficacy.Invigorating heart
Capsule belongs to national essential drugs (2004), while belonging to " basic medical insurance and work-related injury insurance Drug catalogue " again 2004
Version Chinese patent drug Class B, works well, convenient to take, deep to be favored by many patients.
Currently, invigorating heart is relaxed, preparation has tablet, capsule etc. for the dosage form of selection of clinical, and prescription includes ginseng, Radix Ophiopogonis, five
Taste, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn Six-element medicinal material are rich in a variety of effective ingredients, and relax preparation flavonoids in invigorating heart
Play the role of vital；Currently, invigorating heart is relaxed, preparation mostly uses greatly traditional preparation method: such as water extraction and alcohol precipitation method, alcohol extracting
Water sinks method.There are many effective ingredients extracted due to needs, is relaxed and is made by the invigorating heart that above-mentioned traditional preparation process obtains
The effective ingredient of agent is substantially crude extract, and recovery rate and purity are not able to satisfy the demand of production and application, can not only lead
It causes the dose of patient larger, but also will have a direct impact on the quality and clinical efficacy of product.
Summary of the invention
The object of the present invention is to provide a kind of supercritical extractions to extract flavonoids effective constituent in the easypro composition of invigorating heart
Method, this method can be improved the recovery rate and purity of effective component, to reduce preparation dose, the product made is facing
New product is further developed on bed with good prospect.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:
Supercritical extraction extract invigorating heart relax composition in flavones ingredient method are as follows: by ginseng, Radix Ophiopogonis, Schisandra chinensis,
Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn are crushed to 0.3~2.0mm, and low temperature drying, individually or after mixing are extracted by recipe quantity
It takes；Using supercritical carbon dioxide as extractant, 2~4h is extracted, first time extract remainder is obtained；It is again extraction with supercritical carbon dioxide
Agent carries out second to first time extract remainder and extracts, extracts 2~4h, obtain second of extract liquor, subtract to second of extract liquor
Pressure evaporation, vacuum drying, obtain flavones ingredient extract.
Supercritical extraction above-mentioned extracts in the easypro composition of invigorating heart in the method for flavones ingredient, first time extraction process
In, using petroleum ether, methanol, acetone, ethyl acetate or 60%~80% ethyl alcohol as entrainer, pressure is 30~
50MPa, temperature are 40~60 DEG C, and carbon dioxide flow is controlled in 10~30L/h；In second of extraction process, using petroleum ether,
Methanol, acetone, ethyl acetate or 60%~80% ethyl alcohol as entrainer, pressure is 20~30MPa, and temperature is 40~60
DEG C, carbon dioxide flow is controlled in 10~30Kg/h.
Preferably, in first time extraction process, use 60%~80% ethyl alcohol for entrainer, pressure 40Mpa, temperature 50
DEG C, 2 flow of CO is 25L/h, extraction time 3h；In second of extraction process, use 60%~80% ethyl alcohol for entrainer,
Pressure 30Mpa, temperature 50 C, 2 flow of CO are 30Kg/h, extraction time 3h.The flavones ingredient that preceding method extracts
Extract.
The easypro pharmaceutical preparation of the invigorating heart can be the flavonoids effective constituent for extracting preceding method, be added corresponding
Various pharmaceutical preparations, such as capsule, pill, syrup, tablet, granule, masticatory etc. made of auxiliary material.
For the extraction yield for ensuring flavonoids effective constituent in the easypro composition of invigorating heart, applicant carries out extractant condition
A series of experimental study and screening.
1, laboratory apparatus (being shown in Table 1)
Table one
| Instrument title | Manufacturer |
| AH supercritical fluid extraction equipment | Nantong Huaan supercritical extract Co., Ltd |
| 116 swing pulverizers | Hainan Jia Hui food machinery factory |
| R-220 Rotary Evaporators | Its company of Switzerland's cloth |
| Vacuum oven | The permanent laboratory apparatus head factory in Shanghai one |
2, Chinese medicine is extracting and will use organic solvent in effective component enriching and purifying technique more, such as ethyl alcohol, petroleum ether, second
Acetoacetic ester, n-butanol etc..In order to guarantee that the lower the quality of preparation, the residual quantity of organic solvent the better.The advantages of supercritical extract
One of be organic solvent-free residual.By taking Residual ethanol as an example, using headspace gas chromatography to several conventional extractions
The residual quantity of middle ethyl alcohol is compared, and the results are shown in Table 2.
Table 2
| Extracting method | Supercritical extraction | Heating reflux method | Centrifugal process |
| Residual ethanol (ug/g) | It is not detected | 703.66 | 623.85 |
3, the selection of entrainer
Supercritical extract is carried out to each effective component using different types of entrainer, flavones ingredient is with calycosin
For, using its content of sodium nitrite-aluminum nitrate-sodium hydroxide determination of color；Extraction yield calculation formula is equal are as follows: extraction yield
(%)=(quality/medicinal material quality of effective component) × 100%, gained extraction yield is as shown in table 3.
Table 3
As can be seen from Table 3, in the supercritical state, the extraction yield of each effective component is arranged from high to low are as follows: methanol,
Ethyl alcohol, ethyl acetate, acetone, petroleum ether.Since aforementioned effective component polarity is all larger, in order to reinforce extracting the polarity of environment,
The general big substances of intermolecular attractions such as ethyl alcohol that are added are as entrainer.Judging from the experimental results, in the supercritical state, with not
When congener organic solvent is as entrainer, the extraction efficiency highest of methanol, followed by dehydrated alcohol, ethyl acetate and third
The extraction efficiency of ketone, petroleum ether is minimum.The polarity of ethyl alcohol is not so good as methanol, therefore extraction yield is also compared with low, but since ethyl alcohol is nontoxic
And easily and carbon dioxide mix, under comprehensively considering, preferred alcohol does entrainer.
4, flavones ingredient supercritical extraction process conditional filtering
To find the preferable extractant condition of flavones ingredient, the different extracting pressure of this research selection, extraction temperature,
Extraction time, entrainer and 2 flow of CO are as investigation factor, the extraction using onocerin as Testing index, under the conditions of investigating respectively
Rate the results are shown in Table 4.
Table 4
It can be seen from the experiment that the best supercritical extraction process condition of flavones ingredient are as follows: pressure 30Mpa, temperature 50 C, folder
Band agent is 70% ethyl alcohol, CO2Flow is 30Kg/h, extraction time 3h.
Compared with prior art, the present invention replaces the easypro extraction process of traditional invigorating heart, tool using supercritical fluid extraction
It has the advantage that
1, according to the polarity and boiling point of effective component each in bulk pharmaceutical chemicals, the temperature adapted to, pressure, stream are targetedly specified
The extraction conditions such as body flow, time, entrainer, extract one by one, and almost whole effective components, organic solvent-free are residual in retained product
It stays, improves recovery rate, using the easypro righting preparation of invigorating heart made from preparation process of the invention, the drug administration amount of patient is reduced
, therapeutic effect is more preferable.
2, supercritical fluid extraction is simple to operate；Using CO2As extractant, have many good qualities, such as: price
Cheaply, with high purity, it is easy to produce, and can use with repetitive cycling, to significantly reduce cost；CO2It is a kind of torpescence
Gas, do not chemically react in extraction process, and belong to non-flammable gases, tasteless, odorless, nontoxic, safety is very good.
Specific embodiment
The embodiment of the present invention 1:
A kind of method that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart are as follows: by ginseng, Radix Ophiopogonis, the five tastes
Son, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn are crushed to 1.0mm, and low temperature drying, individually or after mixing are extracted by recipe quantity；
Using supercritical carbon dioxide as extractant, the ethyl alcohol that entrainer is 80%, pressure 40MPa, temperature is 50 DEG C, carbon dioxide stream
Amount control extracts 3h, obtains first time extract remainder in 25L/h；Use 70% ethyl alcohol for entrainer again, pressure 30MPa, temperature
It is 50 DEG C, carbon dioxide flow control carries out second to first time extract remainder and extract, extract 3h in 30Kg/h, obtains second
Extract liquor is evaporated under reduced pressure second of extract liquor, is dried in vacuo, and flavones ingredient extract is obtained.
The embodiment of the present invention 2:
A kind of method that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart are as follows: by ginseng, Radix Ophiopogonis, the five tastes
Son, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn are crushed to 0.3mm, and low temperature drying, individually or after mixing are extracted by recipe quantity；
Using supercritical carbon dioxide as extractant, entrainer is petroleum ether, and pressure 30MPa, temperature is 40 DEG C, carbon dioxide flow control
System extracts 2h, obtains first time extract remainder in 10L/h；Use 60% ethyl alcohol for entrainer again, pressure 20MPa, temperature 40
DEG C, carbon dioxide flow control carries out second to first time extract remainder and extracts, extract 2h, obtain second of extraction in 10Kg/h
Liquid is evaporated under reduced pressure second of extract liquor, is dried in vacuo, and flavones ingredient extract is obtained.
The embodiment of the present invention 3:
A kind of method that supercritical extraction extracts flavones ingredient in the easypro composition of invigorating heart are as follows: by ginseng, Radix Ophiopogonis, the five tastes
Son, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn are crushed to 2.0mm, and low temperature drying, individually or after mixing are extracted by recipe quantity；
Using supercritical carbon dioxide as extractant, entrainer is methanol, and pressure 50MPa, temperature is 60 DEG C, carbon dioxide flow control
In 30L/h, 4h is extracted, first time extract remainder is obtained；Use 80% ethyl alcohol for entrainer again, pressure 25MPa, temperature 60
DEG C, carbon dioxide flow control carries out second to first time extract remainder and extracts, extract 4h, obtain second of extraction in 20Kg/h
Liquid is evaporated under reduced pressure second of extract liquor, is dried in vacuo, and flavones ingredient extract is obtained.
Claims (3)
1. supercritical extraction extract invigorating heart relax composition in flavones ingredient method, it is characterised in that: by ginseng, Radix Ophiopogonis,
Schisandra chinensis, Radix Astragali, Radix Salviae Miltiorrhizae, Rhizoma Chuanxiong, hawthorn are crushed to 0.3~2.0mm, and low temperature drying, by recipe quantity individually or after mixing
It is extracted；Using supercritical carbon dioxide as extractant, 2~4h is extracted, first time extract remainder is obtained；Again with supercritical carbon dioxide
For extractant, second is carried out to first time extract remainder and is extracted, 2~4h is extracted, second of extract liquor is obtained, to second of extract liquor
It is evaporated under reduced pressure, is dried in vacuo, obtain flavones ingredient extract.
2. the method that supercritical extraction according to claim 1 extracts flavones ingredient in the easypro composition of invigorating heart, special
Sign is: in first time extraction process, using petroleum ether, methanol, acetone, ethyl acetate or 60%~80% ethyl alcohol conduct
Entrainer, pressure are 30~50MPa, and temperature is 40~60 DEG C, and carbon dioxide flow is controlled in 10~30L/h；Second of extraction
In the process, using petroleum ether, methanol, acetone, ethyl acetate or 60%~80% ethyl alcohol as entrainer, pressure is 20~
30MPa, temperature are 40~60 DEG C, and carbon dioxide flow is controlled in 10~30Kg/h.
3. method as claimed in claim 1 or 2 is extracted to obtain flavones ingredient extract in the easypro composition of invigorating heart.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111388594A (en) * | 2020-04-21 | 2020-07-10 | 广东先通药业有限公司 | Extraction and quality identification method of effective components of Yixinshu tablet composition |
| CN114681561A (en) * | 2022-04-24 | 2022-07-01 | 康芝药业股份有限公司 | Method for purifying active ingredients in Zhenlingdan mixture |
-
2018
- 2018-11-01 CN CN201811297811.7A patent/CN109106847A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111388594A (en) * | 2020-04-21 | 2020-07-10 | 广东先通药业有限公司 | Extraction and quality identification method of effective components of Yixinshu tablet composition |
| CN114681561A (en) * | 2022-04-24 | 2022-07-01 | 康芝药业股份有限公司 | Method for purifying active ingredients in Zhenlingdan mixture |
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