CN102161685A - Method for preparing forsythin extractive by fructus forsythiae leaves - Google Patents
Method for preparing forsythin extractive by fructus forsythiae leaves Download PDFInfo
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- CN102161685A CN102161685A CN2011100584860A CN201110058486A CN102161685A CN 102161685 A CN102161685 A CN 102161685A CN 2011100584860 A CN2011100584860 A CN 2011100584860A CN 201110058486 A CN201110058486 A CN 201110058486A CN 102161685 A CN102161685 A CN 102161685A
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- phyllyrin
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- supersound process
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Abstract
The invention discloses a method for preparing forsythin extractive by fructus forsythiae leaves, which comprises the following steps of: soaking, ultrasonically treating, repeatedly treating filter residue for 2-4 times by means of soaking-ultrasonic treating, merging and concentrating filter liquor, dissolving and centrifugally separating, preparing a target product by liquid supernatant, and the like. The extraction method can be used for extracting the effective constituent forsythin in the fructus forsythiae leaves by increasing the running speed of large-medium molecules and improving the penetrating power of large media by the means that the ultrasonic wave has the mechanical effect, the cavitation effect and the heat effect, so that the method has the characteristics of being simple in technology, environment-friendly, low in energy consumption, and low in cost. The method can be used for preparing the extractive of the traditional Chinese medicine constituent forsythin by taking the fructus forsythiae leaves as the raw material, thereby being suitable for the industrial production; and the extractive can be used as the traditional Chinese medicine constituent.
Description
Technical field
The invention belongs to the Chinese medicine preparation field, especially relate to the extraction of effective constituent in a kind of Chinese medicine material, specifically a kind of method for preparing the phyllyrin extract with Folium Forsythiae.
Background technology
The capsule of weeping forsythia (
Fructus Forsythiae) be the Oleaceae plant capsule of weeping forsythia (
Forsythia suspensa(Thunb.) dry fruit Vahl), tool is clearing heat and detoxicating, the effect of dispersing swelling and dissipating binds, is " the conventional Chinese medicine that Chinese pharmacopoeia version in 2010 is recorded.Gather during the just ripe band still of fruit in autumn green, remove impurity, cook, dry, habit claims " green grass or young crops sticks up ", gathers when fruit is well-done, dries, and removes impurity, practises claiming " sticking up always ".
Phyllyrin is one of main pharmacodynamics composition in the capsule of weeping forsythia, it also is the quality index of the capsule of weeping forsythia medicinal material stipulated in 2010 editions pharmacopeia, have antibiotic, antiviral and effect such as cardiac stimulant, inhibition capillary permeability, anti-liver injury, the content of phyllyrin is 0.7% in the Fructus Forsythiae, then is 4% in the Folium Forsythiae.Mainly be to utilize decocting method, water extraction and alcohol precipitation method, thermal backflow alcohol extracting method, microwave-assisted alcohol extracting method etc. from Fructus Forsythiae, to obtain at present, exist loaded down with trivial details, the consuming time length of technology, big, the shortcomings such as blowdown flow rate is big, productive rate is low, production cost height of power consumption.
Summary of the invention
The technical problem to be solved in the present invention, provide a kind of method for preparing the phyllyrin extract with Folium Forsythiae, mechanical effect, cavitation effect and the heat effect of utilizing ultrasonic wave to have, movement velocity by increasing medium molecule, the penetration power that increases medium to be extracting the effective constituent phyllyrin in the Folium Forsythiae, and method provided by the present invention has that technology is simple, environmental friendliness, less energy-consumption, low cost, be fit to characteristics such as suitability for industrialized production.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind ofly prepare the method for phyllyrin extract, carry out according to the following steps order with Folium Forsythiae:
Repeat this step aforementioned operation 1-3 time, the n time (n=1,2 or 3) repeats is with preceding step gained filter residue B
N-1Immersion, supersound process, filtration all can obtain corresponding filter residue B
N+2With liquor C
N+2, that is: when repeating aforementioned operation according to the difference of order, the filter residue that repeats to obtain for the 1st, 2,3 time is respectively B
3, B
4, B
5, the filtrate that obtains is respectively C
3, C
4, C
5
Filtrate merges, concentrates: with the whole liquor C of aforementioned gained
1, C
2... Deng merging, must merge rear filtrate C, be concentrated into dried, mixture D;
Dissolving, centrifugation: mixture D adds anhydrous alcohol solution, and supernatant liquor E is got in centrifugation;
More than be the basic step of method provided by the present invention, wherein: immersion process makes the abundant water-swelling of capsule of weeping forsythia histocyte of dehydration, makes extracting solution infiltration tissue, for the extraction of phyllyrin creates conditions; The principle of supersound process is to utilize ultrasonic wave to produce the sound wave cavatition between solvent and sample, cause formation, growth and the explosion compression of bubble in the solution, thereby solid sample is disperseed, increase the contact area between sample and the extraction solvent, improve target compound and transfer to the rate of mass transfer of liquid phase from solid phase, effective constituent such as phyllyrin in the Folium Forsythiae was dissolved in the extracting solution in the short time, thereby improves the extraction yield of phyllyrin; Filter residue adds the purpose of extracting solution supersound process repeatedly, is in order to improve the extraction yield of target extract, to accomplish to make the best use of everything; Dissolving is to remove to be insoluble to impurity components such as alcoholic acid polysaccharide, protein with the centrifugal purpose.Mechanical effect, cavitation effect and heat effect that the present invention utilizes ultrasonic wave to have; movement velocity by increasing medium molecule, the penetration power that increases medium to be to extract the effective constituent phyllyrin in the Folium Forsythiae, has that technology is simple, environmental friendliness, less energy-consumption, low cost, is fit to characteristics such as large-scale production.
As a kind of optimization of the present invention, described method also comprises step
Extraction yield is measured, promptly
7. extraction yield is measured: utilize the HPLC method, survey step
The content of phyllyrin in the gained phyllyrin extract, and calculate the extraction yield of phyllyrin in the crude drug in view of the above.
The design of this step is intended to grasp the extraction yield of working as phyllyrin in time preparation process Folium Forsythiae.
As a kind of qualification of the present invention, described
In filtrate merging, the enrichment step, described concentrating is meant in 50-60 ℃ of concentrating under reduced pressure.
Evaporation rate of solvent was slow when the temperature of concentrating under reduced pressure was low, the too high inactivation that then might cause effective constituent of temperature.In 50-60 ℃ of concentrating under reduced pressure, taken into account the inactivation that vaporator rate can not cause effective component again, be preferred concentrating under reduced pressure temperature range.
As another kind of qualification the of the present invention, described centrifugation is meant in rotating speed 3000rpm centrifugation 15 min.
Concrete parameter to centrifugation is carried out above-mentioned qualification, makes the abundant sedimentation of alcohol insoluble matter impurity, improves the content of phyllyrin in the extract.
Owing to adopted above-mentioned technical scheme, the present invention compared with prior art, obtained technical progress is:
The raw materials used Folium Forsythiae of present method have aboundresources, cheap characteristics, and its phyllyrin content is higher, can significantly reduce the production cost that extracts phyllyrin; In addition, the technology of present method is simple, save time, energy-conservation, phyllyrin extraction yield height.It is that raw material extracts the traditional Chinese medicine ingredients phyllyrin that the present invention can be used for the Folium Forsythiae, is suitable for suitability for industrialized production, and extract can be used as traditional Chinese medicine ingredients.
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment
Embodiment
Embodiment 1-5 is respectively a kind of and prepares the method for phyllyrin extract with Folium Forsythiae, and their relevant controlling index is with reference to following table.
Embodiment 1-5 carries out according to the following steps order respectively:
Repeat the corresponding number of times of this step aforementioned operation, the n time (n=1,2 or 3) repeats is with preceding step gained filter residue B
N+1Immersion, supersound process, filtration obtain corresponding filter residue B
N+2With liquor C
N+2.That is: according to the difference of order, the 1-3 time is repeated resulting filter residue is respectively B
3, B
4, B
5, the filtrate that obtains is respectively C
3, C
4, C
5
Prepare target product by supernatant liquor: supernatant liquor E gets purpose extract, i.e. the phyllyrin extract of paste through concentrated, dry.
7. utilize the HPLC method, survey step
The content of phyllyrin in the gained phyllyrin extract, and calculate the extraction yield (the concrete extraction yield of each embodiment is as shown in Table) of phyllyrin in the crude drug in view of the above.
Claims (4)
1. one kind prepares the method for phyllyrin extract with Folium Forsythiae, and it is characterized in that: described extracting method carries out according to the following steps order:
Soak: get Folium Forsythiae, the concentration of doubly measuring with 8-10 is the alcohol immersion 1-2 h of 70-85%, gets mixture A;
Supersound process: get mixture A and carry out supersound process 30-40min, filter then, get filter residue B
1With liquor C
1
Repeat aforementioned operation 1-3 time, the n time is repeated is with preceding step gained filter residue B
N+1Immersion, supersound process, filtration obtain corresponding filter residue B
N+2With liquor C
N+2, the filter residue that the 1-3 time obtains when promptly repeating aforementioned operation according to the difference of order is respectively B
3, B
4, B
5, the filtrate that obtains is respectively C
3, C
4, C
5
Filtrate merges, concentrates: with the whole liquor C of aforementioned gained
1, C
2... Deng merging, must merge rear filtrate C, be concentrated into dried, mixture D;
Prepare target product by supernatant liquor: supernatant liquor E gets purpose extract, i.e. the phyllyrin extract of paste through concentrated, dry.
2. according to claim 1ly prepare the method for phyllyrin extract with Folium Forsythiae, it is characterized in that: described extracting method also comprises step
Extraction yield is measured, promptly
7. extraction yield is measured: utilize the HPLC method, survey step
The content of phyllyrin in the gained phyllyrin extract, and calculate the extraction yield of phyllyrin in the crude drug in view of the above.
3. according to claim 1 and 2ly prepare the method for phyllyrin extract, it is characterized in that: described with Folium Forsythiae
In filtrate merging, the enrichment step, concentrated being meant in 50-60 ℃ of concentrating under reduced pressure.
4. according to claim 1 and 2ly prepare the method for phyllyrin extract with Folium Forsythiae, it is characterized in that: described centrifugation is meant in rotating speed 3000 rpm centrifugations 15 min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100584860A CN102161685A (en) | 2011-03-11 | 2011-03-11 | Method for preparing forsythin extractive by fructus forsythiae leaves |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011100584860A CN102161685A (en) | 2011-03-11 | 2011-03-11 | Method for preparing forsythin extractive by fructus forsythiae leaves |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103504437A (en) * | 2013-10-16 | 2014-01-15 | 左权县桐峪镇嘉百岁农民专业合作社 | Forsythia leaf beverage |
| CN105362283A (en) * | 2014-08-07 | 2016-03-02 | 富力 | Applications of phillyrin/phillygenin composition in preparation of drugs or health products for relieving or/and treatment of viral diseases |
| CN111848702A (en) * | 2020-08-24 | 2020-10-30 | 渠志灿 | Extraction and preparation method of phillyrin |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554400A (en) * | 2003-12-26 | 2004-12-15 | 中山大学 | Use of seniawinii in preparing anti-depression, improving brain or/and defatting medicine or food |
| CN1554401A (en) * | 2003-12-26 | 2004-12-15 | 中山大学 | Use of seguinii in preparing medicine or food |
| CN101735290A (en) * | 2008-11-18 | 2010-06-16 | 黑龙江大学 | Method for extracting phillyrin from forsythia |
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2011
- 2011-03-11 CN CN2011100584860A patent/CN102161685A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1554400A (en) * | 2003-12-26 | 2004-12-15 | 中山大学 | Use of seniawinii in preparing anti-depression, improving brain or/and defatting medicine or food |
| CN1554401A (en) * | 2003-12-26 | 2004-12-15 | 中山大学 | Use of seguinii in preparing medicine or food |
| CN101735290A (en) * | 2008-11-18 | 2010-06-16 | 黑龙江大学 | Method for extracting phillyrin from forsythia |
Non-Patent Citations (4)
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| 卢静华，等: "连翘中连翘苷超声法提取工艺的研究", 《辽宁医学院学报》 * |
| 武果桃，等: "两种提取方法对连翘中连翘苷含量的影响", 《中兽医医药杂志》 * |
| 段飞，等: "连翘叶提取物抑菌作用的研究", 《西北药学杂志》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103504437A (en) * | 2013-10-16 | 2014-01-15 | 左权县桐峪镇嘉百岁农民专业合作社 | Forsythia leaf beverage |
| CN103504437B (en) * | 2013-10-16 | 2014-12-24 | 左权县桐峪镇嘉百岁农民专业合作社 | Forsythia leaf beverage |
| CN105362283A (en) * | 2014-08-07 | 2016-03-02 | 富力 | Applications of phillyrin/phillygenin composition in preparation of drugs or health products for relieving or/and treatment of viral diseases |
| CN105362283B (en) * | 2014-08-07 | 2018-07-27 | 富力 | Forsythin/phillygenol composition is preparing the application in alleviating or/and treating the drug or health products of viral disease |
| CN111848702A (en) * | 2020-08-24 | 2020-10-30 | 渠志灿 | Extraction and preparation method of phillyrin |
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Application publication date: 20110824 |