CN103450211A - Preparation method of perforatic acid - Google Patents
Preparation method of perforatic acid Download PDFInfo
- Publication number
- CN103450211A CN103450211A CN 201310423182 CN201310423182A CN103450211A CN 103450211 A CN103450211 A CN 103450211A CN 201310423182 CN201310423182 CN 201310423182 CN 201310423182 A CN201310423182 A CN 201310423182A CN 103450211 A CN103450211 A CN 103450211A
- Authority
- CN
- China
- Prior art keywords
- perforatic
- acid
- preparation
- blanco
- extracting solution
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
- Medicines Containing Material From Animals Or Micro-Organisms (AREA)
Abstract
The invention relates to a preparation method of perforatic acid, which is easy to operate and has less pollution. The preparation method comprises the following process steps: (1) taking roots of Harrisonia perforata (Blanco) Merr., crushing, performing flash extraction by using alcohol solution and filtering to obtain an extracting solution; (2) passing the extracting solution through a membrane separation system and concentrating and drying to obtain a crude extract; (3) fully mixing normal hexane, ethyl acetate, methanol and water in a separating funnel, standing to layer, taking the bottom phase as a stationary phase, filling a countercurrent chromatograph column, starting a main machine, pumping in the upper phase as a mobile phase, balancing, injecting a sample through an injection valve, and collecting perforatic acid components according to a detection graph; (4) performing vacuum concentration on the perforatic acid components, separating out crystals, and filtering off the crystals to obtain perforatic acid yellow needle crystals. The prepared perforatic acid has high product purity and is easy to realize industrial scale up.
Description
Technical field
The invention belongs to the traditional Chinese medicine extraction separation technology field, relate to a kind of method for preparing perforatic acid of separating from the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco.
Background technology
Perforatic acid (Perforatic acid) derives from the root of Simarubaceae (Simaroubaceae) Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco Harrisonia perforata (Blanco) Merr., mp246.5-248 ℃, and molecular formula is C
16h
14o
6, molecular weight is 302.28, structural formula is:
Perforatic acid has antitumor action.Suppress the external rat liver cancer ascites cells that mixes of 3H-TdR, inhibiting rate is 91.19%.
At present, domestic scholars also in the starting stage, there is not yet the disclosure of perforatic acid industrialized producing technology to the research of perforatic acid.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of perforatic acid.
The objective of the invention is to be achieved through the following technical solutions:
A kind of preparation method of perforatic acid is characterized in that comprising the following steps:
(1) get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, be placed in flash extracter, add 5-12 times of 80-85% ethanolic soln, carry out flash extraction, filter and obtain extracting solution;
(2) nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 2000-3000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, and working pressure is 0.5-2.1MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract;
(3) normal hexane, ethyl acetate, methyl alcohol, water are fully mixed in separating funnel, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, pump into and do mutually moving phase, after balance, annotate sample introduction by sampling valve, according to the detector collection of illustrative plates, collect the perforatic acid component;
(4) the perforatic acid component is carried out to vacuum concentration, crystallization, filtration, washing are drying to obtain perforatic acid.
In described step (1), flash extraction voltage is 140-150V, and extraction time is 60s-90s.
In described step (3), normal hexane, ethyl acetate, methyl alcohol, water blending ratio are 4-6:6-9:3-8:3-5.
In described step (3), the vacuum concentration temperature is 65-75 ℃.
Present method positively effect is:
(1) present method adopts flash extraction method, rapidly and efficiently, low power consuming, environmental protection;
(2) present method adopts membrane separation technique, can effectively remove plurality of impurities, and can not destroy the biological activity of effective constituent;
(3) present method adopts high speed adverse current chromatogram, and yield is high, preparation amount is large, preparation cycle is short, has solved the low and with serious pollution technological deficiency of column chromatography efficiency;
(4) operation of present method processing step is simpler, easy to operate, and products obtained therefrom purity is high.
Further illustrate the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment
Embodiment 1:
Get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, take 1kg, add 5 times of 80% ethanolic soln, extraction voltage is 140V, extraction time is 90s, carries out flash extraction, filters and obtains extracting solution, the nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 3000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, working pressure is 1.2MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract; Get normal hexane, ethyl acetate, methyl alcohol, water, in the 5:6:6:5 ratio, in separating funnel, fully mix, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, adjustment of rotational speed is 900rpm, pump into and do mutually moving phase, after balance, flow velocity is adjusted into 3ml/min, annotate sample introduction by sampling valve, according to the detector collection of illustrative plates, collect the perforatic acid component, carry out vacuum concentration at 68 ℃ of temperature, crystallization, leach crystallization, filtration, washing are drying to obtain the yellow needle of 1.0g perforatic acid, content 94.0%.
Embodiment 2:
Get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, take 1kg, add 12 times of 80% ethanolic soln, extraction voltage is 140V, extraction time is 80s, carries out flash extraction, filters and obtains extracting solution, the nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 2000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, working pressure is 1.8MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract; Get normal hexane, ethyl acetate, methyl alcohol, water, in the 5:8:3:3 ratio, in separating funnel, fully mix, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, adjustment of rotational speed is 1050rpm, pump into and do mutually moving phase, after balance, flow velocity is adjusted into 2.5ml/min, by sampling valve, annotates sample introduction, according to the detector collection of illustrative plates, collect the perforatic acid component, at 75 ℃ of temperature, carry out vacuum concentration, crystallization, filtration, washing are drying to obtain the yellow needle of 1.1g perforatic acid, content 93.4%.
Embodiment 3:
Get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, take 2kg, add 10 times of 85% ethanolic soln, extraction voltage is 140V, extraction time is 70s, carries out flash extraction, filters and obtains extracting solution, the nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 2000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, working pressure is 2.0MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract; Get normal hexane, ethyl acetate, methyl alcohol, water, in the 6:9:8:4 ratio, in separating funnel, fully mix, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, adjustment of rotational speed is 900rpm, pump into and do mutually moving phase, after balance, flow velocity is adjusted into 4ml/min, by sampling valve, annotates sample introduction, according to the detector collection of illustrative plates, collect the perforatic acid component, at 70 ℃ of temperature, carry out vacuum concentration, crystallization, filtration, washing are drying to obtain the yellow needle of 2.5g perforatic acid, content 95.2%.
Embodiment 4:
Get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, take 5kg, add 8 times of 80% ethanolic soln, extraction voltage is 150V, extraction time is 60s, carries out flash extraction, filters and obtains extracting solution, the nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 3000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, working pressure is 0.5MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract; Get normal hexane, ethyl acetate, methyl alcohol, water, in the 5:7:7:5 ratio, in separating funnel, fully mix, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, adjustment of rotational speed is 1000rpm, pump into and do mutually moving phase, after balance, flow velocity is adjusted into 3ml/min, by sampling valve, annotates sample introduction, according to the detector collection of illustrative plates, collect the perforatic acid component, at 75 ℃ of temperature, carry out vacuum concentration, crystallization, filtration, washing are drying to obtain the yellow needle of 7.1g perforatic acid, content 92.8%.
Embodiment 5:
Get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, take 10kg, add 12 times of 85% ethanolic soln, extraction voltage is 150V, extraction time is 90s, carries out flash extraction, filters and obtains extracting solution, the nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 3000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, working pressure is 2.1MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract; Get normal hexane, ethyl acetate, methyl alcohol, water, in the 5:9:8:4 ratio, in separating funnel, fully mix, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, adjustment of rotational speed is 1000rpm, pump into and do mutually moving phase, after balance, flow velocity is adjusted into 2.5ml/min, by sampling valve, annotates sample introduction, according to the detector collection of illustrative plates, collect the perforatic acid component, at 65 ℃ of temperature, carry out vacuum concentration, crystallization, filtration, washing are drying to obtain the yellow needle of 12.7g perforatic acid, content 90.9%.
Claims (4)
1. the preparation method of a perforatic acid is characterized in that comprising the following steps:
(1) get the root of Harrisonia perforata (Blanco)Merr.[Paliurus perforatus Blanco, through pulverization process, be placed in flash extracter, add 5-12 times of 80-85% ethanolic soln, carry out flash extraction, filter and obtain extracting solution;
(2) nanofiltration membrane that the ultra-filtration membrane ultrafiltration that extracting solution is 2000-3000 by molecular weight cut-off and molecular weight cut-off are 200 is concentrated, and working pressure is 0.5-2.1MPa, and membrane concentration liquid concentrating under reduced pressure drying, obtain crude extract;
(3) normal hexane, ethyl acetate, methyl alcohol, water are fully mixed in separating funnel, after stratification, take off the phase that fixes mutually, be full of the counter current chromatograph post, open and turn main frame, pump into and do mutually moving phase, after balance, annotate sample introduction by sampling valve, according to the detector collection of illustrative plates, collect the perforatic acid component;
(4) the perforatic acid component is carried out to vacuum concentration, crystallization, filtration, washing are drying to obtain perforatic acid.
2. the preparation method of a kind of perforatic acid according to claim 1, it is characterized in that: in described step (1), flash extraction voltage is 140-150V, extraction time is 60s-90s.
3. the preparation method of a kind of perforatic acid according to claim 1 is characterized in that: in described step (3), normal hexane, ethyl acetate, methyl alcohol, water blending ratio are 4-6:6-9:3-8:3-5.
4. the preparation method of a kind of perforatic acid according to claim 1 is characterized in that: in described step (3), the vacuum concentration temperature is 65-75 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310423182 CN103450211A (en) | 2013-09-17 | 2013-09-17 | Preparation method of perforatic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201310423182 CN103450211A (en) | 2013-09-17 | 2013-09-17 | Preparation method of perforatic acid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103450211A true CN103450211A (en) | 2013-12-18 |
Family
ID=49733095
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201310423182 Pending CN103450211A (en) | 2013-09-17 | 2013-09-17 | Preparation method of perforatic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103450211A (en) |
-
2013
- 2013-09-17 CN CN 201310423182 patent/CN103450211A/en active Pending
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101759687A (en) | Method for preparing Silymarin | |
| CN103450211A (en) | Preparation method of perforatic acid | |
| CN102381974A (en) | Method for separating and preparing caffeic tannic acid from honeysuckle by utilizing high speed countercurrent chromatography | |
| CN102391344A (en) | Method for preparing picfeltarraenin IA from picria feltarrae lour leaves | |
| CN103232504A (en) | Method for preparing cyanidenon-7-O-beta-D-glucuronide | |
| CN103265556A (en) | Preparation method of castelanone | |
| CN102659736A (en) | Preparation method of sudachitin | |
| CN102827215A (en) | Method for preparing jionoside A1 from purple rehmannia | |
| CN103435471A (en) | Manwuweizic acid preparation method | |
| CN103242333A (en) | Method for purifying Chapa picrasin | |
| CN104072556A (en) | Preparation method of helichrysoside | |
| CN103408405A (en) | Preparation method of dianthus chinensis magnolol | |
| CN102276566A (en) | Method for preparing tricin | |
| CN102532069A (en) | Method for preparing Uvaria calamistrin Hance A | |
| CN104193707A (en) | Bullatanocin preparation method | |
| CN102827113A (en) | Preparation method of annomuricin C | |
| CN104193709A (en) | Method for purifying kavain by utilizing high-speed countercurrent chromatography (HSCCC) | |
| CN102659869A (en) | Preparation method of cassia tora glucoside | |
| CN106620027A (en) | Technological method for extracting tea polyphenol from green tea leaves | |
| CN104072546A (en) | Method for extracting shephagenin A | |
| CN102863496A (en) | Extraction method of Zhankuic acid A | |
| CN102241660A (en) | Method for purifying Brazilein | |
| CN103467562A (en) | Method for extracting Maytenfolone A | |
| CN102643286A (en) | Preparation method of psorospermin | |
| CN102826987A (en) | Extraction method of belamcandaquinone A |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20131218 |