CN102875442A - Preparation method of high-purity hypaphorine - Google Patents
Preparation method of high-purity hypaphorine Download PDFInfo
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- CN102875442A CN102875442A CN 201210382480 CN201210382480A CN102875442A CN 102875442 A CN102875442 A CN 102875442A CN 201210382480 CN201210382480 CN 201210382480 CN 201210382480 A CN201210382480 A CN 201210382480A CN 102875442 A CN102875442 A CN 102875442A
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Abstract
The invention discloses a preparation method of high-purity hypaphorine. The method includes that a raw material of caragana microphylla is smashed, acidic water is added into the raw material to immerse the raw material, extraction is performed for 2-3times, an extraction liquid is subjected to ultrafiltration by using an ultrafiltration membrane and then to concentration by using a nanofiltration membrane, and an ethanol solution is added to a concentrated solution for precipitation to obtain a precipitate; and the precipitate is subjected to separation by using high-speed counter-current chromatography and then to on-line monitoring by using an ultraviolet detector, and a target fraction is collected and dried under reduced pressure to obtain the hypaphorine. By means of the preparation method for producing the hypaphorine, the method is simple in process operation, the production period is short, the purity of the obtained hypaphorine is not lower than 95%, and the preparation method is suitable for industrial popularization.
Description
Technical field
The invention belongs to biological technical field, particularly relate to a kind of preparation method of high purity hypophorine.
Background technology
Hypophorine (Hypaphorine) be again Hypaphorine, CAS number: 487-58-1, molecular formula: C
14O
18N
2O
2, molecular weight 246.3, molecular structure:
Result of study shows that hypophorine can obviously suppress mice auricle swelling, reduces Mice Auricle weight; Increase mouse thymus, spleen weight, improve the mice serum hemolysin level; Obviously reduce due to CCL4 and the α-naphthyl isothiocyanate transaminase activity and content of bilirubin in the liver injury mice serum, the protection liver injury.
Littleleaf peashrub is the plant of Rosales pulse family, and fruit, flower, root enter Chinese medicine, the Chinese medicine fruit: bitter, and cold in nature.Clearing heat and detoxicating.Flower: it is sweet to distinguish the flavor of, and property is flat.Nourishing blood to tranquillize the mind.Root: sweet, little suffering of distinguishing the flavor of, slightly warm in nature.Wind-expelling pain-stopping, expelling phlegm for arresting cough.
The preparation method of hypophorine adopts silicagel column, gel column and preparation liquid phase process to separate more.Such as document " microwave-assisted extraction-efficient liquid phase chromatographic analysis prepares the research of abrine and Hypaphorine in the Herba Abri ".But the solid-filling post separates and has the shortcomings such as yield is low, output is little, complicated operation, and solvent load is large, seriously polluted.
Summary of the invention
The objective of the invention is to overcome defective and the deficiency of prior art, a kind of quick, easy preparation method of high purity hypophorine is provided.
The objective of the invention is to be achieved through the following technical solutions: a kind of preparation method of high purity hypophorine is characterized in that following steps:
I littleleaf peashrub raw material pulverizing adds acid water soaking and extracts 2～3 times, and concentrated with nanofiltration membrane again after the ultrafiltration of extracting solution ultra-filtration membrane, concentrated solution adds the ethanolic soln precipitation, gets throw out;
The above-mentioned throw out of II adopts high speed adverse current chromatogram to separate, and the UV-detector on-line monitoring is collected the target flow point, and drying under reduced pressure gets hypophorine.
The hollow cellulose film of the optional molecular weight cut-off 10000～2000 of the ultra-filtration membrane described in the step I, nanofiltration membrane are the hollow cellulose film of molecular weight cut-off 200～100.
The optional chloroform of solvent systems that high speed adverse current chromatogram described in the Step II separates, methyl alcohol, water combination, ratio is 3～10:3～5:4～9, and upper is lower phasing mutually, and upper is moving phase mutually.
Advantage of the present invention has:
1) production process adopts membrane separation technique, is a kind of remove impurity make use of physics methods process, need not high temperature, and the liquid of simultaneously nanofiltration process generation can re-use, and reduces environmental pollution;
2) purge process produces that to separate with high speed adverse current chromatogram be a kind of efficient, fast separating process, can continuous production, and sample nondestructive loses, and is environmentally friendly.
Embodiment:
Further specify the present invention below in conjunction with embodiment.
Embodiment 1:
Get 1kg littleleaf peashrub raw material pulverizing, each with 8 times of aqueous hydrochloric acid soak at room temperature of measuring pH2 4 hours, extract 2 times, add the hollow cellulose membrane ultrafiltration of holding back component 2000 behind the extracting liquid filtering, it is concentrated with the hollow cellulose nanofiltration membrane of molecular weight cut-off 200 again to see through liquid, concentrated solution adds the ethanolic soln precipitation, filters to get throw out.Get chloroform, methyl alcohol, water and mix by 5:3:5, fully after the layering, take off and fill with mutually the high speed adverse current chromatogram post, open simultaneously and turn main frame 800rpm, pump into and do mutually moving phase, after system balancing, flow rate regulation is 3ml/min, uses simultaneously moving phase dissolution precipitation thing, by the sampling valve sample introduction, the UV-detector monitoring, collect the target flow point, continuous separate from, merge the flow point drying under reduced pressure and get white powder hypophorine 2.1g, detect purity 99.5% through HPLC.
Embodiment 2:
Get 1kg littleleaf peashrub raw material pulverizing, each with 6 times of aqueous sulfuric acid soak at room temperature of measuring pH3 3 hours, extract 3 times, add the hollow cellulose membrane ultrafiltration of holding back component 5000 behind the extracting liquid filtering, it is concentrated with the hollow cellulose nanofiltration membrane of molecular weight cut-off 100 again to see through liquid, concentrated solution adds the ethanolic soln precipitation, filters to get throw out.Get chloroform, methyl alcohol, water and mix by 7:3:4, fully after the layering, take off and fill with mutually the high speed adverse current chromatogram post, open simultaneously and turn main frame 900rpm, pump into and do mutually moving phase, after system balancing, flow rate regulation is 2ml/min, uses simultaneously moving phase dissolution precipitation thing, by the sampling valve sample introduction, the UV-detector monitoring, collect the target flow point, continuous separate from, merge the flow point drying under reduced pressure and get white powder hypophorine 1.9g, detect purity 98.1% through HPLC.
Embodiment 3:
Get 1kg littleleaf peashrub raw material pulverizing, each with 5 times of aqueous sulfuric acid soak at room temperature of measuring pH2 3 hours, extract 3 times, add the hollow cellulose membrane ultrafiltration of holding back component 3 000 behind the extracting liquid filtering, it is concentrated with the hollow cellulose nanofiltration membrane of molecular weight cut-off 100 again to see through liquid, concentrated solution adds the ethanolic soln precipitation, filters to get throw out.Get chloroform, methyl alcohol, water and mix by 5:4:6, fully after the layering, take off and fill with mutually the high speed adverse current chromatogram post, open simultaneously and turn main frame 800rpm, pump into and do mutually moving phase, after system balancing, flow rate regulation is 1ml/min, uses simultaneously moving phase dissolution precipitation thing, by the sampling valve sample introduction, the UV-detector monitoring, collect the target flow point, continuous separate from, merge the flow point drying under reduced pressure and get white powder hypophorine 2.3g, detect purity 96.5% through HPLC.
Embodiment 4:
Get 1kg littleleaf peashrub raw material pulverizing, each with 8 times of aqueous sulfuric acid soak at room temperature of measuring pH2 4 hours, extract 2 times, add the hollow cellulose membrane ultrafiltration of holding back component 3 000 behind the extracting liquid filtering, it is concentrated with the hollow cellulose nanofiltration membrane of molecular weight cut-off 100 again to see through liquid, concentrated solution adds the ethanolic soln precipitation, filters to get throw out.Get chloroform, methyl alcohol, water and mix by 6:5:2, fully after the layering, take off and fill with mutually the high speed adverse current chromatogram post, open simultaneously and turn main frame 700rpm, pump into and do mutually moving phase, after system balancing, flow rate regulation is 2ml/min, uses simultaneously moving phase dissolution precipitation thing, by the sampling valve sample introduction, the UV-detector monitoring, collect the target flow point, continuous separate from, merge the flow point drying under reduced pressure and get white powder hypophorine 2.0g, detect purity 97.1% through HPLC.
Claims (3)
1. the preparation method of a high purity hypophorine is characterized in that following steps:
I littleleaf peashrub raw material pulverizing adds acid water soaking and extracts 2～3 times, and extracting solution concentrates with nanofiltration membrane after using the ultra-filtration membrane ultrafiltration again, and concentrated solution adds the ethanolic soln precipitation, gets throw out;
The above-mentioned throw out of II adopts high speed adverse current chromatogram to separate, and the UV-detector on-line monitoring is collected the target flow point, and drying under reduced pressure gets hypophorine.
2. the preparation method of high purity hypophorine according to claim 1 is characterized in that the hollow cellulose film of the optional molecular weight cut-off 10000～2000 of the ultra-filtration membrane described in the step I, and nanofiltration membrane is the hollow cellulose film of molecular weight cut-off 200～100.
3. the preparation method of high purity hypophorine according to claim 1, it is characterized in that the optional chloroform of solvent systems, methyl alcohol, water combination that the high speed adverse current chromatogram described in the Step II separates, ratio is 3～10:3～5:4～9, and lower is stationary phase mutually, and upper is moving phase mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210382480 CN102875442A (en) | 2012-10-11 | 2012-10-11 | Preparation method of high-purity hypaphorine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201210382480 CN102875442A (en) | 2012-10-11 | 2012-10-11 | Preparation method of high-purity hypaphorine |
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| CN102875442A true CN102875442A (en) | 2013-01-16 |
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| CN 201210382480 Pending CN102875442A (en) | 2012-10-11 | 2012-10-11 | Preparation method of high-purity hypaphorine |
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2012
- 2012-10-11 CN CN 201210382480 patent/CN102875442A/en active Pending
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Application publication date: 20130116 |