CN101492350A - Method for producing D-pinit from plant locust - Google Patents
Method for producing D-pinit from plant locust Download PDFInfo
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- CN101492350A CN101492350A CNA2009100470487A CN200910047048A CN101492350A CN 101492350 A CN101492350 A CN 101492350A CN A2009100470487 A CNA2009100470487 A CN A2009100470487A CN 200910047048 A CN200910047048 A CN 200910047048A CN 101492350 A CN101492350 A CN 101492350A
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Abstract
The invention relates to a method for preparing D-pinitol from the plant of silver chain in the technical field of agriculture. The method comprises the steps as follows: the silver chain is aired, dried and crushed into powder; mixed ethanol and deionized water solvent is used for stirring and extracting at normal temperature; filtrate is decompressed for vacuum concentration; mixed solvent extract is concentrated into extractum; after the extractum is dissolved by deionized water, sherwood oil is used for extracting; a water phase after extraction is concentrated; macroporous resin is a solid phase to be eluted by distilled water; a product is collected; a Sevag method is used for removing protein and reserving supernatant to be concentrated into paste; the paste is dissolved in the deionized water; the ethanol is added for standing and centrifugating; the supernatant is reserved to be concentrated into the paste which is eluted by a silica gel column; and a target product is collected, evaporated to dryness and recrystallized repeatedly to obtain white acicular crystal. In the method, the D-pinitol is prepared by the silver chain as a raw material by the technical methods of solvent extraction, concentration, solvent exhaustion and column chromatography, so that the invention has simple operation and low cost, and the purity of the obtained product is high.
Description
Technical field
That the present invention relates to is a kind of preparation method of agricultural technology field, and specifically, what relate to is a kind of method for preparing the D-pine camphor from plant locust.
Background technology
Locust tree (Robinia pseudoacacia Linn1) originates in the North America, be introduced into Europe at the beginning of the 17th century, early in the twentieth century introduce China, after locust tree is introduced China, because its extensive adaptability and versatility are extensively planted, according to investigations, China mainland is except that Heilungkiang and Hainan Province, and all there is cultivation in other provinces, cities and autonomous regions.Locust tree is to study a more kind of plant at present, but most research lays particular emphasis on the nutritive value and afforestation value of locust tree.More to the The Chemical Constituents of locust tree both at home and abroad, once be reported in compositions such as finding the real glucoside of lectin, rutin and Chinese scholartree in the locust tree fruit; And main component is the Flower of Black Locust essential oil of monoterpenes and sesquiterpenoid and six kinds of tumor cell lines is had inhibiting flavone component.
The D-pine camphor is a kind of monose with important physiologically active, and report treatment metabolism disorder is arranged, cough, and diabetes are strengthened the confining force of sarkosine, and to the provide protection of liver.
The structural formula of Compound D-Song inositol is:
The D-pine camphor can be by chemosynthesis system, but price is very expensive, mainly comes by the natural preparation of separation and purification from plant at present.
Through existing technical literature retrieval is found that patent WO/2002/077251 prepares the method for D-pine camphor by microbial fermentation with the fragment of soybean.Patent US 6699511 utilizes anion-exchange column to extract preparation from carob, but agriculture waste resource leaf of locust also of no use at present prepares the report of D-pine camphor.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of method for preparing the D-pine camphor from plant locust is provided, this method is raw material with the leaf of locust, adopt solvent extraction, concentrate, solvent extraction and column chromatography processing method prepare the D-pine camphor, simple to operate, with low cost and material purity that obtain is higher.
The present invention is achieved by the following technical solutions, comprises the steps:
The first step, after locust tree dried, drying was ground into powder again.
In second step, doubly to the ethanol and the deionized water mixed solvent of locust tree powder quality, normal temperature stirs down and extracts with 20-40, and the filtrate decompression vacuum concentration is condensed into medicinal extract with the mixed solvent extract;
The 3rd step, with 3~5 times behind the deionized water dissolving paste of leaf of locust powder quality, equal-volume~1/2 volume petroleum ether extraction 3 times.
The 4th step was concentrated into 200ml with the water after the extraction, and macroporous resin is a stationary phase, with 3L-5L distilled water wash-out, collected the water elution product.
The 5th step, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, remove albumen, 3 times repeatedly.Keep supernatant concentration and become cream.
The 6th step, alcohol precipitation: the 5th paste that obtain of step is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leave standstill, centrifugal, keep supernatant liquor, be condensed into cream.
The 7th step, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
The 8th step, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals.
In the described the first step, described drying, its temperature are 40 ℃.
In the described the first step, pulverizing is meant with medicinal herb grinder and is ground into 10 orders-50 purpose plant powder.
In described second step, described ethanol and deionized water mixed solvent, wherein the ethanol volumetric concentration is 10%-50%.
In described second step, described normal temperature stirs down and extracts, and its time is 30min~2h.
In described second step, concentrating under reduced pressure is meant solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated.
In described the 4th step, macroporous resin is a polymeric adsorbent, and consumption is more than 150 times of quality of concentrated solution dry-matter.Adsorption time is more than 24 hours.
In described the 6th step, leave standstill and be meant under 4 ℃ and leave standstill 2h.
The present invention compared with prior art has following advantage:
1. starting material: adopting agriculture waste resource leaf of locust is starting material, utilization of waste material, and wide material sources obtain simply, relatively cheap, have the meaning of Sustainable development
2. production technique: tradition is extracted with straight alcohol, can cause a large amount of pigment impurities, and the number of times that needs to increase extraction in the sepn process of back has improved cost, and low with extraction using alcohol D-pine camphor productive rate.Tradition is used water boiling and extraction, and the solution thickness that obtains should not filter, and the heat-processed energy loss.The present invention adopts gradient extraction under the ethanolic soln normal temperature, can take into account the extraction yield, reduces the filtrate viscosity, shortens disengaging time, raise the efficiency, and simple to operate, saved the energy.The ethanol that the evaporate to dryness concentration process reclaims can extract in the recirculation utilization, has saved material, reduces cost.The zymotechnique of comparing has operation and processing condition characteristic of simple.
3. utilize silicagel column to separate and to obtain highly purified D-pine camphor.Through the detection by quantitative of gas-chromatography, purity can reach 98%.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
1, locust tree is dried after, 40 ℃ of dryings are ground into 10 orders-50 purpose plant powder with medicinal herb grinder again.
2, take by weighing 40 ℃ of dried powder 100g, with 20 times 10% ethanolic soln, stirring at normal temperature is extracted 0.5h, filters, and solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated, medicinal extract 23.5g.
3, with behind the deionized water dissolving paste of 300ml, 1/2 volume petroleum ether extraction 3 times.
4, the water after will extracting is concentrated into 200ml, and HZ841 type low-pole macroporous resin is a stationary phase, with 3L distilled water wash-out, collects the water elution product.
HZ841 is the HZ841 type polymeric adsorbent that Shanghai Huazhen Science and Technology Co., Ltd. of East China University of Science produces according to company standard.
5, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, sample: chloroform: propyl carbinol=25: 5: 1, mix concussion, remove albumen, 3 times repeatedly.Keep supernatant concentration and become cream.
6, paste is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leaves standstill 2h under 4 ℃, and is centrifugal, keeps supernatant liquor, is condensed into cream.
7, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
8, cross silicagel column after, be developer with the phospho-molybdic acid, after the spraying colour developing, the heat gun heating, TLC detects and collects target product D-pine camphor, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals and get the 2.73gD-pine camphor.Purity is 98.1%.
Embodiment 2
1, locust tree is dried after, 40 ℃ of dryings are ground into 10 orders-50 purpose plant powder with medicinal herb grinder again.
2, take by weighing 40 ℃ of dried powder 100g, with 30 times 30% ethanolic soln, stirring at normal temperature is extracted 1h, filters, and solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated, medicinal extract 25.3g.
3, with behind the deionized water dissolving paste of 400ml, equal-volume petroleum ether extraction 3 times.
4, the water after will extracting is concentrated into 200ml, and HZ841 type low-pole macroporous resin is a stationary phase, with 4L distilled water wash-out, collects the water elution product.
5, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, sample: chloroform: propyl carbinol=25: 5: 1, mix concussion, remove albumen, 3 times repeatedly.Supernatant concentration becomes cream.
6, paste is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leaves standstill, and is centrifugal, keeps supernatant liquor, is condensed into cream.
7, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
8, cross silicagel column after, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals and get the 2.75gD-pine camphor.Purity is 97.8%.
Embodiment 3
1, locust tree is dried after, 40 ℃ of dryings are ground into 10 orders-50 purpose plant powder with medicinal herb grinder again.
2, take by weighing 40 ℃ of dried powder 100g, with 40 times 50% ethanolic soln, stirring at normal temperature is extracted 2h, filters, and solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated, medicinal extract 29.1g.
3, with behind the deionized water dissolving paste of 500ml, equal-volume petroleum ether extraction 3 times.
4, the water after will extracting is concentrated into 200ml, and HZ841 type low-pole macroporous resin is a stationary phase, with 5L distilled water wash-out, collects the water elution product.
5, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, sample: chloroform: propyl carbinol=25: 5: 1, mix concussion, remove albumen, 3 times repeatedly.Supernatant concentration becomes cream.
6, paste is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leaves standstill, and is centrifugal, keeps supernatant liquor, is condensed into cream.
7, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
8, cross silicagel column after, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals and get the 2.72gD-pine camphor.Purity is 98.0%.
Embodiment 4
1, locust tree is dried after, 40 ℃ of dryings are ground into 10 orders-50 purpose plant powder with medicinal herb grinder again.
2, take by weighing 40 ℃ of dried powder 100g, with 30 times 20% ethanolic soln, stirring at normal temperature is extracted 2h, filters, and solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated, medicinal extract 28.3g.
3, with behind the deionized water dissolving paste of 300ml, equal-volume petroleum ether extraction 3 times.
4, the water after will extracting is concentrated into 200ml, and HZ841 type low-pole macroporous resin is a stationary phase, with 5L distilled water wash-out, collects the water elution product.
5, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, sample: chloroform: propyl carbinol=25: 5: 1, mix concussion, remove albumen, 3 times repeatedly.Keep supernatant concentration and become cream.
6, paste is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leaves standstill, and is centrifugal, keeps supernatant liquor, is condensed into cream.
7, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
8, cross silicagel column after, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals and get the 2.77gD-pine camphor.Purity is 98.2%.
Embodiment 5
1, locust tree is dried after, 40 ℃ of dryings are ground into 10 orders-50 purpose plant powder with medicinal herb grinder again.
2, take by weighing 40 ℃ of dried powder 100g, with 20 times 50% ethanolic soln, stirring at normal temperature is extracted 1h, filters, and solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated, medicinal extract 24.7g.
3, with behind the deionized water dissolving paste of 500ml, equal-volume petroleum ether extraction 3 times.
4, the water after will extracting is concentrated into 200ml, and HZ841 type low-pole macroporous resin is a stationary phase, with 3L distilled water wash-out, collects the water elution product.
5, after the water elution product concentrates, adopt the long-pending method (Sevag method) of husky dimension, sample: chloroform: propyl carbinol=25: 5: 1, mix concussion, remove albumen, 3 times repeatedly.Supernatant concentration becomes cream.
6, paste is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leaves standstill, and is centrifugal, keeps supernatant liquor, is condensed into cream.
7, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution.
8, cross silicagel column after, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals and get the 2.64gD-pine camphor.Purity is 97.7%.
Claims (8)
1, a kind of method for preparing the D-pine camphor from plant locust is characterized in that comprising the steps:
The first step, after locust tree dried, drying was ground into powder again;
In second step, doubly to the ethanol and the deionized water mixed solvent of locust tree powder quality, normal temperature stirs down and extracts with 20-40, and the filtrate decompression vacuum concentration is condensed into medicinal extract with the mixed solvent extract;
The 3rd step, with 3~5 times behind the deionized water dissolving paste of leaf of locust powder quality, equal-volume~1/2 volume petroleum ether extraction 3 times;
The 4th step was concentrated into 200ml with the water after the extraction, and macroporous resin is a stationary phase, with 3L-5L distilled water wash-out, collected the water elution product;
The 5th step, after the water elution product concentrates, adopt the long-pending method of husky dimension, remove albumen, 3 times repeatedly, keep supernatant concentration and become cream;
The 6th step, alcohol precipitation: the 5th paste that obtain of step is dissolved in the deionized water of 10 times of quality, adds the ethanol of 50 times of quality again, leave standstill, centrifugal, keep supernatant liquor, be condensed into cream;
The 7th step, adopt 300-400 order silicagel column, ethyl acetate-methanol-water is that moving phase increases methyl alcohol ratio gradient elution;
The 8th step, target product collect the back evaporate to dryness with ethanol repeatedly recrystallization get white needle-like crystals.
2, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, the drying described in the first step, its temperature are 40 ℃.
3, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, the pulverizing in the first step is meant with medicinal herb grinder and is ground into 10 orders-50 purpose plant powder.
4, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, ethanol and the deionized water mixed solvent described in second step, and wherein the ethanol volumetric concentration is 10%-50%.
5, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, the normal temperature described in second step stirs down and extracts, and its time is 30min~2h.
6, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, the concentrating under reduced pressure described in second step is meant solution is vacuumized-0.1 normal atmosphere that reduces pressure, and places the rotary water bath below 50 ℃, and solution is concentrated.
7, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, the macroporous resin described in the 4th step is a polymeric adsorbent, and consumption is more than 150 times of quality of concentrated solution dry-matter, and adsorption time is more than 24 hours.
8, the method for preparing the D-pine camphor from plant locust according to claim 1 is characterized in that, leaving standstill described in the 6th step is meant under 4 ℃ leaves standstill 2h.
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103202824A (en) * | 2013-02-21 | 2013-07-17 | 陕西华昕经贸有限公司 | Application of pinitol to pharmacy and health care product |
CN104661668A (en) * | 2012-03-20 | 2015-05-27 | 弗朗西斯梅斯公司 | Method for producing a plant extract from desmodium and its extract |
CN107281255A (en) * | 2017-05-23 | 2017-10-24 | 新乡医学院 | Leaf of locust active site and its preparation method and application |
CN110862305A (en) * | 2019-12-07 | 2020-03-06 | 浙江尖峰健康科技有限公司 | Method for purifying D-pinitol from carob water extract |
CN114392222A (en) * | 2021-12-21 | 2022-04-26 | 上海瑞帝安生物科技有限公司 | Gradient extraction process of plants and application thereof |
Family Cites Families (2)
Publication number | Priority date | Publication date | Assignee | Title |
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ES2179767B1 (en) * | 2001-03-16 | 2004-05-16 | Compañia General Del Algarrobo De España, S.A. | PROCEDURE FOR OBTAINING PINITOL FROM ALGARROBA EXTRACTS. |
WO2005077872A1 (en) * | 2004-02-09 | 2005-08-25 | Cargill, Incorporated | Cyclitol separation method |
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2009
- 2009-03-05 CN CN2009100470487A patent/CN101492350B/en not_active Expired - Fee Related
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104661668A (en) * | 2012-03-20 | 2015-05-27 | 弗朗西斯梅斯公司 | Method for producing a plant extract from desmodium and its extract |
CN103202824A (en) * | 2013-02-21 | 2013-07-17 | 陕西华昕经贸有限公司 | Application of pinitol to pharmacy and health care product |
CN103202824B (en) * | 2013-02-21 | 2015-05-20 | 陕西华昕经贸有限公司 | Application of pinitol to pharmacy and health care product |
CN107281255A (en) * | 2017-05-23 | 2017-10-24 | 新乡医学院 | Leaf of locust active site and its preparation method and application |
CN110862305A (en) * | 2019-12-07 | 2020-03-06 | 浙江尖峰健康科技有限公司 | Method for purifying D-pinitol from carob water extract |
CN110862305B (en) * | 2019-12-07 | 2022-09-30 | 浙江尖峰健康科技有限公司 | Method for purifying D-pinitol from water extract of carob |
CN114392222A (en) * | 2021-12-21 | 2022-04-26 | 上海瑞帝安生物科技有限公司 | Gradient extraction process of plants and application thereof |
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