CN102274302A - Preparation method of delphinium total diterpenoid alkaloids - Google Patents
Preparation method of delphinium total diterpenoid alkaloids Download PDFInfo
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- CN102274302A CN102274302A CN2011101517399A CN201110151739A CN102274302A CN 102274302 A CN102274302 A CN 102274302A CN 2011101517399 A CN2011101517399 A CN 2011101517399A CN 201110151739 A CN201110151739 A CN 201110151739A CN 102274302 A CN102274302 A CN 102274302A
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Abstract
The invention discloses a preparation method of delphinium total diterpenoid alkaloids, belonging to the technical field of preparation of natural active components. The preparation method comprises the following steps: soaking delphinium in alkaline water, extracting with ethanol, passing through macroporous resin columns, eluting with the alkaline water, eluting with ethanol solution, passing the eluate through D942 decolorizing resin columns for decolorization, concentrating and drying to obtain the total diterpenoid alkaloids. No toxic organic solvents except alkaline water and ethanol are used in the whole extraction and separation process, and the macroporous resin is reusable; and thus, the invention has the advantages of safe industrial production and low cost, and the purity of the prepared delphinium total diterpenoid alkaloids is high.
Description
Technical field:
The invention belongs to field of medicaments, be specifically related to the alkaloidal preparation method of a kind of Delphinium plant total diterpene.
Background technology:
Diterpene alkaloid is the multi-ring nitrogen-containing compound of a class formation more complicated, have stronger toxicity and extensive biological activity, for many years be the important source that the medicine scholar seeks new drug and lead compound, also be the focus of plant chemotaxonomy man research always.The diterpene alkaloid overwhelming majority is distributed in Aconitum and the Delphinium, in China, and kind surplus the aconitum plant nearly 170, nearly 120 kinds of Delphinium plant, they extensively are distributed throughout the country, and are the most concentrated with the southwest especially, and wherein many is China's Chinese herbal medicine commonly used among the people already.Diterpene alkaloid is not only effective ingredient and the toxic component of this class plant, and is considered to their feature chemical constituent.
Delphinium (Delphinium) is the perennial herb of Ranunculaceae (Ranunculaceae) plant, the whole world is about more than 300 kinds, belong to 3 subgenus, be widely distributed in the north temperate zone, about 113 kinds of China, except that Taiwan, Hainan Island, all there is distribution each provinces and regions, especially with the alpine belt of the north, Yunnan, western Sichuan and Eastern Tibet for seeing more.The principal item of China Delphinium plant has the dry herb of Mere fruit Herba delphinii grandiflori (Delphinium grandiflorum L.var.leiocarpum), poly-umbrella Herba delphinii grandiflori (Delphinium laxicymosum), three lobule Herba delphinii grandifloris (Delphinium trifoliolatum), Qinling Mountains Herba delphinii grandiflori (Delphinium giraldii), Heisui River Herba delphinii grandiflori (Delphinium potaninii), high eyebrow Herba delphinii grandiflori (Delphinium omeiense).The Delphinium plant contains lycaconitine type diterpene alkaloid, and this platymiscium of China has 18 kinds at hyoscine among the people, and diseases such as treatment traumatic injury, rheumatism, toothache, enteritis in addition, have 4 kinds as soil pesticide, kill louse and mosquito, fly larva.
Summary of the invention:
The purpose of this invention is to provide the alkaloidal preparation method of a kind of Delphinium plant total diterpene.
The present invention implements in the following manner:
The alkaloidal preparation method of Delphinium plant total diterpene is characterized in that may further comprise the steps:
(1) extract: the Delphinium plant is ground into coarse powder, places alkali liquor to soak 2-8 hour, filter, remove alkali liquor, filtering residue ethanol heating extraction obtains alcohol extract;
(2) enrichment: with alcohol extract reclaim under reduced pressure reagent, obtain total alkali extractum, add aqueous dispersion, cross the good macroporous resin column of pretreatment, wash with aqueous alkali earlier, the reuse deionized water is eluted to neutrality, discard eluent, use 60-95% ethanol water eluting at last, collect eluent;
(3) decolouring: eluent by the D941 macroporous resin column, is collected effluent, and reuse 4-7 times column volume 90% ethanol elution merges eluent and effluent, and concentrating under reduced pressure, drying obtain the total diterpene alkaloid.
The solid-liquid ratio of raw material and alkali liquor is 1 in the described step (1): 6-26 (kg/L).
Alkali liquor is 0.1-15% sodium hydroxide solution, potassium hydroxide solution, ammonia or aqua calcis in the described step (1), and soaking temperature is 10-80 ℃.
Concentration of alcohol is 60-100% in the described step (1), and extracting temperature is 65-90 ℃, and extraction time is 1-4 hour, and extraction time is 2-4 time.
Selecting macroporous resin in the described step (2) for use is AB-8, D101, HPD100, D201 or D130 type macroporous resin.
Alkali liquor is the alkali liquor of pH7.5-13 in the described step (2), the optional ammonia of alkali liquor, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate or ammonium bicarbonate.
Advantage of the present invention is: be solvent with water, alkali liquor, ethanol in the preparation process, cost is low, pollution is little, and extraction process is simple, and is with short production cycle, is applicable to that industrialization prepares Delphinium plant total diterpene alkaloid in a large number.
The specific embodiment:
Embodiment 1:
Get high eyebrow Herba delphinii grandiflori 5kg, pulverizing is placed in the 40L5% ammonia, under 60 ℃ of conditions, soaked 4 hours, remove by filter alkali liquor,, extract 2 times with 90% alcohol reflux 3 hours, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the D201 macroporous resin column of handling well, earlier be 9.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 80% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 4 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Embodiment 2:
Get Mere fruit Herba delphinii grandiflori 5kg, pulverizing is placed in the 50L0.1% sodium hydroxide, under 80 ℃ of conditions, soaked 6 hours, remove by filter alkali liquor,, extract 2 times with 80% alcohol reflux 4 hours, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the HPD100 macroporous resin column of handling well, earlier be 9.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 75% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 6 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Embodiment 3:
Get poly-umbrella Herba delphinii grandiflori 5kg, pulverizing is placed in the 30L1% potassium hydroxide, under 50 ℃ of conditions, soaked 8 hours, remove by filter alkali liquor,, extract 3 times with 60% alcohol reflux 1.5 hours, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the D130 macroporous resin column of handling well, earlier be 8.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 60% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 5 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Embodiment 4:
Get three lobule Herba delphinii grandiflori 5kg, pulverizing is placed in the 100L15% calcium hydroxide, under 40 ℃ of conditions, soaked 2 hours, remove by filter alkali liquor,, extract 2 times with 75% alcohol reflux 1 hour, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the AB-8 macroporous resin column of handling well, earlier be 10.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 70% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 7 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Embodiment 5:
Get Heisui River Herba delphinii grandiflori 10kg, pulverizing is placed in the 260L0.5% sodium hydroxide, under 20 ℃ of conditions, soaked 5 hours, remove by filter alkali liquor,, extract 3 times with 95% alcohol reflux 2.5 hours, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the HPD100 macroporous resin column of handling well, earlier be 12.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 80% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 4 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Embodiment 6:
Get Qinling Mountains Herba delphinii grandiflori 10kg, pulverizing is placed in the 75L10% ammonia, under 10 ℃ of conditions, soaked 7 hours, remove by filter alkali liquor,, extract 2 times with 85% alcohol reflux 4 hours, merge extractive liquid,, decompression recycling ethanol obtains total alkali extractum to there not being the alcohol flavor, adds aqueous dispersion, by with the D101 macroporous resin column of handling well, earlier be 13.0 aqueous alkali eluting with 2 times of column volume pH, the reuse deionized water is eluted to neutrality, discards eluent, use 5 times of column volume 95% ethanol elutions at last, collect eluent, the eluent of collecting is directly advanced D941 decolorizing resin post, collect effluent, reuse is equivalent to 90% ethanol elution of 5 times of weight resins, merge eluent and effluent, concentrating under reduced pressure, vacuum drying obtain the total diterpene alkaloid.
Claims (6)
1. the alkaloidal preparation method of Delphinium plant total diterpene is characterized in that may further comprise the steps:
(1) extract: the Delphinium plant is ground into coarse powder, places alkali liquor to soak 2-8 hour, filter, remove alkali liquor, filtering residue ethanol heating extraction obtains alcohol extract;
(2) enrichment: with alcohol extract reclaim under reduced pressure reagent, obtain total alkali extractum, add aqueous dispersion, cross the good macroporous resin column of pretreatment, wash with aqueous alkali earlier, the reuse deionized water is eluted to neutrality, discard eluent, use 60-95% ethanol water eluting at last, collect eluent;
(3) decolouring: eluent by the D941 macroporous resin column, is collected effluent, and reuse 4-7 times column volume 90% ethanol elution merges eluent and effluent, and concentrating under reduced pressure, drying obtain the total diterpene alkaloid.
2. preparation method as claimed in claim 1 is characterized in that: the solid-liquid ratio of raw material and alkali liquor is 1 in the described step (1): 6-26 (kg/L).
3. preparation method as claimed in claim 1 is characterized in that: alkali liquor is 0.1-15% sodium hydroxide solution, potassium hydroxide solution, ammonia or aqua calcis in the described step (1), and soaking temperature is 10-80 ℃.
4. preparation method as claimed in claim 1 is characterized in that: concentration of alcohol is 60-100% in the described step (1), and extracting temperature is 65-90 ℃, and extraction time is 1-4 hour, and extraction time is 2-4 time.
5. preparation method as claimed in claim 1 is characterized in that: selecting macroporous resin in the described step (2) for use is AB-8, D101, HPD100, D201 or D130 type macroporous resin.
6. preparation method as claimed in claim 1 is characterized in that: alkali liquor is the alkali liquor of pH7.5-13 in the described step (2), the optional ammonia of alkali liquor, sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, ammonium carbonate or ammonium bicarbonate.
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| CN2011101517399A CN102274302A (en) | 2011-06-07 | 2011-06-07 | Preparation method of delphinium total diterpenoid alkaloids |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961456A (en) * | 2012-10-26 | 2013-03-13 | 西安文理学院 | Preparation method and application of tsinling larkspur root extractive |
| CN108690023A (en) * | 2018-07-03 | 2018-10-23 | 中国科学院新疆理化技术研究所 | Diterpenoid Alkaloids compound and preparation method and purposes in a kind of delphinium of match Tacheng |
-
2011
- 2011-06-07 CN CN2011101517399A patent/CN102274302A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102961456A (en) * | 2012-10-26 | 2013-03-13 | 西安文理学院 | Preparation method and application of tsinling larkspur root extractive |
| CN108690023A (en) * | 2018-07-03 | 2018-10-23 | 中国科学院新疆理化技术研究所 | Diterpenoid Alkaloids compound and preparation method and purposes in a kind of delphinium of match Tacheng |
| CN108690023B (en) * | 2018-07-03 | 2020-11-13 | 中国科学院新疆理化技术研究所 | Diterpene alkaloid compound in Setatarian delphinium flower and preparation method and application thereof |
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