CN102228523A - Preparation method of total diterpenoid alkaloids from Delphinium Staphisagria - Google Patents
Preparation method of total diterpenoid alkaloids from Delphinium Staphisagria Download PDFInfo
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- CN102228523A CN102228523A CN2011101517666A CN201110151766A CN102228523A CN 102228523 A CN102228523 A CN 102228523A CN 2011101517666 A CN2011101517666 A CN 2011101517666A CN 201110151766 A CN201110151766 A CN 201110151766A CN 102228523 A CN102228523 A CN 102228523A
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Abstract
The invention discloses a preparation method of total diterpenoid alkaloids from Delphinium Staphisagria, belonging to the technical field of natural active ingredient preparation. The preparation method comprises the following steps of: soaking Delphinium Staphisagria medicinal material in lye, then extracting with ethanol, allowing the extracting solution to flow past a macroporous resin column, firstly eluting with lye, then eluting with an ethanol solution, decolorizing the eluate with a D942 decolorizing resin column, concentrating and drying to obtain the total diterpenoid alkaloids. The preparation method has the characteristics that, during the whole extraction and separation process, only lye and ethanol are used, other toxic organic solvents are not used, the macroporous resin can be reused, the industrial production is safe, the cost is low and the prepared total diterpenoid alkaloids from Delphinium Staphisagria has high purity.
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.1eiocarpum), 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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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112244042A (en) * | 2020-10-09 | 2021-01-22 | 华南农业大学 | Application of herba delphinii or extract thereof in preventing and treating sisalana ananas comosus |
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2011
- 2011-06-07 CN CN2011101517666A patent/CN102228523A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112244042A (en) * | 2020-10-09 | 2021-01-22 | 华南农业大学 | Application of herba delphinii or extract thereof in preventing and treating sisalana ananas comosus |
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Application publication date: 20111102 |