CN102241565A - Method for synchronously extracting solanesol and nicotine from tobacco - Google Patents
Method for synchronously extracting solanesol and nicotine from tobacco Download PDFInfo
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- CN102241565A CN102241565A CN2011101133435A CN201110113343A CN102241565A CN 102241565 A CN102241565 A CN 102241565A CN 2011101133435 A CN2011101133435 A CN 2011101133435A CN 201110113343 A CN201110113343 A CN 201110113343A CN 102241565 A CN102241565 A CN 102241565A
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- nicotine
- normal hexane
- buddhist nun
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Abstract
The invention relates to the field of natural product chemistry, in particular to a method for synchronously extracting solanesol and nicotine from tobacco. The method for extracting solanesol and nicotine from tobacco leaves adopts a technical process which comprises: mixing crushed tobacco leaves with 0.5-to-4-percent solution of sodium hydroxide according to a mass ratio ranging from 1:4 to 1:15; adding normal hexane or solvent oil No6 according to a normal hexane or solvent oil No6 to solution of sodium hydroxide ratio ranging from 1:0.6 to 1:2; and performing refluxing extraction for 1 to 3 hours, stopping heating, filtering cloth by using 100-to-200 mesh filter cloth, standing the filtrate, demixing, separating out an upper normal hexane or solvent oil No6 phase, extracting by using 2-to-12-percent hydrochloric acid, concentrating the normal hexane or solvent oil No6 phase into paste which is crude extract of solanesol and collecting a water phase which is solution of coarse nicotine hydrochloride.
Description
Technical field:
The present invention relates to the natural product chemistry field, particularly relate to a kind of from tobacco the method for the pure and mild nicotine of simultaneous extraction eggplant Buddhist nun.
Background technology:
At industrial eggplant Buddhist nun alcohol is synthesizing coenzyme Q
10And vitamin K
2Essential raw material.Ubiquinone
10Be the natural antioxidants that cell self produces, the activator of cellular metabolism can improve organic immunizing power.Studies show that in recent years, ubiquinone
10Aspect the treatment cardiovascular disorder unique curative effect is being arranged, aspect treatment vitamin C deficiency, duodenal ulcer and stomach ulcer, gangrenosum acne periodontitis, the viral hepatitis significant curative effect is being arranged, the experimentation on animals result shows ubiquinone
10Have antitumor action, being used to clinically cure changes acute cancer patients late period certain curative effect, ubiquinone is arranged
10Tablet is used for the treatment of circular baldness effectively, and pulmonary emphysema also have certain curative effect to the treatment of dysacousis, and find more that recently it has significant auxiliary curative effect to acquired immune deficiency syndrome (AIDS).Therefore as ubiquinone
10Extraction, the purifying of eggplant Buddhist nun alcohol that must synthesis material also more and more cause people's attention.The content of eggplant Buddhist nun alcohol in tobacco leaf was separated (J.Am.Chem.Soc., 1956,78,4780) by people such as R.L.Rowland the earliest from flue-cured tobacco in 1956 about about 0.5～3%.
Nicotine is a kind of alkaloid in the tobacco leaf, is colourless, liquid with no taste, can be miscible arbitrarily when being lower than 60 ℃ with water, very easily be dissolved in organic solvents such as alcohol, ether, chloroform, sherwood oil.Nicotine can generate crystalline list salt or two salt with various mineral acids and organic acid, and mainly the form with organic acid salt exists in tobacco leaf.Nicotine has severe toxicity, on a small quantity nervus centralis is had excitation, can suppress central nervous system when maximum, makes the heart paralysis, so that dead.Natural nicotine is used very extensive, and its purposes mainly comprises agricultural chemicals and medical two broad aspect.Nicotine series pesticide platymiscium sterilant, have steam smoke, the characteristics of stomach toxicity, the function of tagging and the noresidue of degrading rapidly, being widely used as the sterilant of farm crop such as grain, oil plant, vegetables, fruit, herbage, is ideal efficient green sterilant and biological agricultural chemicals.The nicotine sulfate of nicotine content 40% is good contact insecticide, can make different preparations according to different needs, is used to prevent that effects such as aphid, leaf roller are good.Not only prevention effect is good to cotten aphid by the aphid fourth emulsion of getting killed of nicotine production, and has high selectivity.Nicotine combines with aminoacids complex, has the anti-plant pathogen effect.In addition, utilize the mating reaction of nicotine and transition metal, make the little fertilizer that contains nicotinic acid and trace element, have fertilizer and insecticidal action concurrently.Nicotine and derivative thereof all are important medical materials.Nicotine gets nicotinic acid through oxidation, and nicotinic acid is a member of vitamin B complex, can prepare to prevent pellagra and avitaminotic medicine.Nicotinic acid and ammonia react can get niacinamide, are used for the treatment of peripheral vessel spasm, arteriosclerosis etc.Also can make the Buddhist nun by nicotinic acid and can stop not (Ventramine), this medicine is the central excitation medicine, and is fine to pulmonary heart disease and the excessive respiration inhibition effect that causes of morphine.Nicotine and quinoline make Yi Yansuan through oxidation, get the vazadrine with the hydrazine hydrate condensation again.The vazadrine is efficient, low toxicity, inexpensive antitubercular agent.Nicotine also can be made into smoking cessation cream, and is evident in efficacy to the ES.In addition, high purity nicotine is to develop the extraordinary raw material of the medicine of illness such as treatment is cardiovascular, skin, snake bite and insect sting on the medicine industry.
At present for difference extraction separation eggplant Buddhist nun's alcohol or nicotine from tobacco; The existing bibliographical information of separating solanesol the residuum behind extraction nicotine.
The patent of application number CN200610041915.2 discloses a kind of method of extraction of high purity solanesol alcohol, utilizes supercritical CO
2The high efficiency separation and purification method of fluid extraction and column chromatography associating, with inferior tobacco as raw material, extraction of high purity solanesol alcohol.Adopt the entrainment agent intensifying technology through pretreated tobacco leaf, through supercritical CO
2Fluid one-level extraction separates by secondary simultaneously, makes supercritical CO
2The fluidic extract is optionally separated out in two different extraction kettles, has realized that eggplant Buddhist nun alcohol enrichment and the first of extract separate.The saponification in the alcoholic solution of NaOH of the thick cream of eggplant Buddhist nun alcohol is handled the back and is adopted column chromatography to be further purified, and the elutriant of concentrating under reduced pressure enriched solanesol, its concentrated solution are through freezing and crystallizing and vacuum drying treatment, and eggplant Buddhist nun alcohol purity can reach more than 95%.
The patent of application number CN99105952.2 discloses a kind of nicotine extraction process, and tobacco leaf is used earlier the hot water lixiviate, successively adds Ca (OH) again in vat liquor
2And CO
2Neutralize, in and after-filtration, filtered liquid is that refining smoke succus extracts in packing tower with ethyl acetate or chloroform, the evaporation extraction phase to obtain containing the product of free nicotine 75～85%, the evaporation extracting phase is on good terms raffinate and is obtained recycle as lixiviate with hot water to reclaim extraction agent.
The patent of application number CN200710034942.1, the method of extracting natural nicotine and eggplant Buddhist nun alcohol from abandoned tobacco is disclosed: tobacco oven dry back is pulverized, adopt the mixed solution heating reflux method of second alcohol and water to extract, filter, get nicotine extracting solution and filter residue respectively, nicotine extracting solution vacuum concentration is got nicotine medicinal extract, and water-soluble back adds phase-splitting agent phase-splitting and gets nicotine products; Filter residue gets eggplant Buddhist nun alcohol product after treatment.
Hu Haichao, the first month of spring, Deng (extraction and purification of nicotine and eggplant Buddhist nun alcohol in the waste tobacco leaf. University of Fuzhou's journal, 2008,2:308-312) provide a kind of from waste tobacco leaf the technological line of comprehensively extracting and purifying nicotine and eggplant Buddhist nun alcohol: producing waste tobacco with Longyan, Fujian is raw material, elder generation's extraction nicotine through step process such as ion-exchange, stripping distillation, petroleum ether extraction, vacuum solvent recuperation, can obtain the nicotine of purity 98.2%; The tobacco leaf slag of collection after nicotine extracts is used for the extraction of eggplant Buddhist nun alcohol, and solanesol extract can obtain the eggplant Buddhist nun alcohol of purity 95.8% through saponification, column chromatography, crystallization, lyophilize.
In sum, the prior art utilization is extracted the pure and mild nicotine of eggplant Buddhist nun with a collection of tobacco material and is and successively carries out, can not simultaneous extraction, and operation is many, has increased production cost, has therefore designed patent of the present invention in order to realize the pure and mild nicotine simultaneous extraction of eggplant Buddhist nun.
Summary of the invention:
The objective of the invention is to overcome in the present production technique extract the pure and mild nicotine of eggplant Buddhist nun with a collection of tobacco material can not simultaneous extraction, the shortcoming that operation is many, and the operational path that from tobacco, extracts the pure and mild nicotine of eggplant Buddhist nun that design makes new advances.
The present invention is as a kind of method of extracting the pure and mild nicotine of eggplant Buddhist nun from tobacco leaf, its technical process is: tobacco leaf is pulverized back sodium hydroxide solution with 0.5%～4% mixed in 1: 4～1: 15 by mass ratio, then in adding normal hexane or No. 6 solvent oils with 1: 0.6～1: 2 ratio of sodium hydroxide solution quality, refluxing extraction 1～3 hour, stop heating, filter extract with 100～200 purpose filter clothes, behind the filtrate standing demix, tell upper strata normal hexane or No. 6 solvent oil phases, use 2～12% hcl as extraction agent then, normal hexane or No. 6 solvent oil phases are concentrated into and are paste, are eggplant Buddhist nun alcohol crude extract, and water is a crude salt acid fume alkaline solution.
The present invention has realized the simultaneous extraction of the pure and mild nicotine of eggplant Buddhist nun, and the existing method of resulting eggplant Buddhist nun alcohol crude extract use can obtain the eggplant Buddhist nun alcohol product more than 95%; Nicotine hydrochloride solution is through obtaining nicotine products transition.
Embodiment
The present invention is described further below by embodiment.
Embodiment one
Get 10 kilograms on tobacco leaf after the pulverizing, 150 kilograms of the sodium hydroxide solutions of adding 0.5% add 90 kilograms of normal hexanes, refluxing extraction 2 hours then, stop heating, filter extract with 100 purpose filter clothes, the filtrate standing demix is told upper strata normal hexane phase and lower floor's water, normal hexane is used 25 kilogram of 6% hcl as extraction agent mutually, the upper strata normal hexane is evaporated to mutually and is paste, and eggplant Buddhist nun alcohol content is 18.2% after measured, and water obtains nicotine hydrochloride solution.
Embodiment two
Get 10 kilograms on tobacco leaf after the pulverizing, 100 kilograms of the sodium hydroxide solutions of adding 2% add 100 kilograms of No. 6 solvent oils, refluxing extraction 1 hour then, stop heating, filter extract with 150 purpose filter clothes, the filtrate standing demix is told No. 6 solvent oil phases in upper strata and lower floor's water, No. 6 solvent oil phases are with 30 kilogram of 2% hcl as extraction agent, No. 6 solvent oils in upper strata are evaporated to mutually and are paste, and eggplant Buddhist nun alcohol content is 17.6% after measured, and water obtains nicotine hydrochloride solution.
Embodiment three
Get 10 kilograms on tobacco leaf after the pulverizing, 40 kilograms of the sodium hydroxide solutions of adding 4% add 80 kilograms of normal hexanes, refluxing extraction 3 hours then, stop heating, filter extract with 200 purpose filter clothes, the filtrate standing demix is told upper strata normal hexane phase and lower floor's water, normal hexane is used 20 kilogram of 12% hcl as extraction agent mutually, the upper strata normal hexane is evaporated to mutually and is paste, and eggplant Buddhist nun alcohol content is 17.3% after measured, and water obtains nicotine hydrochloride solution.
Claims (1)
1. method of from tobacco leaf, extracting the pure and mild nicotine of eggplant Buddhist nun, its technical process is: tobacco leaf is pulverized back sodium hydroxide solution with 0.5%～4% mixed in 1: 4～1: 15 by mass ratio, then in adding normal hexane or No. 6 solvent oils with 1: 0.6～1: 2 ratio of sodium hydroxide solution quality, refluxing extraction 1～3 hour, stop heating, filter extract with 100～200 purpose filter clothes, behind the filtrate standing demix, tell upper strata normal hexane or No. 6 solvent oil phases, use 2～12% hcl as extraction agent then, normal hexane or No. 6 solvent oil phases are concentrated into and are paste, are eggplant Buddhist nun alcohol crude extract, and water is a crude salt acid fume alkaline solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101133435A CN102241565A (en) | 2011-05-04 | 2011-05-04 | Method for synchronously extracting solanesol and nicotine from tobacco |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101133435A CN102241565A (en) | 2011-05-04 | 2011-05-04 | Method for synchronously extracting solanesol and nicotine from tobacco |
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| CN102241565A true CN102241565A (en) | 2011-11-16 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2011101133435A Pending CN102241565A (en) | 2011-05-04 | 2011-05-04 | Method for synchronously extracting solanesol and nicotine from tobacco |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104428421A (en) * | 2012-07-13 | 2015-03-18 | 亲切消费者有限公司 | Process for using tobacco |
| CN104606918A (en) * | 2015-01-21 | 2015-05-13 | 云南中海路德科技有限公司 | Comprehensive development and utilization method for tobacco stems in tobacco planting process |
| CN110903277A (en) * | 2018-09-18 | 2020-03-24 | 河南元萃生物科技有限公司 | Method for saponifying and hydrolyzing tobacco leaves by ultrasonic alkaline water and extracting nicotine by reduced pressure distillation |
| CN111777591A (en) * | 2020-07-16 | 2020-10-16 | 晨光生物科技集团股份有限公司 | Method for rapidly preparing nicotine crude product |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944425A (en) * | 2006-08-11 | 2007-04-11 | 三明华健生物工程有限公司 | High effective simultanuous clean extraction of high purity solanesol and nicotine |
-
2011
- 2011-05-04 CN CN2011101133435A patent/CN102241565A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944425A (en) * | 2006-08-11 | 2007-04-11 | 三明华健生物工程有限公司 | High effective simultanuous clean extraction of high purity solanesol and nicotine |
Non-Patent Citations (2)
| Title |
|---|
| 周新光等: "废弃烟草中茄尼醇和烟碱的提取", 《中国医药工业杂志》 * |
| 郑奎玲等: "从废次烟叶中同时提取茄尼醇和烟碱的实验", 《贵州师范大学学报（自然科学版）》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104428421A (en) * | 2012-07-13 | 2015-03-18 | 亲切消费者有限公司 | Process for using tobacco |
| CN104606918A (en) * | 2015-01-21 | 2015-05-13 | 云南中海路德科技有限公司 | Comprehensive development and utilization method for tobacco stems in tobacco planting process |
| CN104606918B (en) * | 2015-01-21 | 2016-02-10 | 云南中海路德科技有限公司 | The comprehensive development and utilization method of tobacco rod in tobacco leaf planting process |
| CN110903277A (en) * | 2018-09-18 | 2020-03-24 | 河南元萃生物科技有限公司 | Method for saponifying and hydrolyzing tobacco leaves by ultrasonic alkaline water and extracting nicotine by reduced pressure distillation |
| CN111777591A (en) * | 2020-07-16 | 2020-10-16 | 晨光生物科技集团股份有限公司 | Method for rapidly preparing nicotine crude product |
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