CN103951650A - Method for extracting and purifying nicotine by using polyethylene glycol (PEG)-disodium hydrogen phosphate aqueous two-phase system - Google Patents
Method for extracting and purifying nicotine by using polyethylene glycol (PEG)-disodium hydrogen phosphate aqueous two-phase system Download PDFInfo
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- CN103951650A CN103951650A CN201410213648.7A CN201410213648A CN103951650A CN 103951650 A CN103951650 A CN 103951650A CN 201410213648 A CN201410213648 A CN 201410213648A CN 103951650 A CN103951650 A CN 103951650A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D401/00—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom
- C07D401/02—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings
- C07D401/04—Heterocyclic compounds containing two or more hetero rings, having nitrogen atoms as the only ring hetero atoms, at least one ring being a six-membered ring with only one nitrogen atom containing two hetero rings directly linked by a ring-member-to-ring-member bond
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Abstract
The invention discloses a method for extracting and purifying nicotine by using a polyethylene glycol (PEG)-disodium hydrogen phosphate aqueous two-phase system. The method comprises the steps of putting 2.8-3.2g of PEG2000 and 1.8-2.2g of disodium hydrogen phosphate into a container, adding 2-4ml of deionized water, shaking out, adding a nicotine solution to be extracted and purified, then adding deionized water again until the total weight reaches 8-12g, shaking out for 3-7 minutes, putting into a water bath kettle at 35-45 DEG C, standing, and separating nicotine in an upper phase after stably layering. The method disclosed by the invention is used for separating and purifying nicotine by adopting the PEG-disodium hydrogen phosphate aqueous two-phase system, and screening and optimizing the process conditions of aqueous two-phase extraction, has the advantages of easy phase splitting, cheap price, efficient and mild extraction, no toxicity, small activity loss of extracts and the like, and is a green process; meanwhile, an aqueous two phase disclosed by the invention has relatively strong selectivity to nicotine, is high in degree of enrichment, and has relatively strong practical values.
Description
Technical field
The present invention relates to a kind of method that adopts polyethylene glycol-phosphorus acid disodium hydrogen double-aqueous phase system to extract purifying nicotine.
Background technology
Nicotine (Nicotine) claim again Nicotine, is mainly present in tobacco leaf, is a kind of natural alkaloid, content accounts for 95% of nicotiana alkaloids total amount, accounts for the 0.50-6.0% of tobacco dry weight, and highly purified nicotine is as the additive of tobacco industry, can improve cigarette quality, make cigarette surrogate.Agriculturally, nicotine derives from nature, noresidue, the solution of containing nicotine sulfate can prevent and treat field crop produce in the crop pest such as aphid.Nicotine series pesticide platymiscium sterilant, have steam smoke, the feature of stomach toxicity, the function of tagging and the noresidue of degrading rapidly, be widely used as the sterilant of the farm crop such as grain, oil plant, vegetables, fruit, herbage, be desirable efficient green sterilant and biological agricultural chemicals, meet the requirement of pollution-free food production.In addition, the compound fertilizer efficiency that increases of nicotine and fertilizer, reduces the loss of ammonium nitrogen.Aspect medical, a small amount of nicotine can stimulate human central nervous system, makes people's ataraxy and anti-melancholy effect, and people's intense strain is had to mitigation; The synthetic nicotinic acid of nicotine is often applied to medicine, can effectively treat Alzheimer and parkinsonism; Highly purified nicotine also can be used as the extraordinary raw material of the illness medicines such as health cigarette, smoking cessation cream, treatment arthralgia, muscle spasm externally applied agent, development treatment cardiovascular diseases, tetter, snake bite and insect sting; Nicotine is also for the production of senior edible or feeding protein tobacco, medicines and health protection functional protein etc.Aspect chemical industry, nicotine is important industrial chemicals, through techniques such as oxidation alcoholization, can prepare nicotinic acid and series derivates-niacinamide thereof, cigarette creatine, Tonostan, nicotinic acid tocopherol etc.Therefore, extract purifying nicotine and there is very high economic worth and meaning.
Nicotine is after reported first in 1809, and separated smoke alkali in 1828 are also purified, and measure the structure of nicotine and synthesize for 19 end of the centurys.More for the separating and purifying method research of nicotine at present, mainly contain following several method: steam distillation, finger is by the material that contains volatile component and water condistillation, volatile component is distillated in the lump with water vapour, divide the leach extraction method of getting volatile component through condensation, this is the most ancient method, cost is low, output is large, but amount of energy consumption is large, technique is long, and the tobacco leaf of alkaline purification is difficult to process, also higher to equipment requirements.Ion exchange method, to electing property of nicotine aqueous solution absorption, then desorption obtains product, but wash-out concentration is still very low, and the pre-treatment of ion exchange resin and regeneration comparatively loaded down with trivial details.Solvent extration can extract the many kinds of substance in tobacco leaf, water soluble protein, chlorophyll, nicotine etc. simultaneously, and white fiber shape residue can be used to production safety type cigarette, industrially developed country is mainly used in before production of cigarettes, and this method is suitable for fairly large production, but solvent loss is larger.Emulsion liquid membrane, emulsion liquid membrane technology is a kind of novel chemical separating method, this technology is by the fine Interfacial Liquid Membranes mass transfer of high dispersing, has that mass transfer velocity is fast, selectivity strong, extraction has been synchronizeed with reextraction, energy consumption is low and pollute the features such as little.Microwave method, ultrasonic extraction and emerging technique supercritical extraction technique, these techniques have the shortcomings such as seriously polluted, energy consumption is high, cost is high, product purity is low.Therefore, a kind of method of efficient, safety, extraction nicotine that energy consumption is low shows for particularly important.
Along with improving constantly and the extensive expansion of high-new isolation technique research work of environmental requirement, traditional liquid-liquid extraction can not adapt to separation requirement, therefore a kind of novel liquid liquid isolation technique-aqueous two phase extraction technique (two-aqueous phaseextraction, ATPE) is arisen at the historic moment.Double-aqueous phase system is during by the aqueous solution of two kinds of different water-soluble polymerss, and when polymer concentration reaches certain value, system can naturally be divided into immiscible two-phase, Here it is double-aqueous phase system.The formation of double-aqueous phase system is mainly that the steric restriction effect of high-polymer molecular, cannot permeate mutually, can not form homogeneous phase due to the immiscible property between superpolymer, thereby has separated tendency, can be divided into two-phase under certain condition.Aqueous two-phase extraction is similar to the principle of water-organic extractant phase, is all to distribute in two alternate selectivity according to material, but the different in kind of extraction system.When material enters after double-aqueous phase system, due to the existence of surface properties, charge effect and various power (as hydrophobic key, hydrogen bond and ionic linkage etc.) and the impact of environment, make them different in upper and lower concentration in mutually.For a certain material, as long as select suitable double-aqueous phase system, control certain condition, just can obtain suitable partition ratio, thereby reach the object of separation and purification.Because Bi-aqueous extraction process condition is gentle, adjustable factor is many, volume is little, processing power is strong, become the phase time short, the rate of recovery is high, energy consumption is low, extraction aftertreatment is easy, facility investment expense is few, be easy to amplification and operation, and can be by correlation theory and the experience of conventional solvent extraction, there is not toxic organic solvent residue problem, be specially adapted to the separated of biological substance and purify.ATPE technology starts from the 60's of 20th century, from the Albertsson of Runde, Sweden university in 1956, find that the people such as Kula of double-aqueous phase system to 1979 year German GBF are applied to biological product separation by Bi-aqueous extraction technology, for later double water-phase is laid a good foundation at applying biological protein, enzyme purification.At present, ATPE technology is successfully applied to the separation and purification of the materials such as protein, nucleic acid and virus, natural product, metal ion.Domesticly from the 80's of 20th century, also carried out ATPE technical study.ATPE method can retain the activity of product, whole operation can serialization, when removing cell or cell debris, and can also protein purification 2～5 times, remove cell debris with traditional filtration method and centrifuging and compare, on yield or all more advantageous on cost.Add China as tobacco big producing country, yield of tobacco 450 ~ 5,000,000 ton/year, but wherein the tankage such as approximately nearly 25% tobacco leaf, offal go out of use.These wastes not only can cause contaminate environment, increase the load of ecotope, also can make in tobacco leaf high added value compound waste as active skull cap components such as nicotine, Salanesols, and they can be used as greatly the abundant source of extracting natural nicotine.Therefore, from inferior tobacco, extract the common concern that natural nicotine has been subject to people.
< < research and development of natural products > > 12 phases in 2012, Liu Baoliang, Cao Guiping and Zhang Jintao have delivered exercise question for " double water-phase extracts the research of Salanesol and nicotine in a hypo-tobacco leaf " literary composition simultaneously, it is that acetone-dipotassium hydrogen phosphate double-aqueous phase system extracts research to Salanesol and nicotine that this article adopts novel double-aqueous phase system, though research obtains certain breakthrough, but also used this poisonous organic solvent of acetone, and exist extraction yield lower, the defect that industrialization value is little.
Summary of the invention
The deficiency existing for solving the prior art of said extracted purifying nicotine, the inventor, through a large amount of scientific practices, invents the method that polyethylene glycol-phosphorus acid disodium hydrogen double-aqueous phase system extracts purifying nicotine finally.
Technical scheme of the present invention is: 2.8-3.2gPEG2000 and 1.8-2.2g Sodium phosphate dibasic are put into container, add the nicotine solution that adds purifying to be extracted after the jolting of 2-4ml deionized water, add again deionized water ad pond om 8-12g, jolting 3-7min, put into 35-45 ℃ of water-bath standing, after layering is stable, the nicotine in isolating mutually and get final product.
After double-aqueous phase system of the present invention is set up, the upper nicotine containing in mutually accounts for the 80-95% of whole nicotine, and selectivity is very strong, upper mutually in the purity 70-90% of nicotine.
The present invention is the double-aqueous phase system separation and purification nicotine that adopts polyoxyethylene glycol and Sodium phosphate dibasic, and screening and optimized the processing condition that double water-phase extracts, compared with prior art, the invention has the beneficial effects as follows: present method has easy phase-splitting, cheap, extracting efficient is gentle, nontoxic, to advantages such as extract loss of activity are little, be a kind of friendly process; Meanwhile, after double-aqueous phase system of the present invention forms, the upper nicotine containing in mutually accounts for the 80-95% of whole nicotine, and selectivity is very strong, upper mutually in the purity 70-90% of nicotine, possess stronger practical value.
Embodiment
Below the method for polyethylene glycol-phosphorus acid disodium hydrogen double-aqueous phase system extraction purifying nicotine is elaborated.
embodiment 1:
2.9gPEG2000 and 1.9 g Sodium phosphate dibasics are put into container, add the nicotine solution that adds purifying to be extracted after the jolting of 2.7ml deionized water, add again deionized water ad pond om 8.8g, jolting 4min, put into 37 ℃ of water-baths standing, after layering is stable, the nicotine in isolating mutually and get final product.
After double-aqueous phase system of the present invention is set up, the upper nicotine containing in mutually accounts for 83% of whole nicotine, and selectivity is very strong, in separation mutually in nicotine, purity reaches 73%.
embodiment 2:
3.1gPEG2000 and 2.15g Sodium phosphate dibasic are put into container, add the nicotine solution that adds purifying to be extracted after the jolting of 3.9ml deionized water, add again deionized water ad pond om 11.3g, jolting 6.5min, put into 42 ℃ of water-baths standing, after layering is stable, the nicotine in isolating mutually and get final product.
After double-aqueous phase system of the present invention is set up, the upper nicotine distributing in mutually accounts for 91% of whole nicotine, and selectivity is very strong, in separation mutually in nicotine, purity 86%.
Above-described embodiment is not done any pro forma restriction to the present invention, any those of ordinary skill in the art, in the situation that not departing from technical solution of the present invention scope, all can utilize the technology contents of above-mentioned announcement to make many possible changes and modification to technical solution of the present invention, or be revised as the equivalent embodiment of equivalent variations.Therefore, every content that does not depart from technical solution of the present invention,, all should drop in the scope of technical solution of the present invention protection any simple modification made for any of the above embodiments, equivalent variations and modification according to the technology of the present invention essence.
Claims (1)
1. polyethylene glycol-phosphorus acid disodium hydrogen double-aqueous phase system extracts the method for purifying nicotine, it is characterized in that: 2.8-3.2gPEG2000 and 1.8-2.2g Sodium phosphate dibasic are put into container, add the nicotine solution that adds purifying to be extracted after the jolting of 2-4ml deionized water, add again deionized water ad pond om 8-12g, jolting 3-7min, put into 35-45 ℃ of water-bath standing, after layering is stable, the nicotine in isolating mutually and get final product.
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| CN201410213648.7A CN103951650A (en) | 2014-05-21 | 2014-05-21 | Method for extracting and purifying nicotine by using polyethylene glycol (PEG)-disodium hydrogen phosphate aqueous two-phase system |
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| CN201410213648.7A CN103951650A (en) | 2014-05-21 | 2014-05-21 | Method for extracting and purifying nicotine by using polyethylene glycol (PEG)-disodium hydrogen phosphate aqueous two-phase system |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880019A (en) * | 2017-11-13 | 2018-04-06 | 李辉 | The preparation method and application of ionic liquid sodium hydrogen phosphate buffer double-aqueous phase system |
| CN115594663A (en) * | 2022-10-25 | 2023-01-13 | 云南中烟工业有限责任公司（Cn） | Continuous extraction and purification method of nicotine |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050212A (en) * | 2007-05-18 | 2007-10-10 | 中南大学 | Method for extracting high pure natural nicotine and solanesol at same time from waste and low-grade tobacco |
-
2014
- 2014-05-21 CN CN201410213648.7A patent/CN103951650A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101050212A (en) * | 2007-05-18 | 2007-10-10 | 中南大学 | Method for extracting high pure natural nicotine and solanesol at same time from waste and low-grade tobacco |
Non-Patent Citations (3)
| Title |
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| 刘宝亮 等: "PEG 6000/(NH4)2SO4 双水相同时提取烟叶中茄尼醇和烟碱的研究", 《化工技术与开发》 * |
| 刘宝亮 等: "双水相同时提取次烟叶中茄尼醇和烟碱的研究", 《天然产物研究与开发》 * |
| 邢健敏 等: "双水相体系/溶剂反萃取法制备高纯天然烟碱", 《天然产物研究与开发》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107880019A (en) * | 2017-11-13 | 2018-04-06 | 李辉 | The preparation method and application of ionic liquid sodium hydrogen phosphate buffer double-aqueous phase system |
| CN115594663A (en) * | 2022-10-25 | 2023-01-13 | 云南中烟工业有限责任公司（Cn） | Continuous extraction and purification method of nicotine |
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Application publication date: 20140730 |