CN100571548C - A kind of method of controlling nicotine content in the tobacco leaf - Google Patents
A kind of method of controlling nicotine content in the tobacco leaf Download PDFInfo
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- CN100571548C CN100571548C CNB2006100863868A CN200610086386A CN100571548C CN 100571548 C CN100571548 C CN 100571548C CN B2006100863868 A CNB2006100863868 A CN B2006100863868A CN 200610086386 A CN200610086386 A CN 200610086386A CN 100571548 C CN100571548 C CN 100571548C
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Abstract
A kind of method of controlling nicotine content in the tobacco leaf is at first used the water-wet tobacco leaf, uses supercritical CO then
2In 15～20MPa, extracted 1～2 hour under 45～65 ℃ of conditions.This method can realize the nicotine in the tobacco leaf is carried out the gradient extraction, obtains the serial tobacco leaf of nicotine content distribution gradient.With this tobacco leaf is the serial cigarette that raw material can be processed different nicotine content in smoke, has both alleviated harm of smoking, can satisfy the needs of different regions and different smoking populations again.
Description
One, technical field:
But the present invention relates to the method for active component in a kind of gradient extraction plant, exactly is with the method for supercritical fluid gradient extraction with nicotine content in the control tobacco leaf.
Two, background technology:
Nicotine (nicotine) has another name called nicotine, is a kind of pyridine type alkaloid, is present in the Nicotiana economic plants.Nicotine at room temperature is colourless or light bronze-colored oily liquids, and pure product are colourless oil liquid, contacts with air to become pale brown look very soon, and strong impulse is arranged, and it is pungent to distinguish the flavor of.
Nicotine has severe toxicity, enters in the human body, and 90% absorbs in lung, enter blood after 6 seconds can arrive brain.On a small quantity nervous centralis is had excitation, the blood pressure that can raise then suppresses central nervous system in a large number, makes the heart paralysis so that dead.Several milligrams nicotine just can cause headache, vomiting, poisoning symptom such as clouding of consciousness.
Nicotine is important physical active material in the cigarette smoke, also is a leading indicator of cigarette.The sign that nicotine content in smoke is usually arranged on cigarette case mostly, as 1.3mg, 1.4mg etc., alleged this " lightly seasoned ", those " highly seasoned " of smoker are closely related with this index.The smoker can regulate soakage automatically to satisfy its needs.
Harm of smoking is common people's common recognition.The nicotine amount that reduces in the flue gas is one of approach that reduces its harm.But if transition reduces, even be zero, then will lose the use value of cigarette, embarrass the smoker to accept.Yet, the domestic and international at present safety standard of all not having nicotine content in smoke.In the case, with minimum nicotine content in smoke (1.3mg) in the market is reference, reduce to below the 1.0mg it and distribution gradient, the serial cigarette that is to say the different nicotine content in smoke of production distribution gradient one of the effective ways that reduce harmfulness of smoking of can yet be regarded as have also satisfied the needs of different regions, different smoking populations simultaneously.
Nicotine in the flue gas is from raw tobacco.Nicotine content is relatively-stationary in the tobacco leaf in the same place of production, and its nicotine content has difference in the tobacco leaf of the different places of production, different brackets, but is not very big.The serial cigarette that is difficult to process the nicotine content in smoke of different gradients with such raw material.Therefore be necessary nicotine content in the tobacco leaf is controlled.
Three, summary of the invention:
The experimental study that the present invention carries out under above-mentioned thinking instructs just is intended to reduce nicotine content in the tobacco leaf, even make tobacco leaf form series with its nicotine content distribution gradient of a kind of tobacco leaf.Technical problem to be solved is not only the reduction nicotine content, and importantly this reduction process can be regulated and control, and can control in other words.
Technical scheme of the present invention is to use supercritical CO
2Extraction nicotine is realized the gradient extraction to reduce the content of nicotine in the tobacco leaf by the control to extraction, separating technology condition.Difference with the prior art is at first to have used the water of entrainer effect that tobacco leaf is soaked into to make it wetting, makes that water content reaches certain level in the tobacco leaf, improves the free degree of nicotine, with the efficient that promotes that follow-up supercritical fluid extraction separates.Concrete process conditions:
1., infiltration reagent is water, its consumption is 15～30wt% of tobacco leaf weight, infiltrating time 1.5～2.5h, 45～65 ℃ of infiltration temperatures; Preferred 50～60 ℃;
2., extracting pressure 15～20MPa, extraction temperature is 45～65 ℃, preferred 50～60 ℃, extraction time 1～2h; Separating pressure 3～5MPa, separation temperature is 20～30 ℃.
When using supercritical CO
2Extraction is during polar component, to add usually have certain polarity entrainer to improve extraction efficiency.Nicotine has polarity, and water plays entrainer in this application, but is not by supercritical CO
2Carry secretly and enter extraction kettle, make tobacco leaf wetting under certain conditions, variation has taken place through so handling the character that other active components that can be extracted extract in back nicotine and the tobacco leaf but mix with tobacco leaf.
Think CO in theory
2During as solvent, different material is different solubility therein, and with temperature and pressure two factors of system direct relation is arranged.In general, along with the rising of extracting pressure, nicotine solubility in solvent is big more, and the solubility of other active material is also big more in the tobacco, cause take off nicotine after product quality also poor more.But, the present invention finds: by in advance to tobacco leaf carry out wetting after, at pressure is 15～20MPa, in temperature 45-65 ℃ the scope, nicotine is to the variation sensitivity and the positive correlation of pressure, and insensitive to variation of temperature, the ability that is extracted of other active components then descends and obviously descends with temperature on the contrary, so the present invention by adjusting extracting pressure and temperature, under the situation that does not influence quality of tobacco, realizes the gradient extraction to nicotine in the tobacco leaf.
In order to improve the comprehensive utilization value of tobacco leaf, from separating still, obtain the nicotine crude product and can carry out separation and purification, to improve the purity of nicotine, be used to develop biological pesticide.
Four, the specific embodiment:
Now the natural tobacco leaf that is about 4.87mg/g with nicotine content is a raw material, and non-limiting examples is described below:
Method of operating:
Earlier dry tobacco leaf is sprayed distilled water, then be placed on airtight temperature control and in 50～60 ℃ of containers, soak into 2h; Between infiltration stage, can connect overcritical device power supply (DPS), restart the temperature controlled water bath switch, to equipment preheating 30min; To soak into back raw tobacco material weighing afterwards and drop in the extraction kettle, close the extraction kettle capping, open CO again
2Gas cylinder when extraction kettle, when separating still arrives required temperature, is opened diaphragm type compressor and is also controlled CO
2Flow velocity makes extraction kettle, separating still reach required pressure respectively, opens pressure regulator valve and begins cycling extraction, closes CO simultaneously
2Gas cylinder is regulated pressure regulator valve at any time and is made extraction kettle, separating still keep the constant compression force cycling extraction.When extraction reaches seclected time, shut down, open extraction kettle, can obtain the low nicotine tobacco leaf, open the separating still bleeder valve, promptly get the nicotine crude product.
1, with the raw tobacco material of drying, take by weighing 1kg after the chopping and spray, be placed into airtight temperature control again and in 50～60 ℃ of containers, soaked into 2 hours; Drop into again in the extraction kettle of overcritical device, begin after material installs extraction kettle and extraction-container are carried out temperature control.When extraction temperature reaches 60 ℃, when the separating still temperature reaches 20 ℃, begin to pour CO
2And pressurization, when extraction kettle pressure reaches 15MPa and separating still pressure and reaches 3MPa, open pressure regulator valve and begin extraction, and the control by pressure regulator valve, CO
2Flow velocity 10L/min keeps above parameter constant, behind the extraction 90min, shuts down discharging and obtains 991 gram dry tobacco leafs.The HPLC method detects, in the dry tobacco leaf in the 1g tobacco leaf content of nicotine be 1.80mg.
2, with the raw tobacco material of drying, take by weighing 1kg after the chopping and spray, be placed into airtight temperature control again and in 50～60 ℃ of containers, soaked into 2 hours; Drop into again in the extraction kettle of overcritical device, begin after material installs extraction kettle and extraction-container are carried out temperature control.When extraction temperature reaches 65 ℃, when the separating still temperature reaches 20 ℃, begin to pour CO
2And pressurization, when extraction kettle pressure reaches 15MPa and separating still pressure and reaches 4MPa, open pressure regulator valve and begin extraction, and the control by pressure regulator valve, CO
2Flow velocity 10L/min keeps above parameter constant, behind the extraction 90min, shuts down discharging and obtains 984 gram dry tobacco leafs, and the HPLC method detects, in the dry tobacco leaf in the 1g tobacco leaf content of nicotine be 1.76mg.
3, with the raw tobacco material of drying, take by weighing 1kg after the chopping and spray, be placed into airtight temperature control again and in 50～60 ℃ of containers, soaked into 2 hours; Drop into again in the extraction kettle of overcritical device, begin after material installs extraction kettle and extraction-container are carried out temperature control.When extraction temperature reaches 60 ℃, when the separating still temperature reaches 20 ℃, begin to pour CO
2And pressurization, when extraction kettle pressure reaches 20MPa and separating still pressure and reaches 5MPa, open pressure regulator valve and begin extraction, and the control by pressure regulator valve, CO
2Flow velocity 10L/min keeps above parameter constant, behind the extraction 60min, shuts down discharging and obtains 960 gram dry tobacco leafs, and the HPLC method detects, in the dry tobacco leaf in the 1g tobacco leaf content of nicotine be 1.37mg.
4, with the raw tobacco material of drying, take by weighing 1kg after the chopping and spray, be placed into airtight temperature control again and in 50～60 ℃ of containers, soaked into 2 hours; Drop into again in the extraction kettle of overcritical device, begin after material installs extraction kettle and extraction-container are carried out temperature control.When extraction temperature reaches 65 ℃, when the separating still temperature reaches 20 ℃, begin to pour CO
2And pressurization, when extraction kettle pressure reaches 20MPa and separating still pressure and reaches 4MPa, open pressure regulator valve and begin extraction, and the control by pressure regulator valve, CO
2Flow velocity 10L/min keeps above parameter constant, behind the extraction 60min, shuts down discharging and obtains 955 gram dry tobacco leafs, and the HPLC method detects, in the dry tobacco leaf in the 1g tobacco leaf content of nicotine be 1.28mg.
5, with the raw tobacco material of drying, take by weighing 1kg after the chopping and spray, be placed into airtight temperature control again and in 55 ℃ of containers, soaked into 2 hours; Drop into again in the extraction kettle of overcritical device, begin after material installs extraction kettle and extraction-container are carried out temperature control.When extraction temperature reaches 65 ℃, when the separating still temperature reaches 20 ℃, begin to pour CO
2And pressurization, when extraction kettle pressure reaches 20MPa and separating still pressure and reaches 5MPa, open pressure regulator valve and begin extraction, and the control by pressure regulator valve, CO
2Flow velocity 10L/min keeps above parameter constant, behind the extraction 90min, shuts down discharging and obtains 941 gram dry tobacco leafs, and the HPLC method detects, in the dry tobacco leaf in the 1g tobacco leaf content of nicotine be 1.12mg.
Claims (2)
1, a kind of method of controlling nicotine content in the tobacco leaf comprises wetting, extraction and separates, and it is characterized in that: described wetting be exactly that water with 15～30wt% soaked into tobacco leaf 1.5～2.5 hours under 45～65 ℃ of conditions; Use supercritical CO then
2Extract and separate extracting pressure 15～20MPa, 45～65 ℃ of extraction temperature, 1～2 hour extraction time; Separating pressure 3～5MPa, 20～30 ℃ of separation temperatures.
2, method according to claim 1 is characterized in that: infiltration temperature is 50～60 ℃, and extraction temperature is 50～60 ℃.
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| CNB2006100863868A CN100571548C (en) | 2006-07-11 | 2006-07-11 | A kind of method of controlling nicotine content in the tobacco leaf |
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| CNB2006100863868A CN100571548C (en) | 2006-07-11 | 2006-07-11 | A kind of method of controlling nicotine content in the tobacco leaf |
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| CN100571548C true CN100571548C (en) | 2009-12-23 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB201003887D0 (en) | 2010-03-09 | 2010-05-12 | British American Tobacco Co | Methods for extracting and isolating constituents of cellulosic material |
| GB201707758D0 (en) | 2017-05-15 | 2017-06-28 | British American Tobacco Investments Ltd | Ground tobacco composition |
| CN107149161B (en) * | 2017-07-20 | 2018-07-10 | 安徽中烟工业有限责任公司 | A kind of low nicotine tobacco extract and preparation method thereof |
| CN110946318A (en) * | 2018-09-26 | 2020-04-03 | 浙江中烟工业有限责任公司 | Preparation method of natural nicotine for electronic cigarette |
| CN109275947B (en) * | 2018-10-08 | 2021-10-15 | 浙江中烟工业有限责任公司 | Supercritical extraction treatment method suitable for tobacco shreds in heating and non-combustion state |
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