CN105146739B - The preparation method of a kind of mao of cigarette quintessence oil and application thereof - Google Patents
The preparation method of a kind of mao of cigarette quintessence oil and application thereof Download PDFInfo
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Abstract
A kind of preparation method of mao of cigarette quintessence oil, it is characterised in that: adopt subcritical abstraction and molecular distillation multiple techniques, carry out extracting and developing with hair cigarette for raw material, the content being effectively improved in quintessence oil Volatile infochemicals.Hair cigarette quintessence oil is applied in Medicated cigarette, flavouring essence quality and the mouthfeel of Medicated cigarette can be improved, improve the sense organ comfort level of Medicated cigarette；Hair cigarette quintessence oil is applied in tobacco juice for electronic smoke, this perfume of Nicotiana tabacum L. that electronic cigarette is strong can be given, strengthen gratification, reduce the sweet soapy feeling of solvent.The maximum of the present invention is characterized in that: (1), compared with vapor distillation, substantially increases the extraction ratio of quintessence oil；(2) subcritical abstraction and molecular distillation technique coupling, reduce the content of difficult volatilization macromolecular substances in quintessence oil, the content of volatile fragrance matter is improved, wherein the content relatively subcritical abstraction absolute oil of nicotine, solanone, neophytadiene, Megastigmatrienone, farnesyl acetone etc. is significantly improved so that the characteristic perfume of Nicotiana tabacum L. is more prominent.
Description
Technical field
The present invention relates to the extraction of natural plant essential oils and application, specifically the preparation method of a kind of mao of cigarette quintessence oil and application in Medicated cigarette and electronic cigarette thereof.
Background technology
Recently as the reduction of tar content in cigarette, it is thin out to there is smoke in low-coke tar cigarette, and fragrance weakens, and cigarette product style and features weakens, it is difficult to accepted by consumer.So while Jiao drops in Harm reduction techniques, Medicated cigarette flavouring and raising flue gas concentration are urgent problems.Perfuming cigarette can make up the insufficient fragrance part on cigarette tobacco leaf formulation, is improve one of product style and the effective means improving cigarette flavor quality.Tobacco extract is to extract isolated compound from tobacco material, good with the harmony of cigarette smoke and compatibility, is one of optimal additive of Medicated cigarette.
Bai Maoyan and paste hair smoke are the principal item that after Sichuan Province fifties, cultivated area is maximum, its distinctive paste rice water by fermentation technique, it is possible to improving flavor and taste so that fragrance is plentiful, pure, pleasant impression is pure, comfortable, is the important source material of cigar and blended type cigarette.Yunnan hair cigarette is different from Sichuan hair cigarette, and it is by light, Folium Salicis Babylonicae cutting to be formed, because its tobacco shred is soft, the thin hair cigarette as therefore named in hair of silk, abounds with in counties such as Yunnan Province's Tengchong, Longchuan, Lianghes.It is cut into the tobacco shred of wide 0.6 ~ 0.8mm after tobacco leaf picking by knife, is placed on air-curing of tobacco leaves pole to tan by the sun to dry, then with paper wrapper or be stored in large bamboo or wicker basket, allow its natural fermentation refine.It is less that Yunnan hair cigarette is applied in cigarette composition, how to use as pipe tobacco tobacco shred.
Subcritical fluid extraction technology is one of extractive technique emerging in recent years, have nontoxic, harmless, environmental protection, active component pollution-free, that retain extract does not destroy, does not aoxidize, can the feature such as industrialized production, therefore, the extraction of active ingredient of natural plant, natural pigment, special oil extraction etc. in be widely used.With tobacco material or Nicotiana tabacum L. crude extract for object of study in " method (200410022307.8) of refining waste tobacco primary extract at subcritical DMC " and " method (200410022306.3) of extracting waste tobacco at subcritical DMC ", prepared the higher Salanesol of pure tobacco oil, content and nicotine by subcritical abstraction technology.But, owing to the composition extracted is not had Selective Separation, pure tobacco oil still contains substantial amounts of non-volatile material, and some is to the disadvantageous composition of cigarette odor-absorbing, in the side effect such as inhaling taste discomfort, dry sensation that simultaneously results in of flavouring.In addition, what subcritical abstraction was conventional is butane, dimethyl ether etc. be nonpolar or weak polar solvent, according to the similar principle that mixes, also contains the materials such as substantial amounts of plant waxiness, fat-soluble chlorophyll while extracting containing plant effective component, these materials cause that extract is poorly soluble on the one hand, on the other hand cigarette odor-absorbing are played negative interaction.Molecular distillation belongs to special high vacuum distillation technology, and its vapo(u)rizing temperature is low, heated time is short, it is adaptable to the separation of thermal sensitivity effective ingredient, but cannot be directly used to the extraction of natural plants.Raw material is had certain requirement by molecular distillation when operation, as low in sugar content, viscosity is low, extraction gained extractum usually contains the macromolecular substances such as substantial amounts of saccharide, protein, cannot be used directly for molecular distillation, and the solvent polarity of subcritical abstraction is little, the content of extract obtained middle glucide is low, can meet the requirement of molecular distillation.Subcritical abstraction technology and molecular distillation coupling can reduce the content of macromolecular substances in pure tobacco oil, improve the content of small molecule volatile fragrance matter, are effectively improved the quality of essential oil of tobaccos.But up to now, utilize subcritical abstraction and molecular distillation multiple techniques to prepare hair cigarette quintessence oil have not been reported.
Summary of the invention
The purpose of the present invention is based on above-mentioned present situation and carries out, it is provided that the preparation method of a kind of mao of cigarette quintessence oil and application thereof.Adopt subcritical abstraction and molecular distillation multiple techniques, the content being effectively improved in quintessence oil Volatile infochemicals, prepared hair cigarette quintessence oil as cigarette products additive, can have effects such as improving Nicotiana tabacum L. suction taste, increase this perfume of Nicotiana tabacum L., increase flue gas concentration, reduction stimulation.
The purpose of the present invention can be achieved through the following technical solutions:
The preparation method of a kind of mao of cigarette quintessence oil, adopts subcritical abstraction and molecular distillation multiple techniques, carries out extracting and developing with hair cigarette for raw material, the content being effectively improved in quintessence oil Volatile infochemicals, specifically comprises the following steps that
(1) subcritical abstraction: tobacco leaf powder is broken to 10 ~ 100 orders, 0～50oUsing propane, butane or dimethyl ether as subcritical abstraction solvent when C, solid-liquid ratio is 1:8 ~ 1:15, and extracting pressure is the saturated vapor pressure of solvent for use under relevant temperature, and entrainer used is ethanol, and extraction time is 0.5～2h；After extraction terminates, extract mixed liquor and enter knockout drum, a mao smoke-dipping paste can be obtained by principle is evaporated under reduced pressure after extractant separation；Adding 95% ethanol of 5 ~ 10 times of quality in extractum, heating is to 30 ~ 50oC also keeps 20 ~ 60min to make it be cooled to room temperature after fully dissolving, and is transferred to-5oC~-20oIn C environment (such as refrigerator) freezing 8 ~ 24h；Sucking filtration or centrifugal (4000rpm, 10 ~ 30min) separation of supernatant, supernatant is evaporated to without, till ethanol, obtaining a mao cigarette absolute oil；
(2) molecular distillation: with hair cigarette absolute oil for raw material, separates purification further by molecular distillation technique, and condition is: pressure 0.01 ~ 0.1mbar, vapo(u)rizing temperature 40oC~100oC, the light component of gained is a mao cigarette quintessence oil.
The concentration of described entrainer ethanol is 55-95%, and the consumption of entrainer ethanol is 1-3 times of raw materials quality.
Described hair cigarette raw material is the Bai Maoyan in Sichuan, paste hair smoke or Yunnan hair cigarette.
Hair cigarette quintessence oil is added in tobacco shred, can improving flavouring essence quality and the mouthfeel of Medicated cigarette, improve the sense organ comfort level of Medicated cigarette, addition is the 0.001% ~ 0.01% of tobacco shred weight, with, after finite concentration ethanol dissolved dilution, being injected in blank Medicated cigarette with injection perfuming instrument automatically during interpolation.Can be used alone and also can be deployed into essence use with other spice.
Hair cigarette quintessence oil is added in tobacco juice for electronic smoke, this perfume of Nicotiana tabacum L. that electronic cigarette is strong can be given, strengthen gratification, reduce the sweet soapy feeling of solvent, consumption is the 0.01% ~ 0.5% of tobacco juice quality, after diluting with a certain amount of propylene glycol or glycerol during interpolation, it is filled in electronic cigarette cartridge, can be used alone and also can be made into essence use with other spice.
The maximum of the present invention is characterized in that: (1), compared with vapor distillation, substantially increases the extraction ratio of quintessence oil；(2) subcritical abstraction and molecular distillation technique coupling, greatly reduce the content of difficult volatilization macromolecular substances in quintessence oil, the content of volatile fragrance matter is improved, wherein the content relatively subcritical abstraction absolute oil of nicotine, solanone, neophytadiene, Megastigmatrienone, farnesyl acetone etc. is significantly improved so that the characteristic perfume of Nicotiana tabacum L. is more prominent.The present invention establishes simply effectively, is easy to the hair cigarette extraction of essential oil separating technology of industrialized production, and is applied in cigarette products by hair cigarette quintessence oil, can effectively strengthen this perfume of Nicotiana tabacum L., strengthen gratification, improve the similarity degree of electronic cigarette and traditional cigarette in electronic cigarette；Medicated cigarette does not change original performance and the processing technique of Medicated cigarette, improves flavouring essence quality and the mouthfeel of Medicated cigarette, improve flue gas concentration, reduce miscellaneous QI and zest, therefore have more meaning and the value of actual production.
Detailed description of the invention
Below in conjunction with example, the present invention is described further, but is not limiting as the present invention.
Embodiment 1
Taking the white hair Nicotiana tabacum L. of 200g, carry out subcritical abstraction: extracting pressure 0.78MPa after being crushed to 50 orders, extraction temperature is room temperature, and extractant is dimethyl ether, and solid-liquid ratio is 1:8, and entrainer is 95% ethanol, and entrainer consumption is 1.5 times of raw material, extraction time 1h.After extraction terminates, extract mixed liquor and enter knockout drum, a mao smoke-dipping paste can be obtained by principle is evaporated under reduced pressure after extractant separation.Adding 95% ethanol of 5 times of quality under stirring in above-mentioned extractum, heating is to 50oC also keeps 30min to make it fully dissolve, and is transferred in refrigerator (-5 after being cooled to room temperatureoC) freezing 24h；After sucking filtration, filtrate reduced in volume is to without, ethanol, obtaining a mao cigarette absolute oil.Being transferred in the head tank of molecular distillation by above-mentioned hair cigarette absolute oil, parameter is provided that vapo(u)rizing temperature 60oC, pressure is 0.2mbar, collects light component and is a mao cigarette quintessence oil.
Adopt GC/MS that hair cigarette quintessence oil is carried out component analysis, quintessence oil be mainly composed of nicotine, solanone, neophytadiene, Megastigmatrienone, farnesyl acetone etc., compared with subcritical abstraction gained absolute oil, the content of volatile material is improved, and the content such as neophytadiene is 2.1 times before separating.
Above-mentioned hair cigarette quintessence oil propylene glycol is diluted to mass concentration is 0.5%, it is filled in electronic cigarette cartridge and is smoked panel test, show through the 7 people comprehensive smoking result of above judging panel: this electronic cigarette has strong this perfume of Nicotiana tabacum L., oral cavity and throat stimulate less, sweet soapy feeling is substantially reduced, physiology gratification is relatively strong, higher with the similarity of Medicated cigarette.
Embodiment 2
Taking 200g Yunnan hair cigarette raw material, carry out subcritical abstraction: extracting pressure 0.89MPa after being crushed to 100 orders, extraction temperature is 40oC, extractant is propane, and solid-liquid ratio is 1:15, extraction time 1.5h.After extraction terminates, extract mixed liquor and enter knockout drum, a mao smoke-dipping paste can be obtained by principle is evaporated under reduced pressure after extractant separation.Adding 95% ethanol of 10 times of quality under stirring in above-mentioned extractum, heating is to 40oC also keeps 50min to make it fully dissolve, and is transferred in refrigerator (-20 after being cooled to room temperatureoC) freezing 8h；After sucking filtration, filtrate reduced in volume is to without, ethanol, obtaining a mao cigarette absolute oil.Being transferred in the head tank of molecular distillation by above-mentioned hair cigarette absolute oil, parameter is provided that vapo(u)rizing temperature 100oC, pressure is 0.1mbar, collects light component and is a mao cigarette quintessence oil.
Adopt GC/MS that hair cigarette quintessence oil is carried out component analysis, quintessence oil be mainly composed of nicotine, solanone, neophytadiene, Megastigmatrienone, farnesyl acetone etc., compared with subcritical abstraction gained absolute oil, the content of volatile material is improved, and the content such as farnesyl acetone is 1.95 times before separating.
Being 1% by above-mentioned hair cigarette quintessence oil with 95% ethanol dilution to mass concentration, be injected in blank Medicated cigarette with injection perfuming instrument automatically, injection volume is that 1 μ L/ props up.After injection, Medicated cigarette is loaded in cigarette case, be sealed under 22 ° of C ± 2 ° C and RH60% ± 5% conditions and place 1 week, then perfuming effect is evaluated.Smoking result shows that perfume quantity, perfume quantity all have to be increased significantly, and miscellaneous QI and zest reduce, and concentration improves.
Embodiment 3
Taking 200g paste hair smoke leaf, carry out subcritical abstraction: extracting pressure 0.45MPa after being crushed to 10 orders, extraction temperature is 50oC, extractant is butane, and solid-liquid ratio is 1:10, extraction time 0.5h.After extraction terminates, extract mixed liquor and enter knockout drum, a mao smoke-dipping paste can be obtained by principle is evaporated under reduced pressure after extractant separation.Adding 95% ethanol of 8 times of quality under stirring in above-mentioned extractum, heating is to 30oC also keeps 60min to make it fully dissolve, and is transferred in refrigerator (-10 after being cooled to room temperatureoC) freezing 12h；Centrifugation supernatant (4000rpm, 30min), supernatant is evaporated to without, till ethanol, obtaining a mao cigarette absolute oil.Being transferred in the head tank of molecular distillation by above-mentioned hair cigarette absolute oil, parameter is provided that vapo(u)rizing temperature 40oC, pressure is 0.01mbar, collects light component and is a mao cigarette quintessence oil.
Adopt GC/MS that hair cigarette quintessence oil is carried out component analysis, quintessence oil be mainly composed of nicotine, solanone, neophytadiene, Megastigmatrienone, farnesyl acetone etc., compared with subcritical abstraction gained absolute oil, the content of volatile material is improved, and the content such as nicotine is 3.14 times before separating.
Being 1% by above-mentioned hair cigarette quintessence oil with 95% ethanol dilution to mass concentration, be injected in blank Medicated cigarette with injection perfuming instrument automatically, injection volume is that 10 μ L/ prop up.After injection, Medicated cigarette is loaded in cigarette case, be sealed under 22 ° of C ± 2 ° C and RH60% ± 5% conditions and place 1 week, then perfuming effect is evaluated.Smoking result shows that flue gas exquisiteness is soft, and concentration increases, and residual and stimulation reduce.
Table 1 fragrance and flue gas characteristic evaluation result
| Sample number into spectrum | Aroma quality | Perfume quantity | Miscellaneous QI | Concentration | The property sent out thoroughly | Fine and smooth | Soft | Stimulate | Residual |
| 1#(embodiment 2) | 24.23 | 18.88 | 12.48 | 15.85 | 17.77 | 18.71 | 15.69 | 12.92 | 12.60 |
| 2#(embodiment 3) | 20.22 | 20.11 | 13.30 | 13.76 | 12.54 | 21.38 | 16.82 | 10.48 | 11.67 |
Note: blank Medicated cigarette indices is 0, when more than 11.2, average mark illustrates that this index has clear improvement, score value is more big, and the degree of improvement is more high.
Claims (6)
1. the preparation method of a hair cigarette quintessence oil, it is characterised in that: adopt subcritical abstraction and molecular distillation multiple techniques, carry out extracting and developing with hair cigarette for raw material, the content being effectively improved in quintessence oil Volatile infochemicals, specifically comprise the following steps that
(1) subcritical abstraction: tobacco leaf powder is broken to 10 ~ 100 orders, 0～50oUsing propane, butane or dimethyl ether as subcritical abstraction solvent when C, solid-liquid ratio is 1:8 ~ 1:15, and extracting pressure is the saturated vapor pressure of solvent for use under relevant temperature, and entrainer used is ethanol, and extraction time is 0.5～2h；After extraction terminates, extract mixed liquor and enter knockout drum, a mao smoke-dipping paste can be obtained by principle is evaporated under reduced pressure after extractant separation；Adding 95% ethanol of 5 ~ 10 times of quality in extractum, heating is to 30 ~ 50oC also keeps 20 ~ 60min to make it be cooled to room temperature after fully dissolving, and is transferred to-5oC~-20oFreezing 8 ~ 24h in C environment；Sucking filtration or centrifugation supernatant, supernatant is evaporated to without, till ethanol, obtaining a mao cigarette absolute oil；
(2) molecular distillation: with hair cigarette absolute oil for raw material, separates purification further by molecular distillation technique, and condition is: pressure 0.01 ~ 0.1mbar, vapo(u)rizing temperature 40oC~100oC, the light component of gained is a mao cigarette quintessence oil.
2. the preparation method of according to claim 1 mao of cigarette quintessence oil, it is characterised in that: the concentration of described entrainer ethanol is 55-95%, and the consumption of entrainer ethanol is 1-3 times of raw materials quality.
3. the preparation method of according to claim 1 mao of cigarette quintessence oil, it is characterised in that: described centrifugal condition is: rotating speed 4000rpm, time 10 ~ 30min.
4. the preparation method of according to claim 1 mao of cigarette quintessence oil, it is characterised in that: described hair cigarette raw material is the Bai Maoyan in Sichuan, paste hair smoke or Yunnan hair cigarette.
5. the hair cigarette quintessence oil that a kind utilizes method described in claim 1 to prepare application in cigarette products, it is characterized in that: hair cigarette quintessence oil is added in tobacco shred, can improving flavouring essence quality and the mouthfeel of Medicated cigarette, improve the sense organ comfort level of Medicated cigarette, addition is the 0.001% ~ 0.01% of tobacco shred weight.
6. the hair cigarette quintessence oil that a kind utilizes method described in claim 1 to prepare application in electronic cigarette, it is characterized in that: hair cigarette quintessence oil is added in tobacco juice for electronic smoke, this perfume of Nicotiana tabacum L. that electronic cigarette is strong can be given, strengthen gratification, reducing the sweet soapy feeling of solvent, consumption is the 0.01% ~ 0.5% of tobacco juice quality.
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