CN103027378B - Preparation method of composite additive for reducing phenol in cigarette smoke - Google Patents
Preparation method of composite additive for reducing phenol in cigarette smoke Download PDFInfo
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- CN103027378B CN103027378B CN201210583462.1A CN201210583462A CN103027378B CN 103027378 B CN103027378 B CN 103027378B CN 201210583462 A CN201210583462 A CN 201210583462A CN 103027378 B CN103027378 B CN 103027378B
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Abstract
The invention discloses a method for preparing the composite additive for reducing phenol in cigarette smoke. The composite additive is a schizonepeta essential oil and cyclodextrin inclusion compound which contains cyclodextrin and schizonepeta essential oil. The cyclodextrin is utilized for schizonepeta essential oil inclusion, the stability of the schizonepeta essential oil under normal temperature is increased, the composite additive can be used in a cigarette filter, so that the capability of the cigarette filter in absorbing the phenol in main cigarette smoke is enhanced, and the health-care effect of the schizonepeta essential oil is prolonged.
Description
Technical field
The present invention relates to a kind of compound additive that reduces phenol in cigarette smoke and its production and use.
Background technology
Along with social progress, smoking and the healthy focus that day by day becomes people's concern.In cigarette mainstream flue gas, phenol is as one of seven kinds of indexs of evaluating cigarette harmfulness, and is put into Canadian government list.Therefore, reducing phenol in cigarette mainstream flue gas is of great practical significance.In Chinese patent CN201010200267.7, the nuisance cigarette forming paper functional paint such as phenol in elective reduction flue gas is disclosed, in coating, contain the compounds such as polyethylene glycol, levulic acid, triethylene-glycol diacetate, this functional paint can be effectively, highly selective reduces phenol, NH in cigarette smoke
3burst size, greatly reduced the harm to smoker.In Chinese patent CN201110194289.1, a kind of selective harm reduction cigarette and preparation method thereof is disclosed, this method is by surface hydrophobicity nanometer SiO
2particle, adds by the 0.5-10% of pipe tobacco, reconstituted tobacco or stem percentage by weight, 27.2% phenol and 12.4% crotonaldehyde in alternative harm reduction cigarette reduction main flume.
Said method is only that the angle of phenol from reduce cigarette is considered.And the phenol of the present invention in not only can selectivity reducing cigarette main flume also has the effect of health care.There is bibliographical information phenol can be dissolved in volatile oil, herein Herba Schizonepetae volatile oil is added in cigarette filter, remove the phenol in cigarette mainstream flue gas.
The pharmacological action of Herba Schizonepetae volatile oil mainly contains: anti-inflammatory, analgesia, antiviral, antibacterial, cooling, eliminating phlegm and relieving asthma etc.Due to unstable under Herba Schizonepetae volatile oil nature, volatile, see that light easily decomposes, so directly additive effect is bad, affect its action effect.Therefore, also choose another purposes chemical reagent beta-schardinger dextrin-very widely herein Herba Schizonepetae volatile oil is carried out to inclusion, increase the stability of Herba Schizonepetae volatile oil.
The special construction of beta-schardinger dextrin-has determined the little molecule of its object with inclusion moderate dimensions.Application comprises: food industry, medical industry, cosmetics, environmental science etc.
Summary of the invention
The object of the present invention is to provide compound additive of phenol in the reduction cigarette smoke that a kind of result of use is good and its production and use.
Technical solution of the present invention is:
A compound additive that reduces phenol in cigarette smoke, is characterized in that: be the Herba Schizonepetae volatile oil cyclodextrin inclusion compound that contains cyclodextrin and Herba Schizonepetae volatile oil.
Described cyclodextrin is alpha-cyclodextrin, beta-schardinger dextrin-or gamma-cyclodextrin.
A preparation method who reduces the compound additive of phenol in cigarette smoke, is characterized in that: comprise the following steps:
(1) cyclodextrin is dissolved in solvent, makes saturated solution I;
(2) by Herba Schizonepetae volatile oil and absolute ethyl alcohol 1:1 mixing by volume, wiring solution-forming II;
(3) solution II is added in solution I, stir and obtain Herba Schizonepetae volatile oil cyclodextrin inclusion compound solution; Wherein the mass volume ratio of cyclodextrin and Herba Schizonepetae volatile oil is 1:1 ~ 10g/mL;
(4) the above-mentioned Herba Schizonepetae volatile oil cyclodextrin inclusion compound solution making is placed to 24 ~ 48h in 1 ~ 4 ℃, separate out white precipitate, filter, absolute ethanol washing, dry at the temperature of 30 ~ 50 ℃, obtain the Herba Schizonepetae volatile oil cyclodextrin inclusion compound powder of solid.
Solvent in step (1) is water, pyridine, dimethyl formamide, dimethyl sulfoxide (DMSO) or ethylene glycol.
The purposes of the compound additive of phenol in described reduction cigarette smoke, is characterized in that: in the cigarette filter tip of cigarette, add the Herba Schizonepetae volatile oil cyclodextrin inclusion compound that contains cyclodextrin and Herba Schizonepetae volatile oil.
Herba Schizonepetae volatile oil cyclodextrin inclusion compound addition is the 0.2%-5% of cigarette gross mass.
The present invention carries out inclusion by cyclodextrin to Herba Schizonepetae volatile oil, increases the stability under Herba Schizonepetae volatile oil normal temperature, can be used in cigarette filter, increases the ability of phenol in its absorption cigarette mainstream flue gas, extends the health-care efficacy of Herba Schizonepetae volatile oil.
The flue gas analysis experiment of carrying out with Herba Schizonepetae volatile oil cyclodextrin inclusion compound is as follows:
The filter tip of cigarette is taken out with tweezers, then cut as two sections equal in length with scissors, and a section of being crossed by tweezers tweezer is first got back in cigarette; To the solid Herba Schizonepetae volatile oil cyclodextrin inclusion compound powder that adds appropriate preparation in every cigarette, then other one section of filter tip is got back in cigarette more again, cut the part that filter tip has more with scissors.Sample adds 80, and it is all put into climatic chamber constant temperature and humidity (22.0 ℃ of temperature, humidity 60.0%) 48 hours.The demonstration of flue gas analysis result, the cigarette that has added Herba Schizonepetae volatile oil cyclodextrin inclusion compound can reduce the amount of phenol in cigarette mainstream flue gas better.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
Fig. 1 is the XRD collection of illustrative plates of the inclusion compound adsorbing phenol front and back of volatile oil-beta-schardinger dextrin-.
In figure: before (1) adsorbing phenol; (2) after adsorbing phenol;
The specific embodiment
Embodiment 1:
Balance takes 7.29g beta-schardinger dextrin-, is placed in the beaker of 300mL, and the distilled water that adds 100mL is heated to dissolve completely in the thermostat water bath of 60 ℃.The isopyknic anhydrous alcohol solution of Herba Schizonepetae volatile oil that measures 1.2mL, the volatile oil of dissolving is at 1000rmin
-1speed high-speed stirred under slowly add in the beta-schardinger dextrin-aqueous solution, after treating that volatile oil dropwises, inclusion 2 hours.After inclusion, inclusion compound is placed on to refrigerator and cooled and freezes placement 24h.After the frequent press filtration of inclusion compound, with absolute ethyl alcohol, wash away the volatile oil on inclusion compound surface, in the baking oven of 50 ℃, dry to constant weight and obtain solid Herba Schizonepetae volatile oil cyclodextrin inclusion compound powder.
Embodiment 2:
The preparation method of additive is with embodiment 1, and the additive that takes 30mg manually adds in cigarette filter.Under GB/T16447 defined terms, carry out balance, select the cigarette of average weight ± 0.02g, with SM450 smoking machine, according to YC/T29-1996 specified standard condition smoking cigarette, adopt the mensuration high performance liquid chromatography > > of YC/T255-2008 < < main phenolic compounds in main stream smoke of cigarette to detect the content of phenol in cigarette mainstream flue gas.Testing result is as shown in table 1.
The impact of table 1 additive on phenol content in cigarette mainstream flue gas
As can be seen from Table 1, having added phenol content in the cigarette sample of additive of beta-schardinger dextrin-and volatile oil inclusion compound has significantly and reduces with respect to contrast cigarette.This may be because on the one hand, phenol enters after beta-schardinger dextrin-cavity, by cyclodextrin encapsulated, thereby has reduced the content of phenol in flue gas; On the other hand, phenol enters after the inclusion compound cavity of Herba Schizonepetae volatile oil-beta-schardinger dextrin-, and phenol is not only by inclusion compound inner chamber inclusion, also and volatile oil have an effect, thereby make the content reduction of phenol in flue gas.After inclusion compound adsorbing phenol, having formed new material, there is the variation of some in structure, as in Fig. 1 1., 2., 3., 4. the diffracted intensity at peak weakens before compared with adsorbing phenol to some extent; In figure, I, II, III, IV are the new diffraction maximums producing after adsorbing phenol.XRD collection of illustrative plates before and after the inclusion compound adsorbing phenol of volatile oil-beta-schardinger dextrin-as shown in Figure 1.
Embodiment 3:
The preparation method of additive is with embodiment 1, and the additive that takes 20mg manually adds in cigarette filter.Under GB/T16447 defined terms, carry out balance, select the cigarette of average weight ± 0.02g, with SM450 smoking machine, according to YC/T29-1996 specified standard condition smoking cigarette, adopt the mensuration high performance liquid chromatography > > of YC/T255-2008 < < main phenolic compounds in main stream smoke of cigarette to detect the content of phenol in cigarette mainstream flue gas.Testing result is as shown in table 2.
The impact of table 2 additive on phenol content in cigarette mainstream flue gas
As can be seen from Table 2, added after different additive, in cigarette sample main flume, the content of phenol has had reduction in various degree with respect to contrast cigarette.Wherein, the reduced rate that adds Herba Schizonepetae volatile oil inclusion compound is the highest, can reach 47.69%.But compare with the cigarette test result of adding 30mg, the effect that reduces phenol in cigarette mainstream flue gas has reduced much.But considering cost and additive account for the many factors such as cigarette percetage by weight, select 20mg comparatively reasonable.
Embodiment 4:
Reducing a compound additive for phenol in cigarette smoke, is the Herba Schizonepetae volatile oil cyclodextrin inclusion compound that contains cyclodextrin and Herba Schizonepetae volatile oil.
Described cyclodextrin is beta-schardinger dextrin-(or alpha-cyclodextrin or gamma-cyclodextrin).
Preparation method comprises the following steps:
(1) cyclodextrin is dissolved in solvent, makes saturated solution I;
(2) by Herba Schizonepetae volatile oil and absolute ethyl alcohol 1:1 mixing by volume, wiring solution-forming II;
(3) solution II is added in solution I, stir and obtain Herba Schizonepetae volatile oil cyclodextrin inclusion compound solution; Wherein the mass volume ratio of cyclodextrin and Herba Schizonepetae volatile oil is 1:1 ~ 10g/mL(example 1:1,1:5,1:10);
(4) the above-mentioned Herba Schizonepetae volatile oil cyclodextrin inclusion compound solution making is placed to 24 ~ 48h(example 24h, 26h, 28h in 1 ~ 4 ℃ (1 ℃, 3 ℃, 4 ℃ of examples)), separate out white precipitate, filter, absolute ethanol washing, at the temperature of 30 ~ 50 ℃ (30 ℃, 40 ℃, 50 ℃ of examples), be dried, obtain the Herba Schizonepetae volatile oil cyclodextrin inclusion compound powder of solid.
Solvent in step (1) is water, pyridine, dimethyl formamide, dimethyl sulfoxide (DMSO) or ethylene glycol.
The purposes of the compound additive of phenol in described reduction cigarette smoke is added the Herba Schizonepetae volatile oil cyclodextrin inclusion compound that contains cyclodextrin and Herba Schizonepetae volatile oil in the cigarette filter tip of cigarette.
Herba Schizonepetae volatile oil cyclodextrin inclusion compound addition is the 0.2%-5%(example 02%, 3%, 5% of cigarette gross mass).
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| CN113040419A (en) * | 2019-12-27 | 2021-06-29 | 湖南中烟工业有限责任公司 | Electronic cigarette liquid capable of stably releasing nicotine |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088785A (en) * | 1992-12-30 | 1994-07-06 | 何其果 | Cigarette type imbibition as health product |
| CN1391847A (en) * | 2001-06-14 | 2003-01-22 | 刘仲华 | Cigarette imitating health sucked article |
| CN101736654A (en) * | 2009-12-08 | 2010-06-16 | 湖南中烟工业有限责任公司 | Preparation and application of cigarette paper filter material containing Chinese herbal components |
| CN102805425A (en) * | 2012-08-30 | 2012-12-05 | 江苏中烟工业有限责任公司 | Application of beta-carotene/beta-cyclodextrin inclusion compounds to release quantity reduction of phenolic compounds in cigarette smoke gas |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088785A (en) * | 1992-12-30 | 1994-07-06 | 何其果 | Cigarette type imbibition as health product |
| CN1391847A (en) * | 2001-06-14 | 2003-01-22 | 刘仲华 | Cigarette imitating health sucked article |
| CN101736654A (en) * | 2009-12-08 | 2010-06-16 | 湖南中烟工业有限责任公司 | Preparation and application of cigarette paper filter material containing Chinese herbal components |
| CN102805425A (en) * | 2012-08-30 | 2012-12-05 | 江苏中烟工业有限责任公司 | Application of beta-carotene/beta-cyclodextrin inclusion compounds to release quantity reduction of phenolic compounds in cigarette smoke gas |
Non-Patent Citations (2)
| Title |
|---|
| 《超声法制备荆芥精油/β-环糊精包合物的研究》;刘艳芳等;《郑州轻工业学院学报》;20100228;第25卷(第1期);26-28 * |
| 刘艳芳等.《超声法制备荆芥精油/β-环糊精包合物的研究》.《郑州轻工业学院学报》.2010,第25卷(第1期),26-28. |
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