CN103386292B - A kind of adsorbent that reduces nitrosamine burst size in cigarette mainstream flue gas - Google Patents
A kind of adsorbent that reduces nitrosamine burst size in cigarette mainstream flue gas Download PDFInfo
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Abstract
The present invention relates to a kind of adsorbent that reduces nitrosamine burst size in cigarette mainstream flue gas, made by tea stalks particle and cape jasmine petal extract, wherein said tea stalks particle obtains after being pulverized by tea stalks after hydrochloric acid solution soaks, described cape jasmine petal extract is obtained by the suitable solvent extraction of cape jasmine petal ECDC, and described suitable solvent is selected from citric acid, malic acid, tartaric acid or its combination. Adsorbent provided by the invention can reduce the unique nitrosamine that grows tobacco of 4 in cigarette mainstream flue gas, and preparation is simple, and easy to operate, cost is low, can make cigarette smoke coordinate after being added in filter stick, and the comfortable taste of flue gas is obviously improved.
Description
Technical field
The invention belongs to Harm reduction techniques and fall burnt field, specifically, relate to one and can reduce cigarette masterAdsorbent and the preparation method and application of nitrosamine burst size in stream flue gas.
Background technology
Epidemiology survey shows, smoking can cause the diseases such as Human Lung, bronchus, oral cavity. CigaretteIn grass and flue gas, virulence factor mainly contains multiring aromatic hydrocarbon, nitrosamines etc., wherein the peculiar N-of tobaccoNitrosamine (tobacco-specificN-nitrosamines, TSNAs) is with N-nitroso demethylNicotine (NNN), N-nitroso anabasine (NAB), N-nitroso anatabine (NAT) and4-(N-methyl-N-nitrosamine)-1-(3-pyridine radicals)-butanone (NNK) is main. This is that a class is only depositedBe the N-nitrosamine compound in tobacco and flue gas, belong to organ specificity carcinogen, haveStronger carcinogenicity, the main target organ of its effect is lung tissue, at tobacco and flue gas associated diseasesIn play very important effect, thereby become people pay close attention to focus. Reduce in cigarette smokeTSNAs content is significant to improving safety cigarette.
In order to reduce the burst size of tobacco-specific nitrosamine, tobacco researcher has done greatly both at home and abroadThe research of amount. Nanjing University's Zhu Jianhua etc. discloses for absorbing nitrosamine in main flow flue gas in tobaccoNovel mesoporous material (CN101053446A), is used as cigarette mistake by the mesoporous material of high absorption propertyThe interpolation material of filter stick, adding material is to spread over Jie by the liquid film compound of high viscosity, difficult volatilizationThe surfaces externally and internally of porous molecular sieve forms, or the meso-porous molecular sieve material that contains template micella.In Hunan cigarette disclose a kind of cigarette filter that reduces nitrosamine and aldehydes matter in cigarette smoke andIts preparation method, utilizes metal oxide modified NACF to reduce the nitrosamine in cigarette smokeAnd phenols (CN101015394A). But these mouths rod adds the more expensive or system of material pricesStandby process is compared with complicated difficult for suitability for industrialized production, and its security also needs further to be studied. Fine jadeBuddhist nun R Williams discloses a kind of method (CN that plant is carried out to microwave in drying stage1231583A), for reducing NNN and the NNK of tobacco. Yuxi Hongta tobacco group is giving birth toIn product process, spray sodium alginate soln, reduce the nitrosamine (CN in main flume1335107A). But the amount that these methods are removed tobacco-specific nitrosamine is less and industrial productionThere is potential safety hazard.
Summary of the invention
For solving the problem of above-mentioned current existence, the object of this invention is to provide one can significantly reduceAdsorbent of tobacco-specific nitrosamine burst size and preparation method thereof in cigarette smoke. This cigarette filter rodCan significantly reduce in main flume the 4 unique nitrosamine (N-nitrosonornicotine (NN that grow tobaccoN), N-nitroso anabasine (NAT), N-nitroso anabasine (NAB) and 4-(methyl AsiaNitramine base)-4-(3-pyridine radicals)-1-butanone (NNK)) burst size, reduce tobacco in cigarette smokeThe harm that unique nitrosamine produces human body.
The object of the invention is to be achieved by following technical proposals:
Reduce an adsorbent for tobacco-specific nitrosamine burst size in cigarette smoke, according to the following stepsMake:
(1) take by weight 50～70 parts of tea stalks, 10～15 parts, cape jasmine petal;
(2) by tea stalks-20 DEG C～0 DEG C freezing 2～10 hours, control moisture content 5%～25%, after taking-up, tea stalks are placed in fast to the baking oven of 105 DEG C～150 DEG C, make its sizing of expanding.Then cooling, pulverized 40～60 mesh sieves, and soaked in the hydrochloric acid solution of 0.5～1.5mol/L2～10 hours, obtain tea stalks particle;
(3) being 0.1～1mol/L by cape jasmine petal and concentration is selected from citric acid, malic acid, wineOne or more solvent in stone acid, the consumption of solvent is 40～60ml/g cape jasmine petal (exampleAs 50ml/g cape jasmine petal), be positioned in closed container, at 60 DEG C～90 DEG C, react 30min～60min, filters to get filtrate, i.e. cape jasmine petal extract;
(4) the cape jasmine petal extract mix and blend 5 that tea stalks particle and step (3) obtained～15 hours, rear filtration, dried, and obtains filter stick adsorbent.
The above-mentioned adsorbent preparing is sieved, choose 40～60 order particles, be scattered in cigaretteThe acetate fibres of filter stick is intrafascicular, makes binary compound filter candle.
Further, the addition of adsorbent in filter stick is that 5～50mg/ props up.
The present invention is specifically related to the following aspects:
A first aspect of the present invention relates to a kind of nitrosamine burst size in cigarette mainstream flue gas of reducingAdsorbent, is made up of tea stalks particle and cape jasmine petal extract, wherein said tea stalks particleAfter being pulverized by tea stalks, after hydrochloric acid solution soaks, obtain, described cape jasmine petal extract is by cape jasminePetal obtains through suitable solvent extraction, described suitable solvent be selected from citric acid, malic acid,Tartaric acid or its combination.
According to the adsorbent described in first aspect present invention, wherein said tea stalks particle is being pulverizedFront first make its expand sizing.
In a preferred embodiment, the sizing of the expansion described in the present invention is that tea stalks are existed-20 DEG C～0 DEG C freezing 2～10 hours, control moisture content 5%～25%, after taking-up by tea stalksBe placed in fast the baking oven of 105 DEG C～150 DEG C, make its sizing of expanding.
According to the adsorbent described in first aspect present invention any one, it is characterized in that following a)～c)In one or more:
A) described tea stalks particle is that tea stalks were pulverized to 40～60 mesh sieves, and 0.5～In the hydrochloric acid solution of 1.5mol/L, soak 2～10 hours, obtain tea stalks particle;
B) described cape jasmine petal extract is the choosing that is 0.1～1mol/L by cape jasmine petal and concentrationOne or more solvent in citric acid, malic acid, tartaric acid, the consumption of solvent is 40～60ml/g cape jasmine petal (for example 50ml/g cape jasmine petal), be positioned in closed container 60 DEG C～At 90 DEG C, react 30min～60min, filter to get filtrate, be cape jasmine petal extract;
C) described adsorbent is by tea stalks particle and cape jasmine petal extract mix and blend 5～15Hour, rear filtration, dries, and obtains adsorbent.
A second aspect of the present invention relates to the adsorbent described in a kind of first aspect present invention any onePreparation method, comprise the following steps:
(1) take by weight 50～70 parts of tea stalks, 10～15 parts, cape jasmine petal;
(2) by tea stalks-20 DEG C～0 DEG C freezing 2～10 hours, control moisture content 5%～25%, after taking-up, tea stalks are placed in fast to the baking oven of 105 DEG C～150 DEG C, make its sizing of expanding.Then cooling, pulverized 40～60 mesh sieves, and soaked in the hydrochloric acid solution of 0.5～1.5mol/L2～10 hours, obtain tea stalks particle;
(3) being 0.1～1mol/L by cape jasmine petal and concentration is selected from citric acid, malic acid, wineOne or more solvent in stone acid, the consumption of solvent is 40～60ml/g cape jasmine petal (exampleAs 50ml/g cape jasmine petal), be positioned in closed container, at 60 DEG C～90 DEG C, react 30min～60min, filters to get filtrate, i.e. cape jasmine petal extract;
(4) the cape jasmine petal extract mix and blend 5 that tea stalks particle and step (3) obtained～15 hours, rear filtration, dried, and obtains adsorbent.
A third aspect of the present invention relate to adsorbent described in first aspect present invention any one forThe purposes of tobacco-specific nitrosamine in absorption cigarette mainstream flue gas.
A fourth aspect of the present invention relates to a kind of cigarette filter rod, wherein contains first aspect present inventionAdsorbent described in any one.
In the present invention, according to the cigarette filter rod described in fourth aspect, wherein said adsorbentAddition is that 5～50mg/ props up.
In the present invention, described " tobacco-specific nitrosamine ", " nitrosamine in main flume "," nitrosamine ", " N-nitrosamine " have identical implication, refer to only at tobacco and tobacco productThe N-nitrosamine of middle existence.
The usefulness of technique scheme is:
Adsorbent specific surface prepared by the present invention is 150～250m2/ g. In described adsorbent, teaAfter leaf stalk expands and shapes, specific area is larger, easily contact with the oxious component in flue gas, meanwhile,After tea stalks soak after pulverizing in acid hydrochloric acid solution, tea stalks particle surface forms H+ electricityLotus, make tea stalks particle have faintly acid, and nitrosamine has alkalescent, and therefore the two is mutualBetween there is certain chemical action, can reduce the tobacco-specific nitrosamine in flue gas. Cape jasmine PittosporumIn acid flower, with after citric acid, malic acid, tartaric acid solvent extraction, extract not only hasFaintly acid, also can coordinate mutually with the smell of tealeaves. In addition, the preparation of this adsorbent is simple, operationConvenient, cost is low, Material Addition in filter stick after, the comfortable taste of flue gas is obviously improved.
Detailed description of the invention
Below in conjunction with embodiment, embodiment of the present invention are described in detail, but abilityField technique personnel will be understood that, the following example is only for the present invention is described, and should not be considered as limitFixed scope of the present invention. Unreceipted actual conditions person in embodiment, according to normal condition or manufactureThe condition of business's suggestion is carried out. The unreceipted person of production firm of agents useful for same or instrument, is and can leads toCross the conventional products of commercial acquisition.
Below in embodiment, the BET specific area QuantschromeNOVA of adsorbent4200E type physical adsorption appearance is measured.
Below in embodiment, four in main flume grow tobacco unique nitrosamine measuring method asUnder:
1 cigarette smoking
Suction on SM400 orthoscopic smoking machine (suction capacity 35ml/min), according to GB/T19609, use the TPM of 5 cigarette of glass fiber filter that 1 diameter is 44mm trapping,Each sample is answered parallel determination 2 times.
2 sample extraction
Filter disc is placed in to 50mL conical flask, accurately adds 15.0mL extraction solution, ultrasonic extractionGet after 30min, leave standstill 5min. Get 1mL extract and cross 0.22 μ m filter membrane, move to chromatogram and divideAnalyse in bottle to be analyzed.
3 analysis conditions
According to manufacturer's operation manual operation high performance liquid chromatography-tandem mass combined instrument.
3.1 Quick-type high-efficient liquid phase chromatogram conditions
---chromatographic column: C18 post (1.7 μ m, 2.1mm × 100mm) or equivalent post;
---flow velocity: 0.4mL/min;
---column temperature: 40 DEG C;
---sample size: 5 μ L;
---mobile phase A: methyl alcohol, Mobile phase B: 0.2%(volume ratio) acetic acid solution,Condition of gradient elution is in table 1.
Table 1 Quick-type Gradient Elution condition
3.2 mass spectrum reference conditions
---ion gun: electron spray ionisation source (ESI);
---scan mode: cation scanning;
---detection mode: multiple-reaction monitoring (MRM);
---electron spray voltage: 5500V;
---ion source temperature: 650 DEG C;
---assisted gas Gas1 pressure: 0.349MPa;
---assisted gas Gas2 pressure: 0.483MPa;
The quota ion of each analyte to, qualitative ion pair and collision energy (CE) in table 2.
Table 2 the MS detection parameters table
4 sample determinations
1 parent ion of every kind of tested compositional selecting, more than 2 or 2 daughter ion, in identical realityTest under condition, in sample, the relative retention time of test substance is corresponding with standard operation solutionRetention time deviation is within ± 2.5%; And in sample spectrogram, each component characteristics ion is relatively richThe relative abundance of spending characteristic of correspondence ion in the standard operation solution closing on concentration compares, when relative abundance > 50% time, tolerance ± 20%, when relative abundance is 20%～50%Time, tolerance ± 25%, when relative abundance is 10%～20% time, tolerance ± 30%,In the time of relative abundance < 10%, tolerance ± 50%. Preparation nitrosamine standard operation solution, pointAnalyse sample introduction, drawing standard working curve, coefficient R2Should be not less than 0.99, inner mark method ration.
The calculating of 5 results and statement
In cigarette mainstream flue gas, the transmission quantity of TSNAs is calculated by formula (1):
In formula:
M---the transmission quantity of TSNAs in every cigarette mainstream flue gas, unit is every of nanogram (ng/cig);
A---the concentration of TSNAs in extraction solution, unit is every milliliter of nanogram (ng/mL);
The volume of V---extraction solution, unit is milliliter (mL);
N---cigarette quantity, unit is (cig).
Embodiment 1: take by weight 70 parts of tea stalks, 15 parts, cape jasmine petal; By tealeavesStalk-20 DEG C freezing 2 hours, control moisture content 5%, after taking-up, tea stalks are placed in to 105 DEG C fastBaking oven in, make its expand sizing. Then cooling, pulverized 40～60 mesh sieves, and at 0.5mol/LHydrochloric acid solution in soak 2 hours, the consumption of hydrochloric acid can not have tea stalks particle, obtains teaLeaf stalk particle; Cape jasmine petal is mixed with 0.1mol/L citric acid solution, and the consumption of citric acid is50ml/g cape jasmine petal, is positioned in closed container and reacts 30min at 60 DEG C, filters to get filtrate;Tea stalks particle and filtrate are stirred 5 hours, and rear filtration, dries, and obtains filter stick adsorbent.The BET specific area of this adsorbent is 241m2/ g. The above-mentioned adsorbent preparing is sieved,Choose 40～60 order particles, the acetate fibres that is scattered in cigarette filter rod is intrafascicular, makes binary compoundFilter stick. In every filter stick, add adsorbent 15mg/ and prop up, composite filter cigarette is become to cigarette.
In the filter stick that mensuration above-described embodiment 1 prepares, add the main flume of the cigarette of adsorbentIn four content that grow tobacco unique nitrosamine, (contrast with the cigarette that does not add adsorbent in filter stickSample) contrast. Result is as shown in table 3.
Table 3 composite filter reduces in main flume 4 results that grow tobacco unique nitrosamine
The above results shows, adsorbent prepared by the present invention can be used for composite filter production of cigarettes, rightNAB in main flume, NAT, NNK, the range of decrease of NNN reaches respectively 28.42%, 44.17%,55.03% and 47.44%. In addition, sensory evaluating smoking's result shows, this adsorbent is added in filter stickAfter can make cigarette smoke coordinate, the comfortable taste of flue gas is obviously improved.
Embodiment 2:
Take by weight 50 parts of tea stalks, 15 parts, cape jasmine petal; Tea stalks are cold at-10 DEG CFreeze 10 hours, control moisture content 25%, after taking-up, tea stalks are placed in fast to the baking oven of 150 DEG CIn, make its sizing of expanding. Then cooling, pulverized 40～60 mesh sieves, and at the salt of 1.5mol/LIn acid solution, soak 10 hours, the consumption of hydrochloric acid can not have tea stalks particle, obtains tea stalksParticle; Cape jasmine petal is mixed with 1mol/L malic acid solution, and the consumption of malic acid is 50ml/g Cape jasmineSub-petal, is positioned in closed container and reacts 40min at 90 DEG C, filters to get filtrate; By tealeavesStalk particle and filtrate are stirred 15 hours, and rear filtration is dried, and obtains filter stick adsorbent. This absorptionThe BET specific area of agent is 225m2/ g. The above-mentioned adsorbent preparing is sieved, choose40～60 order particles, the acetate fibres that is scattered in cigarette filter rod is intrafascicular, makes binary compound filter candle,In every filter stick, add adsorbent 20mg/ and prop up, composite filter cigarette is become to cigarette.
In the filter stick that mensuration above-described embodiment 2 prepares, add the main flume of the cigarette of adsorbentIn four content that grow tobacco unique nitrosamine, (contrast with the cigarette that does not add adsorbent in filter stickSample) contrast. Result is as shown in table 4.
Table 4 composite filter reduces in main flume 4 results that grow tobacco unique nitrosamine
The above results shows, adsorbent prepared by the present invention can be used for composite filter production of cigarettes, rightNAB in main flume, NAT, NNK, the range of decrease of NNN reaches respectively 33.88%, 49.09%,62.89% and 51.02%. In addition, sensory evaluating smoking's result shows, this adsorbent is added in filter stickAfter can make cigarette smoke coordinate, the comfortable taste of flue gas is obviously improved.
Embodiment 3:
Take by weight 60 parts of tea stalks, 15 parts, cape jasmine petal; By tea stalks at-15 DEG CFreezing 7 hours, control moisture content 15%, after taking-up, tea stalks are placed in fast to the baking oven of 120 DEG CIn, make its sizing of expanding. Then cooling, pulverized 40～60 mesh sieves, and 1.0mol/L'sIn hydrochloric acid solution, soak 8 hours, the consumption of hydrochloric acid can not have tea stalks particle, obtains tealeavesStalk particle; Cape jasmine petal is mixed with 0.7mol/L tartaric acid solution, and tartaric consumption is50ml/g cape jasmine petal, is positioned in closed container and reacts 50min at 80 DEG C, filters to get filtrate;Tea stalks particle and filtrate are stirred 10 hours, and rear filtration, dries, and obtains filter stick adsorbent.The BET specific area of this adsorbent is 237m2/ g. The above-mentioned adsorbent preparing is sieved,Choose 40～60 order particles, the acetate fibres that is scattered in cigarette filter rod is intrafascicular, makes binary compoundFilter stick, adds adsorbent 10mg/ and props up in every filter stick, composite filter cigarette is become to cigarette.
In the filter stick that mensuration above-described embodiment 3 prepares, add the main flume of the cigarette of adsorbentIn four content that grow tobacco unique nitrosamine, (contrast with the cigarette that does not add adsorbent in filter stickSample) contrast. Result is as shown in table 5.
Table 5 composite filter reduces in main flume 4 results that grow tobacco unique nitrosamine
The above results shows, adsorbent prepared by the present invention can be used for composite filter production of cigarettes, rightNAB in main flume, NAT, NNK, the range of decrease of NNN reaches respectively 13.11%, 32.41%,43.88% and 35.32%. In addition, sensory evaluating smoking's result shows, this adsorbent is added in filter stickAfter can make cigarette smoke coordinate, the comfortable taste of flue gas is obviously improved.
Claims (9)
1. reduce an adsorbent for nitrosamine burst size in cigarette mainstream flue gas, by tea stalks particleMake with cape jasmine petal extract, wherein said tea stalks particle pulverized by tea stalks after through hydrochloric acidSolution obtains after soaking, and described cape jasmine petal extract is by the suitable solvent extraction of cape jasmine petal ECDCObtain, described suitable solvent is selected from citric acid, malic acid, tartaric acid or its combination;
Wherein said tea stalks particle first makes its sizing of expanding before pulverizing.
2. the adsorbent of claim 1, wherein said expansion sizing be by tea stalks-20 DEG C～0 DEG C freezing 2～10 hours, control moisture content 5%～25%, after taking-up, tea stalks are put fastIn the baking oven of 105 DEG C～150 DEG C, make its sizing of expanding.
3. the adsorbent of claim 1 or 2, it is characterized in that following a)～one or more in c):
A) described tea stalks particle is that tea stalks were pulverized to 40～60 mesh sieves, and 0.5～In the hydrochloric acid solution of 1.5mol/L, soak 2～10 hours, obtain tea stalks particle;
B) described cape jasmine petal extract is the choosing that is 0.1～1mol/L by cape jasmine petal and concentrationOne or more solvent in citric acid, malic acid, tartaric acid, the consumption of solvent is 40～60ml/g cape jasmine petal, is positioned in closed container and reacts 30min～60min at 60 DEG C～90 DEG C,Filter to get filtrate, be cape jasmine petal extract;
C) described adsorbent is by tea stalks particle and cape jasmine petal extract mix and blend 5～15Hour, rear filtration, dries, and obtains adsorbent.
4. the adsorbent of claim 3, wherein b) consumption of a described solvent is 50ml/g cape jasminePetal.
5. a preparation method for the adsorbent described in claim 1-4 any one, comprises following stepRapid:
(1) take by weight 50～70 parts of tea stalks, 10～15 parts, cape jasmine petal;
(2) by tea stalks-20 DEG C～0 DEG C freezing 2～10 hours, control moisture content 5%～25%, after taking-up, tea stalks are placed in fast to the baking oven of 105 DEG C～150 DEG C, make its sizing of expanding,Then cooling, pulverized 40～60 mesh sieves, and soaked in the hydrochloric acid solution of 0.5～1.5mol/L2～10 hours, obtain tea stalks particle;
(3) being 0.1～1mol/L by cape jasmine petal and concentration is selected from citric acid, malic acid, wineOne or more solvent in stone acid, the consumption of solvent is 40～60ml/g cape jasmine petal, putsBe placed in closed container and react 30min～60min at 60 DEG C～90 DEG C, filter to get filtrate, i.e. Cape jasmineSub-petal extract;
(4) the cape jasmine petal extract mix and blend 5 that tea stalks particle and step (3) obtained～15 hours, rear filtration, dried, and obtains adsorbent.
6. the preparation method of claim 5, wherein the consumption of the described solvent of step (3) is 50ml/gCape jasmine petal.
7. the adsorbent described in claim 1-4 any one is used for adsorbing the cigarette mainstream flue gas Central AsiaThe purposes of nitramine.
8. a cigarette filter rod, wherein contains the adsorbent described in claim 1-4 any one.
9. the cigarette filter rod of claim 8, the addition of wherein said adsorbent is 5～50mg/ props up.
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| CN103837633A (en) * | 2014-03-16 | 2014-06-04 | 国家烟草质量监督检验中心 | Liquid chromatogram tandem mass spectrum measurement method for tobacco-specific nitrosamines in electronic cigarette liquid |
| CN104223355B (en) * | 2014-09-09 | 2015-10-28 | 安徽中烟工业有限责任公司 | A kind of electroosmose process that utilizes is separated the method removing TSNA in burley tobaccos extract |
| CN110367584B (en) * | 2019-06-28 | 2020-06-09 | 北京荣超利科技有限公司 | Tobacco additive and application thereof |
| CN112056613A (en) * | 2020-09-07 | 2020-12-11 | 广西中烟工业有限责任公司 | Preparation method of cigarette filter stick with gardenia fragrance |
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| CN102217782A (en) * | 2010-04-15 | 2011-10-19 | 厦门中海钓台生物工程有限公司 | Tea leaf thin sheet for cigarette, preparation method thereof and cigarette |
| CN102783712A (en) * | 2012-08-08 | 2012-11-21 | 福建中烟工业有限责任公司 | Filter stick flavor enhancing tea particle and preparation method thereof |
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| CN102217782A (en) * | 2010-04-15 | 2011-10-19 | 厦门中海钓台生物工程有限公司 | Tea leaf thin sheet for cigarette, preparation method thereof and cigarette |
| CN102783712A (en) * | 2012-08-08 | 2012-11-21 | 福建中烟工业有限责任公司 | Filter stick flavor enhancing tea particle and preparation method thereof |
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