CN1298096A - Microwave spectrophotometric process for the fast detection of nitrosamine and nitroxide content in tobacco - Google Patents
Microwave spectrophotometric process for the fast detection of nitrosamine and nitroxide content in tobacco Download PDFInfo
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- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 58
- XKLJHFLUAHKGGU-UHFFFAOYSA-N nitrous amide Chemical compound ON=N XKLJHFLUAHKGGU-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title claims abstract description 27
- 241000208125 Nicotiana Species 0.000 title claims description 57
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical class ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 title 1
- 238000001514 detection method Methods 0.000 title 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 6
- 150000004008 N-nitroso compounds Chemical class 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 30
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 27
- 229910052757 nitrogen Inorganic materials 0.000 claims description 15
- 230000005855 radiation Effects 0.000 claims description 14
- FDDDEECHVMSUSB-UHFFFAOYSA-N sulfanilamide Chemical compound NC1=CC=C(S(N)(=O)=O)C=C1 FDDDEECHVMSUSB-UHFFFAOYSA-N 0.000 claims description 10
- 229940124530 sulfonamide Drugs 0.000 claims description 10
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 8
- 239000007789 gas Substances 0.000 claims description 8
- 238000010521 absorption reaction Methods 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- 238000002835 absorbance Methods 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000008363 phosphate buffer Substances 0.000 claims description 4
- FYKDNWHPKQOZOT-UHFFFAOYSA-M sodium;dihydrogen phosphate;2-hydroxypropane-1,2,3-tricarboxylic acid Chemical compound [Na+].OP(O)([O-])=O.OC(=O)CC(O)(C(O)=O)CC(O)=O FYKDNWHPKQOZOT-UHFFFAOYSA-M 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- MNZMECMQTYGSOI-UHFFFAOYSA-N acetic acid;hydron;bromide Chemical compound Br.CC(O)=O MNZMECMQTYGSOI-UHFFFAOYSA-N 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 238000010504 bond cleavage reaction Methods 0.000 claims description 2
- 239000001307 helium Substances 0.000 claims description 2
- 229910052734 helium Inorganic materials 0.000 claims description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 2
- 238000002044 microwave spectrum Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 abstract 3
- 244000061176 Nicotiana tabacum Species 0.000 abstract 1
- 230000003139 buffering effect Effects 0.000 abstract 1
- 238000004452 microanalysis Methods 0.000 abstract 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 abstract 1
- 235000019799 monosodium phosphate Nutrition 0.000 abstract 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 abstract 1
- 235000019504 cigarettes Nutrition 0.000 description 35
- 150000004005 nitrosamines Chemical class 0.000 description 19
- 239000000779 smoke Substances 0.000 description 18
- 239000000243 solution Substances 0.000 description 10
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 9
- 229960002715 nicotine Drugs 0.000 description 9
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 9
- 239000000047 product Substances 0.000 description 7
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 6
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 239000003546 flue gas Substances 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000002798 spectrophotometry method Methods 0.000 description 4
- 239000002671 adjuvant Substances 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000006378 damage Effects 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 208000005623 Carcinogenesis Diseases 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000007853 buffer solution Substances 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 230000036952 cancer formation Effects 0.000 description 1
- 231100000504 carcinogenesis Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 231100000260 carcinogenicity Toxicity 0.000 description 1
- 230000007670 carcinogenicity Effects 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019506 cigar Nutrition 0.000 description 1
- 238000004737 colorimetric analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001031 gas chromatography-thermal energy analyser Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000010977 jade Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- -1 nitrosamine compound Chemical class 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 210000002826 placenta Anatomy 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 230000000391 smoking effect Effects 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 210000001835 viscera Anatomy 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
Tobacco inside one container is irradiated by microwave and volatilized NOx and nitrosamine are blown out with N2 gas. The nitrosamine is absorbed by buffering solution comprising citric acid and sodium dihydrogen phosphate and the nitrosamine content is then detected by means of "the microanalysis process for the apparent total amount of N-nitroso compound" (Patent No.97107228.0). The unabsorbed NOx is absorbed and converted into colorating NO2 by using sulfanilamide-naphthylethylenediamide hydrochloride and the NOx content is then detected and calculated with a spectropotometer.
Description
The present invention relates to microwave radiation and detect nitrosamine and oxides of nitrogen (NO in the tobacco in conjunction with improving spectrophotometric method
x) method of content.
Contained nitrosamine causes people's great vigilance with its strong carcinogenicity in tobacco and the cigarette smoke.Nitrosamine is the extensive chemical carcinogenic substance, has about 90% to be proved to be and to have carcinogenesis surplus in the of 300 in kind of the nitrosamine compound: internal organs that animal is all and organize all can be by induced tumor, and main target organ is liver, oesophagus, lung, stomach and kidney; Can also carry out heredity by placenta, cause the offspring to distort.The Chinese adult male sex on average consumes 10 cigarette for each person every day, and the average annual aggregate consumption of cigarette has reached 18,000 hundred million, accounts for 1/3rd of global aggregate consumption.The crowd who is subjected to the cigarette smoke influence reaches several hundred million crowds in China.Slightly different with benzo (a) pyrene (promptly 3,4-benzopyrene) and bioxin, low therefore easier the evaporateing in the cigarette smoke of the boiling point of nitrosamine, contaminated environment also injures the healthy of people.Increasing expert thinks that the content of nitrosamines in the cigarette will be the 3rd parameter should indicating on cigarette case after T/N, and should reduce as much as possible.
In order to reduce the pollution of nitrosamine from the source, the timely content of nitrosamines of grasping in the raw tobacco in the time of just need and making cigarette the purchase tobacco.Usually detect the method for the content of nitrosamines in tobacco and the smoke of tobacco: (1) external main chromatogram-thermal energy analyzer (GC-TEA) method of using, but these methods all relate to expensive instrument and cross complicated operations programs such as post separates, and are difficult to apply in grass-roots unit; Moreover producer only need know roughly that the nitrosamine total amount in the tobacco gets final product, and does not need nitrosamine is separated accurate mensuration concentration separately one by one.(2) extract nitrosamine with chemical solution leaching tobacco, extraction then-concentrate and measure needs 2 day time at least.(3) the applicant is at patented claim (publication number: disclose the content of nitrosamines in a kind of improvement type spectrophotometry smoke of tobacco CN1193741A), but be mainly used in the mensuration of finished cigarettes.This just requires at first tobacco leaf to be made cigarette; Yet refire mensuration after making cigarette by the time, every cigarette burns in airflow and also needs about 20 minutes, not only consuming time taking a lot of work, and can't instruct production to reduce the content of nitrosamines in the product.Obviously, press for the method for measuring the content of nitrosamines in the raw tobacco fast and quickly and easily.Nitrite in the tobacco and nitrate at high temperature decompose the oxides of nitrogen (NO of generation
x), can with nicotine or amine thermal synthesis nitrosamine once more, therefore be counted as the precursor compound that produces nitrosamine.In addition, the microwave radiation tobacco leaf also can make some nitrosamine decompose and generate NO
xSo, the amount of nitrogen oxides (NO in the tobacco leaf
x) and content of nitrosamines important relation is arranged.But, if, can't measure oxides of nitrogen (NO simultaneously with the nitrosamine in the solution leaching method mensuration tobacco
x) content.Light a cigarette when collecting flue gas also because the interference of impurity such as tar is difficult to measure the content in the flue gas; Obviously, equally also press for new tool and measure oxides of nitrogen (NO in the raw tobacco fast and quickly and easily
x) content.
The purpose of this invention is to provide nitrosamine and oxides of nitrogen (NO in a kind of simple and direct, fast measuring tobacco
x) new method of content.
The aliphatics nitrosamine is strong polar organic matter, and the N-NO key is weaker than C-H, C-C, C-N key in the functional group, can be disconnected in 300 ℃ pyrolytic reaction and produces NO
xFine jade Buddhist nun R William Si discloses dried after microwave radiation is used for tobacco and hemp results, has reduced the technology of its tobacco-specific nitrosamine content in its patented claim WO9805226 and WO9858555 and CN97198261, use the destruction at the sub-nitrosamine of tobacco leaf.But we find that the nitrosamine of significant proportion is volatilized under microwave radiation, and have set up method of the present invention based on this new discovery.
Therefore technical scheme of the present invention is as follows:
Nitrosamine and oxides of nitrogen (NO in a kind of fast detecting tobacco
x) microwave-spectra photometric method of content, it is:
1. pipe tobacco or tobacco leaf are placed and carry out microwave radiation in the container;
2. use the carrier gas of inertia with decomposition product NO
xGo out with the nitrosamine stripping that volatilizes;
3. the nitrosamine that blows out is absorbed with citric acid-sodium dihydrogen phosphate buffer;
4. unabsorbed NO
xUse CrO
3Oxidation tube is oxidized to NO
2
5.NO
2Absorb with quantitative sulfanilamide (SN), hydrochloride naphthodiamide solution, be converted into NO
2 -And colour developing;
6. measure its absorbance in wavelength 540nm place, calculate oxides of nitrogen (NO
x) content Y
1
7. with the absorption liquid dichloromethane extraction of step 3;
8. the dichloromethane solution anhydrous Na after will extracting
2SO
4Dry;
With dried dichloromethane solution at N
2Gas shiled concentrates down;
10. the N-NO of HBr-HOAc solution of the dichloromethane solution after will concentrating with the N-nitroso compound
N-N bond cleavage in the functional group is separated;
11. will decompose the NO that produces with the carrier gas of inertia
xStripping goes out;
12. the gas that stripping goes out purifies through alkaline Drexel bottle;
13. the NO after will purifying
xUse CrO
3Oxidation tube is oxidized to NO
2
14.NO
2Absorb, be converted into NO with quantitative sulfanilamide (SN), hydrochloride naphthodiamide solution
2 -And colour developing;
15. measure its absorbance with wavelength 540nm place, calculate the content Y of nitrosamine
2
Microwave spectrophotometric process of the present invention, used microwave can be that frequency is the microwave of 2450MHz or 915MHz, the power of microwave radiation is 500-2000W, preferred power is 800-1000W, radiated time is 30-400 second, and preferred radiated time is 60-220 second, and the carrier gas of inertia can be high-purity nitrogen, helium or argon gas, the flow velocity of carrier gas is 10-500mL/min, and preferred speed is to be 100-140mL/min.Used nitrosamine absorption liquid is that PH is citric acid-sodium dihydrogen phosphate buffer of 4.5, used CrCO
3Oxidation tube is filling CrO
3 -The oxidation tube of sea sand.
Measure these nitrosamine and oxides of nitrogen NO by method of the present invention
x, just can understand the content of nitrosamines in the raw tobacco roughly.The advantage of the inventive method is: contain volatility, the non-volatile and distinctive nitrosamine of tobacco in (1) tobacco and the smoke of tobacco, the main harm environment be that those can evaporate into the nitrosamine in the flue gas, exactly also be those nitrosamine that can volatilize and microwave method detects.(2) Nitrates in the tobacco can decompose generation oxides of nitrogen (NO when cigarette burning
x), go out some nitrosamine with nicotine and amine thermal synthesis.With the nitrosamine in the solution leaching tobacco, can't reflect that owing to carry out at normal temperatures this high temperature changes.Microwave radiation meeting spot heating pipe tobacco is so the content in data that obtain and the cigarette gas is comparatively approaching.(3) microwave method can detect pipe tobacco, tobacco leaf, is not subjected to the restriction of sample shape, does not also require to be rolled into cigarette.Compare with the collection flue gas determination method that lights a cigarette, microwave method is consuming time shorter, only needs just nitrosamine to be collected in the solution about 3 minutes, for mensuration.(4) with the raw material tobacco directly through microwave treatment, required small investment, technology are simple and be suitable for applying in grass-roots unit.
Further specify the present invention by the following examples.
[example 1] is with cigarette A (fire-cured tobacco type, is produced from Yunnan Province, tar content is that 15mg/ props up, nicotine content in smoke is that 1.2mg/ props up) pipe tobacco (16 cigarette) place and be placed on the WP850D micro-wave oven in the container, behind container, connect the Drexel bottle of 4 series connection, respectively fill pH value in the Drexel bottle and be citric acid-sodium dihydrogen phosphate buffer 15mL of 4.5, absorb the nitrosamine that volatilizes, connect a two ball oxidation tube after the Drexel bottle, the CrO about oxidation casing pack 8 grams
3 -Sea sand (mass ratio is 1: 20) connects an absorption bottle behind the oxidation tube, 50.0mL colour developing liquid (5 gram sulfanilamide (SN) and 0.05 gram hydrochloride naphthodiamide are dissolved in the 1000mL distilled water that contains the 50mL glacial acetic acid) is housed, with carrier gas N in the absorption bottle
2The container of flowing through, N
2Flow velocity be 100mL/min, start micro-wave oven and carry out radiation, power is 850W, radiated time is 70 seconds, pipe tobacco decomposes the NO that produces in the container
xBlown out by carrier gas with the nitrosamine that volatilizes, the nitrosamine of volatilization is absorbed by Drexel bottle, decomposes the NO that produces
xOxidized pipe is oxidized to NO
2, entering in the colour developing bottle, radiation finishes the back with colorimetric method for determining (540nm place), calculates NO
2 -Content Y
1, in addition the buffer solution in four Drexel bottles is merged, extract nitrosamine with methylene chloride, use improved spectrophotometric method (referring to CN97107228.0A) to detect NO then
2 -Content Y
2, the content of nitrosamine is Y in the pipe tobacco
2The content that records cigarette A nitrosamine is that 2.50nmol/ props up, oxides of nitrogen (NO
x) content be that 10.01nmol/ props up.Repeated experiments 2 times, measure content of nitrosamines be respectively 2.48 and 2.63nmol/ prop up (NO
x) content be respectively 9.80 and 10.11nmol/ prop up.The error of three secondary data and mean value is respectively 1.6%, 2.4% and 3.5% for nitrosamine, for NO
xBe respectively 0.4%, 1.7% and 1.4%.
[example 2] puts into container such as embodiment 1 assay method and measure content of nitrosamines, but radiated time changes pipe tobacco (12) cigarette of cigarette B (tar content is that 18mg/ props up for fire-cured tobacco type, Jiangsu Province's product, and nicotine content in smoke is that 1.4mg/ props up) 210 seconds into, N
2Flow velocity change 120mL/min into, twice measurement result, the total content of nitrosamine is respectively 3.17nmol/ and props up with 3.13nmol/ and prop up.The error of two secondary data is 1.3%.
[example 3] is with cigarette C (fire-cured tobacco type, is produced from Jiangsu Province, tar content is that 17mg/ props up, nicotine content in smoke is that 1.1mg/ props up), add 3%m/m poriness scavenging material in pipe tobacco after, the side-stream smoke content of nitrosamines props up from 4.57nmol/ and is reduced to 2.31nmol/ and props up, and has reduced 49.5%, (method of testing is seen patent application publication number CN1193741A, down together).Get pipe tobacco (20 cigarette) and press the content that the method for embodiment 1 is measured nitrosamine in the pipe tobacco, radiated time is 210 seconds, N
2Flow velocity is 120mL/min, survey the pipe tobacco content of nitrosamines do not contain adjuvant and to contain adjuvant be respectively 4.88 and 2.74nmol/ prop up, the minimizing amplitude is 43.9%, reflects the effect of adjuvant exactly.
The side-stream smoke content of nitrosamines of [example 4] cigarette D (tar content is that 15mg/ props up for fire-cured tobacco type, U.S.'s product, and nicotine content in smoke is that 1.3mg props up) is that 6.65nmol/ props up.The side-stream smoke content of nitrosamines of cigarette E (tar content is that 12mg/ props up for fire-cured tobacco type, Britain's product, and nicotine content in smoke is that 1.0mg/ props up) is that 3.65nmol/ props up, and is 54.9% of cigarette D.The content of nitrosamines that the pipe tobacco of the two is measured through microwave spectrophotometric process of the present invention (radiation is 210 seconds under the 850W power) be respectively 3.00 and 1.85nmol/ prop up, cigarette E is 61.7% of cigarette D, reflects the gap of the two.
The side-stream smoke content of nitrosamines of [example 5] cigarette F (tar content is that 12mg/ props up for mixed type, U.S.'s product, and nicotine content in smoke is that 1.0mg props up) is that 4.17nmol/ props up.The side-stream smoke content of nitrosamines of cigarette G (tar content is that 11mg/ props up for mixed type, Yunnan Province's product, and nicotine content in smoke is that 1.0mg props up) is that 3.00 nmol/ prop up, and is 71.9% of cigarette F.The content of nitrosamines that the pipe tobacco of the two is measured through microwave spectrophotometric process of the present invention (radiation is 210 seconds under the 850W power) be respectively 3.45 and 2.65nmol/ prop up, cigarette G is 75.9% of cigarette F, the two gap of measuring with ignition method is close.
As from the foregoing, can fast measuring nitrosamine and oxides of nitrogen (NO wherein in conjunction with the improvement type spectrophotometric method with tobacco with microwave radiation
x) content, good reproducibility not only, and can reflect the difference of different tobaccos.Technical application of the present invention is strong, and equipment needed thereby is few and with low cost, measures easy, weak point consuming time, be adapted at cigar mill and other tobacco departments and apply, develop new cigarette, and then gradually reduce the pollution of smoking for environment to grasp the content of nitrosamines in the tobacco.
Claims (4)
- -kind of fast detecting tobacco in nitrosamine and oxides of nitrogen (NO x) microwave-spectra photometric method of content, it is characterized in that:(1) pipe tobacco or tobacco leaf placed carry out microwave radiation in the container,(2) use the carrier gas of inertia with NO xGo out with the nitrosamine stripping that volatilizes,(3) nitrosamine that blows out is absorbed with citric acid-sodium dihydrogen phosphate buffer,(4) unabsorbed NO xUse CrO 3Oxidation tube is oxidized to NO 2,(5) NO 2Absorb with quantitative sulfanilamide (SN), hydrochloride naphthodiamide solution, be converted into NO 2 -And colour developing,(6) measure its absorbance in wavelength 540nm place, calculate the content Y of oxides of nitrogen 1,(7) with the absorption liquid dichloromethane extraction of step 3,(8) the dichloromethane solution anhydrous Na after will extracting 2SO 4Drying,(9) with dried dichloromethane solution at N 2Gas shiled concentrates down,(10) dichloromethane solution after will concentrating is with the N-of HBr-HOAc solution with the N-nitroso compoundN-N bond cleavage in the NO functional group is separated,(11) will decompose the NO that produces with the carrier gas of inertia xStripping goes out,(12) gas that goes out of stripping purifies through alkaline Drexel bottle,(13) NO after will purifying xUse CrO 3Oxidation tube is oxidized to NO 2,(14) NO 2Absorb, be converted into NO with quantitative sulfanilamide (SN), hydrochloride naphthodiamide solution 2 -And colour developing,(15) measure its absorbance with wavelength 540nm place, calculate the content Y of nitrosamine 2,
- 2. microwave spectrophotometric process according to claim 1, the frequency that it is characterized in that used microwave is 2450MHz or 915MHz, power is 500-2000W.
- 3. microwave spectrophotometric process according to claim 1, the time that it is characterized in that radiation is 30-400 second.
- 4. microwave spectrophotometric process according to claim 1, the carrier that it is characterized in that used inertia is a nitrogen, helium or argon gas, gas flow rate are 10-500mL/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00134373.4A CN1121158C (en) | 2000-12-08 | 2000-12-08 | Microwave spectrophotometric process for the fast detection of nitrosamine and nitroxide content in tobacco |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00134373.4A CN1121158C (en) | 2000-12-08 | 2000-12-08 | Microwave spectrophotometric process for the fast detection of nitrosamine and nitroxide content in tobacco |
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| Publication Number | Publication Date |
|---|---|
| CN1298096A true CN1298096A (en) | 2001-06-06 |
| CN1121158C CN1121158C (en) | 2003-09-17 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2292106A3 (en) * | 2002-07-18 | 2011-06-01 | Phasex Corporation | Reduction of constituents in tobacco |
| CN102087177A (en) * | 2010-11-19 | 2011-06-08 | 红塔烟草(集团)有限责任公司 | Absorption solution and method for recognizing smoke smell |
| CN102894469A (en) * | 2012-10-31 | 2013-01-30 | 河南中烟工业有限责任公司 | CO2 flow extraction process for reducing tar and harmful components of tobacco |
| CN105353068A (en) * | 2015-12-09 | 2016-02-24 | 中国烟草总公司郑州烟草研究院 | GC-MS/MS assay determination method for volatile N-nitrosamine in tobacco and smokeless tobacco products |
-
2000
- 2000-12-08 CN CN00134373.4A patent/CN1121158C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2292106A3 (en) * | 2002-07-18 | 2011-06-01 | Phasex Corporation | Reduction of constituents in tobacco |
| US8555895B2 (en) | 2002-07-18 | 2013-10-15 | U.S. Smokeless Tobacco Company Llc | Reduction of constituents in tobacco |
| US10045557B2 (en) | 2002-07-18 | 2018-08-14 | Us Smokeless Tobacco Co. | Reduction of constituents in tobacco |
| CN102087177A (en) * | 2010-11-19 | 2011-06-08 | 红塔烟草(集团)有限责任公司 | Absorption solution and method for recognizing smoke smell |
| CN102894469A (en) * | 2012-10-31 | 2013-01-30 | 河南中烟工业有限责任公司 | CO2 flow extraction process for reducing tar and harmful components of tobacco |
| CN102894469B (en) * | 2012-10-31 | 2014-12-24 | 河南中烟工业有限责任公司 | CO2 flow extraction process for reducing tar and harmful components of tobacco |
| CN105353068A (en) * | 2015-12-09 | 2016-02-24 | 中国烟草总公司郑州烟草研究院 | GC-MS/MS assay determination method for volatile N-nitrosamine in tobacco and smokeless tobacco products |
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