CN101598709B - Method for determining fragrance stabilizing capacity of tobacco humectant on additional flavors in cut tobaccos - Google Patents
Method for determining fragrance stabilizing capacity of tobacco humectant on additional flavors in cut tobaccos Download PDFInfo
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- CN101598709B CN101598709B CN2009100654014A CN200910065401A CN101598709B CN 101598709 B CN101598709 B CN 101598709B CN 2009100654014 A CN2009100654014 A CN 2009100654014A CN 200910065401 A CN200910065401 A CN 200910065401A CN 101598709 B CN101598709 B CN 101598709B
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Abstract
A method for determining the fragrance stabilizing capacity of a tobacco humectant on additional flavors in cut tobaccos aims at determining the fragrance stabilizing ratio of the tobacco humectant to the additional flavors in the cut tobaccos mainly by comparing the contents of the additional flavors in the cut tobaccos before and after the humectant is added. The method is characterized by taking two parts of flavored cut tobaccos in the same mass, one part of which is added with the evenly distributed humectant; after a certain period of placement, using dichloromethane solution containing certain concentration of standard substances for ultrasonic extraction; after filtration by microfiltration membranes, employing gas chromatography/mass spectrometer instruments for determination and determining the content of the additional flavor ingredients by time retention and mass spectral database retrieval; comparing the quantity of the additional flavors in the cut tobaccos added with the humectant with the quantity of the additional flavors in the cut tobaccos without the humectant, thereby determining the fragrance stabilizing ratio of the tobacco humectant to the additional flavors in the cut tobaccos. The method can rapidly and correctly judge the fragrance stabilizing capacity of the tobacco humectant on the additional flavors in the cut tobaccos and has the advantages of simple process, fast analysis speed, certain resistance to interference of external factors and the like.
Description
Technical field
The invention belongs to the Food Science field, relate to a kind of method of measuring tobacco humectant to pipe tobacco China and foreign countries perfuming fixation ability.Mainly be to add the spiced content in pipe tobacco China and foreign countries, humectant front and back, determine that tobacco humectant is to the spiced fixation ability in pipe tobacco China and foreign countries by contrast.
Background technology
Along with to Chinese style cigarette style and features understanding deepen continuously and China's cigarette brand is integrated the continuous propelling of expansion, industry is had higher requirement to cigarette flavouring humectation technology.
Tobacco humectant is in production of cigarettes, transportation, storage, sale and sucking process, has the maintenance moisture content in leaves, increase pliability, reduce make broken, reduce pungency and improve jealous effect, therefore the tobacco worker of various countries has carried out studying (Liu Li congruence, the research of humectant and application progress Shanghai cigarette industry .1998 (1): 10-13.) to the humectation effect and the influence jealous to cigarette and that smoke chemistry is formed thereof of various materials.
Humectant commonly used has polyalcohols; also have sugar and glycitols, organic salt, natural extract and bionical protective agent etc. in addition; (Stoilova, COMPARATIVE INVESTIGATIONS OF THE INFLUENCEOF POL YVALENT ALCOHOLS AND FRUIT EXTRACTS ON THE PHYSI
At present, in pipe tobacco, keep the spices Research on ability to yet there are no report to humectant.
Summary of the invention
The present invention just is being based on the problems referred to above, and a kind of method of measuring tobacco humectant to pipe tobacco China and foreign countries perfuming fixation ability that proposes, add the spiced content in pipe tobacco China and foreign countries, humectant front and back by contrast, and then definite tobacco humectant is to the spiced fixation ability in pipe tobacco China and foreign countries.
The objective of the invention is to realize by following technical measures:
Mensuration tobacco humectant of the present invention is to add the spiced content in pipe tobacco China and foreign countries, humectant front and back by contrast to the method for pipe tobacco China and foreign countries perfuming fixation ability, determines tobacco humectant to the spiced fixation rate in pipe tobacco China and foreign countries, and its concrete steps are as follows:
1), sample is prepared: get two equal portions aromatic tobacco samples, a copy of it adds humectant, and guarantees that humectant is evenly distributed;
2), sample places: step 1) gained sample respectively after 48-72h is placed in thermostatic constant wet chamber's (22 ± 2 ℃, RH 60 ± 5%) sealing, is opened wide fully and placed 4-10h hour;
3), sample pre-treatments: the dichloromethane solution that usefulness contains the finite concentration standard substance carries out ultrasonic Extraction 20-40 minute to pipe tobacco, and is standby behind the 0.2-0.5um filtering with microporous membrane;
4), instrumental analysis: determine gas chromatography, mass spectrometer and condition and sample is detected according to the character of target fragrances, determine to add the content of fragrance component by retention time and mass spectrometric data library searching;
5), the fixation rate is calculated: fixation rate=(add behind the humectant adding in the pipe tobacco amount of flavorants/the do not add amount of flavorants that adds in the humectant pipe tobacco) * 100%;
6), according to the fixation rate, judge the external spiced fixation ability of this humectant.
In the present invention, gas chromatography, mass spectrometer and condition are to determine according to the character of target fragrances.
When target fragrances was alcohols spices, its gas chromatography, mass spectrometer and condition were:
Chromatographic column: HP-5 (5% phenyl polysiloxane) capillary column 60m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 70 ℃, keep 1min; Rise to 260 ℃ with 2 ℃/min speed, keep 30min;
Carrier gas: helium, 1.0mL/min;
Sample size 1 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
When target fragrances when containing ketone fragrance, its gas chromatography, mass spectrometer and condition are:
Chromatographic column: DB-5 quartz elastic capillary tube chromatographic column (30m * 0.25mm * 0.25mm injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 280 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 5.5min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
When target fragrances was ester perfume, its gas chromatography, mass spectrometer and condition were:
Chromatographic column: HP-5 capillary column 50m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 270 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
The used aromatic tobacco sample size of the present invention is 5-10mg.
Characteristics of the present invention are: can judge tobacco humectant rapidly and accurately to the spiced fixation ability in pipe tobacco China and foreign countries, have that technology is simple, analysis speed is fast, be difficult for by advantages such as extraneous factor interference.
Description of drawings
Accompanying drawing is the process chart of assay method of the present invention.
Embodiment
The present invention is further described below in conjunction with embodiment, but does not limit the present invention.
Embodiment one,
1, getting two equal portions quality is the pipe tobacco that 7.982g alcohols flavour content is about 150ppm, a copy of it add mass percent be 1/10000 (pipe tobacco) humectant A (for example: hyaluronic acid ten thousand/aqueous solution), and guarantee that humectant is evenly distributed;
2, with 1 gained sample respectively after 48h is placed in thermostatic constant wet chamber's (22 ± 2 ℃, RH 60 ± 5%) sealing, open wide fully and place 8h;
3, the dichloromethane solution that contains 150ppm phenethyl acetate (chromatographically pure) with 20ml is to pipe tobacco ultrasonic Extraction 35 minutes, and is standby behind the 0.45um filtering with microporous membrane;
4, gas chromatography/mass spectrometry condition:
Chromatographic column: HP-5 (5% phenyl polysiloxane) capillary column 60m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 70 ℃, keep 1min; Rise to 260 ℃ with 2 ℃/min speed, keep 30min;
Carrier gas: helium, 1.0mL/min;
Sample size 1 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev;
5, humectant A is respectively the fixation rate of each spices:
Illustrate that humectant A has stronger fixation ability to these alcohols spices.
Embodiment two,
1, getting two equal portions quality is that 8.597g contains the pipe tobacco about ketone fragrance 100ppm, and it is the humectant B of 5/1000 (pipe tobacco) that a copy of it adds mass percent, and guarantees that humectant is evenly distributed;
2, with 1 gained sample respectively after 72h is placed in thermostatic constant wet chamber's (22 ± 2 ℃, RH 60 ± 5%) sealing, open wide fully and place 6h;
3, the dichloromethane solution that contains 100ppm phenethyl acetate (chromatographically pure) with 20ml is to pipe tobacco ultrasonic Extraction 40 minutes, and is standby behind the 0.45um filtering with microporous membrane;
4, gas chromatography/mass spectrometry condition:
Chromatographic column: DB-5 quartz elastic capillary tube chromatographic column (30m * 0.25mm * 0.25mm injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 280 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 5.5min; Ion source temperature: 230 ℃; Electronic voltage: 70ev;
5, humectant B is respectively the fixation rate of spices:
Illustrate that humectant B has stronger fixation ability to these ketones.
Embodiment three,
1, getting two equal portions quality is the pipe tobacco that 8.127g ester perfume content is about 167ppm, and it is the humectant C of 1/5000 (pipe tobacco) that a copy of it adds mass percent, and guarantees that humectant is evenly distributed;
2, with 1 gained sample respectively after 60h is placed in thermostatic constant wet chamber's (22 ± 2 ℃, RH 60 ± 5%) sealing, open wide fully and place 10h;
3, the dichloromethane solution that contains 150ppm phenethyl acetate (chromatographically pure) with 20ml is to pipe tobacco ultrasonic Extraction 30 minutes, and is standby behind the 0.45um filtering with microporous membrane;
4, gas chromatography/mass spectrometry condition:
Chromatographic column: HP-5 capillary column 50m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 270 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev;
5, humectant C is respectively the fixation rate of selected spices:
Illustrate that humectant C has stronger fixation ability to these ester classes.
Claims (7)
1. method of measuring tobacco humectant to pipe tobacco China and foreign countries perfuming fixation ability, it is characterized in that: add the spiced content in pipe tobacco China and foreign countries, humectant front and back by contrast, determine tobacco humectant to the spiced fixation rate in pipe tobacco China and foreign countries, its concrete steps are as follows:
1), sample is prepared: get two equal portions aromatic tobacco samples, a copy of it adds humectant, and guarantees that humectant is evenly distributed;
2), sample places: step 1) gained sample respectively after 48-72h is placed in thermostatic constant wet chamber's sealing, is opened wide fully and placed 4-10h hour;
3), sample pre-treatments: pipe tobacco is extracted after standby behind the 0.2-0.5um filtering with microporous membrane with the dichloromethane solution that contains the finite concentration standard substance;
4), instrumental analysis: determine gas chromatography, mass spectrometer and condition and sample is detected according to the character of target fragrances, determine to add the content of fragrance component by retention time and mass spectrometric data library searching;
5), the fixation rate is calculated: fixation rate=(add behind the humectant adding in the pipe tobacco amount of flavorants/the do not add amount of flavorants that adds in the humectant pipe tobacco) * 100%;
6), according to the fixation rate, judge the external spiced fixation ability of this humectant.
2. mensuration tobacco humectant according to claim 1 is to the method for pipe tobacco China and foreign countries perfuming fixation ability, and it is characterized in that: gas chromatography, mass spectrometer and condition are to determine according to the character of target fragrances.
3. mensuration tobacco humectant according to claim 2 is to the method for pipe tobacco China and foreign countries perfuming fixation ability, and it is characterized in that: when target fragrances was alcohols spices, its gas chromatography, mass spectrometer and condition were:
Chromatographic column: HP-5 capillary column 60m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 70 ℃, keep 1min; Rise to 260 ℃ with 2 ℃/min speed, keep 30min;
Carrier gas: helium, 1.0mL/min;
Sample size 1 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
4. mensuration tobacco humectant according to claim 2 is characterized in that the method for pipe tobacco China and foreign countries perfuming fixation ability: when target fragrances when containing ketone fragrance, its gas chromatography, mass spectrometer and condition are:
Chromatographic column: DB-5 quartz elastic capillary tube chromatographic column 30m * 0.25mm * 0.25mm, injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 280 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 5.5min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
5. mensuration tobacco humectant according to claim 2 is to the method for pipe tobacco China and foreign countries perfuming fixation ability, and it is characterized in that: when target fragrances was ester perfume, its gas chromatography, mass spectrometer and condition were:
Chromatographic column: HP-5 capillary column 50m * 0.20mm * 0.50 μ m;
Injector temperature: 250 ℃;
Temperature programme: 60 ℃, keep 1min; Rise to 270 ℃ with 3 ℃/min speed, keep 40min;
Carrier gas: helium, 1.0mL/min;
Sample size 2 μ L, split sampling, split ratio 10: 1;
Transmission line temperature: 280 ℃; The solvent delay time: 6min; Ion source temperature: 230 ℃; Electronic voltage: 70ev.
6. mensuration tobacco humectant according to claim 1 is to the method for pipe tobacco China and foreign countries perfuming fixation ability, and it is characterized in that: described extracting mode is Extraction by Ultrasound 20-40 minute.
7. mensuration tobacco humectant according to claim 1 is to the method for pipe tobacco China and foreign countries perfuming fixation ability, and it is characterized in that: the aromatic tobacco sample size is 5-10mg.
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| CN104198457B (en) * | 2014-09-04 | 2017-02-08 | 国家烟草质量监督检验中心 | Cut tobacco component recognition method based on spectral imaging technology |
| CN106198861B (en) * | 2016-06-30 | 2018-07-20 | 云南中烟工业有限责任公司 | A kind of method of quantitatively evaluating cigarette shreds and humectant compatibility |
| CN108088946A (en) * | 2017-10-21 | 2018-05-29 | 云南中烟工业有限责任公司 | A kind of cigarette flavors additive distribution determination method under flue gas different-grain diameter |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292499A (en) * | 1999-07-06 | 2001-04-25 | 川崎制铁株式会社 | Method and device for analysing free fluorine in solution containing hydrofluoric acid |
| CN1479870A (en) * | 2000-12-05 | 2004-03-03 | ���������Ǵ�ѧ���»� | Optical determination of glucose utilizing boronic acid adducts |
| CN1851456A (en) * | 2006-03-30 | 2006-10-25 | 上海大学 | Formaldehyde, methanol and N,N dimethyl hydroxyamine coexisting anlytical method |
| CN1936577A (en) * | 2006-03-30 | 2007-03-28 | 上海大学 | Analysis method while alcohol, aldehyde, acetic acid, nitroethane and N,N-diethylated hydroxylammonium hydroxylamine common existing |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1292499A (en) * | 1999-07-06 | 2001-04-25 | 川崎制铁株式会社 | Method and device for analysing free fluorine in solution containing hydrofluoric acid |
| CN1479870A (en) * | 2000-12-05 | 2004-03-03 | ���������Ǵ�ѧ���»� | Optical determination of glucose utilizing boronic acid adducts |
| CN1851456A (en) * | 2006-03-30 | 2006-10-25 | 上海大学 | Formaldehyde, methanol and N,N dimethyl hydroxyamine coexisting anlytical method |
| CN1936577A (en) * | 2006-03-30 | 2007-03-28 | 上海大学 | Analysis method while alcohol, aldehyde, acetic acid, nitroethane and N,N-diethylated hydroxylammonium hydroxylamine common existing |
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