CN106248843A - A kind of quantitative forecasting technique of Medicated cigarette medicinal herbs odor type - Google Patents
A kind of quantitative forecasting technique of Medicated cigarette medicinal herbs odor type Download PDFInfo
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- CN106248843A CN106248843A CN201610795895.1A CN201610795895A CN106248843A CN 106248843 A CN106248843 A CN 106248843A CN 201610795895 A CN201610795895 A CN 201610795895A CN 106248843 A CN106248843 A CN 106248843A
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- medicated cigarette
- medicinal herbs
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
Abstract
The invention discloses a kind of detection based in Medicated cigarette 20 kinds of volatile component contents to come Medicated cigarette medicinal herbs odor type quantitative forecasting technique.The sample treatment first set up according to independent development and GC MS/MS analyze method and are measured the content of in tobacco shred 20 kinds of volatile ingredients, and then the content of mensuration be brought in regression equation calculating YHerbalNumerical value, be the predictive value of this kind of Medicated cigarette medicinal herbs odor type quantitative forecasting technique score, in the range from 0 10 points.Quantitative forecasting technique smoking result actual with the sense organ goodness of fit of the Medicated cigarette medicinal herbs odor type of the present invention is preferable, it was predicted that mean absolute error be 0.1085 point.The technical support favourable for safeguarding the stable offer of Sensory Quality of Cigarette.
Description
Technical field
The invention belongs to quantitative forecast and the control field of Medicated cigarette medicinal herbs odor type, be specifically related to a kind of based in cigarette shreds
The detection of 20 kinds of volatile component contents, and combine regression coefficient and build quantitative to Medicated cigarette medicinal herbs odor type of method of regression model
Forecasting Methodology.
Background technology
Stable and the lifting of cigarette product quality, it is critical only that the stable of organoleptic quality and promotes, how setting up Medicated cigarette sense
The evaluation methodology of official's quality always is the study hotspot of industry.At present, expert is mainly passed through in the evaluation of cigarette sensory quality
Sensory evaluating smoking carry out, and issued and implemented concerned countries and industry standard.Such as, GB 5606.4-2005 " Medicated cigarette the 4th
Part: sense organ technology requires " and YC/T 497-2014 " Medicated cigarette Chinese-style cigarette style sensory evaluation method ".But due to the person of smokeing panel test
In smokeing panel test, there is subjectivity, make the repeatability of smoking result and stability there is certain deficiency, to such an extent as to evaluation result
Reliability produce impact.
There is internal relation between the organoleptic feature of Medicated cigarette and its chemical composition, different chemical component can be special to Medicated cigarette sense organ
Levy the impact produced in various degree.In recent years, Medicated cigarette sensory evaluation and the Study on Forecasting Method of chemically based composition there has also been relatively
Many reports.Such as, the not magnificence etc. of Harbin Engineering University provides one and predicts volume by immune neural net algorithm
The method (CN 101419209 A) of cigarette sensory evaluating smoking and fume indication, but its component substances including computation modeling in is only total
Sugar, total nicotine, reducing sugar etc. more than 10 plant routine chemical components index, and it cannot represent the overall permanence of Medicated cigarette sense organ.Yizhong cigarette
The Hu Shengguo etc. of grass (group) company limited has invented the BP neural network model of a kind of combination FUZZY SET APPROACH TO ENVIRONMENTAL, and uses this mould
Medicated cigarette sensory evaluating smoking and fume indication are predicted (CN 1525394 A) by type, but it is for the chemical composition modeled and calculate
Up to 110 remainders, Indexs measure is qualitative, the most loaded down with trivial details, and difficulty in computation is bigger.In turn result in it predict the outcome relatively low or not may be used
The shortcoming such as lean on.
Summary of the invention
Present invention aims to and overcome the deficiencies in the prior art, it is provided that a kind of quantitative to Medicated cigarette medicinal herbs odor type
Forecasting Methodology, to simplify the flow process of the quantitative forecast of Medicated cigarette medicinal herbs odor type, thus completes fast and accurately to Medicated cigarette medicinal herbs odor type
Quantitative forecast work.
The purpose of the present invention is achieved by the following technical programs.
The quantitative forecasting technique of a kind of Medicated cigarette medicinal herbs odor type, comprises the following steps:
(1) the 2-methylpyrazine in cigarette sample to be predicted, alpha-angelica lactone, 2,3,5-trimethylpyrazine, acetic acid are measured
Phenethyl ester, methyl cyclopentenyl ketone, β-caryophyllene, 3,5,5-trimethyl-cyclohexane-1,2-diketone, oxidation isophorone, L-are thin
Lotus alcohol, D-menthol, fenchene, δ-nonalactone, 2,6-lutidines, dihydro tonquin butter, eugenol, γ-hexalactone, benzene second
Aldehyde, phenethanol, 2-methyltetrahydrofuran-3-ketone, the mass percentage content of these 20 kinds of materials of γ-decalactone, respectively with X1Extremely
X20Represent;
(2) by X1To X20Substitute in following regression equation respectively, calculate YHerbalNumerical value:
YHerbal=10.169X1+10.018X2+9.729X3+9.429X4-9.538X5-9.135X6+8.953X7+8.636X8-
8.571X9+8.235X10-8.229X11+7.318X12-7.129X13+7.086X14-7.428X15-7.035X16+6.053X17+
6.036X18-6.071X19+4.235X20-197.475;
(3) Y of gained is calculatedHerbalNumerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette medicinal herbs odor type, its scope
Divide for 0-10.
Listing in table 1 below for above-mentioned 20 kinds of substance to be measured, the quantitative forecast of Medicated cigarette medicinal herbs odor type is obtained by it
The regression equation coefficient divided.
Table 1 regression equation coefficient
Relative to prior art, the invention have the advantages that
1, the present invention 20 kinds of volatile component contents from cigarette shreds, it is possible to be given more than sensory evaluating smoking method
Objective, stable result of determination, eliminates the impact of artificial difference in sensory evaluating smoking.
2, the material quantitative forecast score prediction as Medicated cigarette medicinal herbs odor type of the plurality of classes such as pyrazine, ester, ketone, alcohol is used
Foundation, more accurate than existing method.
3, use less material for modeling the quantitative forecast to Medicated cigarette medicinal herbs odor type, have and detect speed faster
Degree, the quantitative flow process relatively simplified, it is to avoid the problem of regression modeling overfitting, the result making quantitative forecast is accurate and reliable.
The technical support favourable for safeguarding the stable offer of Sensory Quality of Cigarette.
Accompanying drawing explanation
Fig. 1: 30 kinds of sample regression value of calculation and the hyperbolic chart of sensory evaluating smoking's result.
Detailed description of the invention
By the following examples the present invention is described in further detail, but specific embodiment is not to skill of the present invention
The restriction of art scheme.
Embodiment 1
(box mark tar 8-12mg/ props up, and box mark nicotine 0.6-1.2mg/ props up, box mark to buy 30 kinds of domestic commercially available finished cigarettes
CO 9-13mg/ props up, and 2015 respectively purchased from markets such as Kunming, Shanghai City, Changshas);Collected sample is according to YC/T
497-2014 carries out sensory evaluation, determines that its herbal style and features sensory evaluating smoking's score range is that 0.5-4.0 divides.
A, sample treatment and analysis
The cigarette of the same brand taking Xin Kaibao at random carries out sample and prepares, and sample preparation quick and precisely, and should guarantee sample
Product are the most contaminated, and each laboratory sample prepares three parallel samples.Peel off cigarette paper and filter tip, take out tobacco shred, record weight, then
It is respectively put in 3 100ml conical flasks, as sample.The internal standard of 1mL 60 μ g/mL it is separately added in ready sample
Naphthalene, 9mL ether, close the lid rapidly and shake up, and is placed on concussion shaking table and shakes 2h, takes upper layer of extraction liquid through 0.22 μm with 10ml syringe
Filtering with microporous membrane, analyzes for GC-MS/MS (gas chromatography-mass spectrum/mass spectrograph).
B, gas chromatography-mass spectrum/mass spectral analysis condition
Chromatographic column: DB-5MS (30m × 0.25mm i.d. × 0.25 μm d.f., Agilent company of the U.S.) elastic quartz
Capillary chromatographic column;Injector temperature: 250 DEG C;Carrier gas: He, constant current mode, post flow 1mL/min, sample size: 1 μ L, shunting
Ratio: 10:1;Heating schedule: 50 DEG C (2min), with the ramp of 5 DEG C/min to 250 DEG C (20min);Transmission line temperature: 250
℃;Ionization mode: EI;Ion source temperature: 170 DEG C;Ionization energy 70eV;Heater current: 80 μ A;Full scan monitoring Full scan
Pattern, sweep limits: 10-500amu;Multiple-reaction monitoring MRM pattern, qualitative, quota ion is shown in Table 2 to Selection parameter.
20 kinds of volatile components and the qualitative ion pair of interior target in table 2 tobacco shred, quota ion to and collision energy
C, index assay
The retention time of test control, qualitative ion pair and quota ion pair, determine the target compound in sample.Work as examination
Sample and standard specimen at identical retention time (± 0.2min) occur, and the standard that the relative abundance of each qualitative ion is suitable with concentration
The ion relative abundance of solution is consistent, then can determine whether to exist in sample the measured object of correspondence.Each sample parallel measures 3 times.Root
According to volatility and the content of semi-volatile organic compounds in the quota ion calculated by peak area sample of target compound in sample.
In sample, the content of volatility and semi-volatile organic compounds is calculated by formula (1):
Wherein, Cs represents the content of a certain property material in sample, and unit is mg/kg;As be in sample volatility or
The peak area of semi-volatile organic compounds, unit is U (integration unit);Ai is the peak area of internal standard material, and unit is that U is (long-pending
Divide unit);Ci is the amount adding internal standard material, and unit is μ g/mL;M is for weighing tobacco quality, and unit is g;K is each volatility
Or the standard working curve slope of semi-volatile organic compounds;A is the standard of each volatility or semi-volatile organic compounds
Working curve intercept.
D, the 2-methylpyrazine according in method mensuration cigarette sample to be predicted described in a-c, alpha-angelica lactone, 2,3,5-tri-
Methylpyrazine, phenethyl acetate, methyl cyclopentenyl ketone, β-caryophyllene, 3,5,5-trimethyl-cyclohexane-1,2-diketone, oxidation
Isophorone, MENTHOL, D-menthol, fenchene, δ-nonalactone, 2,6-lutidines, dihydro tonquin butter, eugenol,
The content of 20 kinds of materials such as γ-hexalactone, hyacinthin, phenethanol, 2-methyltetrahydrofuran-3-ketone, γ-decalactone.Various things
The descriptive statistics of matter content detection result is shown in Table 3.
The descriptive statistics of 20 kinds of volatile material testing results in table 3 tobacco shred
Note: statistical sample number is: 30
E, the content detecting obtained 20 kind material in d is brought in following regression equation respectively, calculates YHerbal's
Numerical value:
YHerbal=10.169X1+10.018X2+9.729X3+9.429X4-9.538X5-9.135X6+8.953X7+8.636X8-
8.571X9+8.235X10-8.229X11+7.318X12-7.129X13+7.086X14-7.428X15-7.035X16+6.053X17+
6.036X18-6.071X19+4.235X20-197.475;
F, the Y of calculating gainedHerbalNumerical value, be the quantitative forecast score of this kind of Medicated cigarette medicinal herbs odor type.Calculate 30 respectively
Plant the Y of sampleHerbalNumerical value, and with sensory evaluating smoking's result comparison, result is as shown in Figure 1.The curve of diamond indicia is regression equation
Prediction score, and the square marks actual score of smokeing panel test that is sense organ.There it can be seen that use the Medicated cigarette medicinal herbs of forecast of regression model
Fragrant style and features sensory evaluating smoking's score is preferable with the actual smoking result goodness of fit, it was predicted that average MAE (mean absolute error)=
0.1085 point.
Claims (1)
1. a quantitative forecasting technique for Medicated cigarette medicinal herbs odor type, comprises the following steps:
(1) the 2-methylpyrazine in cigarette sample to be predicted, alpha-angelica lactone, 2,3,5-trimethylpyrazine, acetic acid benzene second are measured
Ester, methyl cyclopentenyl ketone, β-caryophyllene, 3,5,5-trimethyl-cyclohexane-1,2-diketone, oxidation isophorone, MENTHOL,
D-menthol, fenchene, δ-nonalactone, 2,6-lutidines, dihydro tonquin butter, eugenol, γ-hexalactone, hyacinthin, benzene
Ethanol, 2-methyltetrahydrofuran-3-ketone, the mass percentage content of these 20 kinds of materials of γ-decalactone, respectively with X1To X20Carry out table
Show;
(2) by X1To X20Substitute in following regression equation respectively, calculate YHerbalNumerical value:
YHerbal=10.169X1+10.018X2+9.729X3+9.429X4-9.538X5-9.135X6+8.953X7+8.636X8-
8.571X9+8.235X10-8.229X11+7.318X12-7.129X13+7.086X14-7.428X15-7.035X16+6.053X17+
6.036X18-6.071X19+4.235X20-197.475;
(3) Y of gained is calculatedHerbalNumerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette medicinal herbs odor type, in the range from 0-
10 points.
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Cited By (2)
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CN108645746A (en) * | 2018-06-08 | 2018-10-12 | 云南中烟工业有限责任公司 | Electrical heating based on stove volatile matter is not burnt Sensory Quality of Cigarette analysis method |
CN109613141A (en) * | 2019-01-09 | 2019-04-12 | 吉林烟草工业有限责任公司 | The detection method of gamma lactone and delta-lactone class compound in a kind of quick-fried pearl liquid of cigarette filter tip |
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CN108645746A (en) * | 2018-06-08 | 2018-10-12 | 云南中烟工业有限责任公司 | Electrical heating based on stove volatile matter is not burnt Sensory Quality of Cigarette analysis method |
CN108645746B (en) * | 2018-06-08 | 2020-08-14 | 云南中烟工业有限责任公司 | Electrical heating non-combustible cigarette sensory quality analysis method based on furnace volatile matter |
CN109613141A (en) * | 2019-01-09 | 2019-04-12 | 吉林烟草工业有限责任公司 | The detection method of gamma lactone and delta-lactone class compound in a kind of quick-fried pearl liquid of cigarette filter tip |
CN109613141B (en) * | 2019-01-09 | 2021-09-21 | 吉林烟草工业有限责任公司 | Method for detecting gamma-lactone and delta-lactone compounds in bead blasting liquid of cigarette filter tip |
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