CN106093246A - A kind of quantitative forecasting technique of Medicated cigarette spicy - Google Patents

A kind of quantitative forecasting technique of Medicated cigarette spicy Download PDF

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Publication number
CN106093246A
CN106093246A CN201610656099.XA CN201610656099A CN106093246A CN 106093246 A CN106093246 A CN 106093246A CN 201610656099 A CN201610656099 A CN 201610656099A CN 106093246 A CN106093246 A CN 106093246A
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China
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spicy
medicated cigarette
cigarette
forecasting technique
quantitative
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Inventor
蒋次清
李超
李利君
吴亿勤
张承明
朱保昆
王家俊
郭青
杨帅
毕玉波
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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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
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025—Gas chromatography

Abstract

The invention discloses a kind of detection level based in Medicated cigarette 29 kinds of volatile ingredients and carry out the quantitative forecasting technique to Medicated cigarette spicy.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 29 kinds of volatile ingredients, and then the content of mensuration be brought in regression equation calculating YXin XiangNumerical value, be the predictive value of this kind of Medicated cigarette spicy 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 spicy of the present invention is preferable, it was predicted that mean absolute error be 0.0920 point.The technical support favourable for safeguarding the stable offer of Sensory Quality of Cigarette.

Description

A kind of quantitative forecasting technique of Medicated cigarette spicy
Technical field
The invention belongs to quantitative forecast and the control field of Medicated cigarette spicy, be specifically related to a kind of based in cigarette shreds 29 The detection level of kind of volatile ingredient, and combine regression coefficient and build the method for the regression model quantitative forecast to Medicated cigarette spicy Method.
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/T497-2014 " Medicated cigarette Chinese-style cigarette style sensory evaluation method ".But owing to the person of smokeing panel test exists There is subjectivity in smokeing panel test, make the repeatability of smoking result and stability there is certain deficiency, to such an extent as to evaluation result Reliability produces 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 quantitatively pre-to Medicated cigarette spicy Survey method, to simplify the flow process of the quantitative forecast of Medicated cigarette spicy, thus complete Medicated cigarette spicy fast and accurately quantitative Prediction work.
The purpose of the present invention is achieved by the following technical programs.
The quantitative forecasting technique of a kind of Medicated cigarette spicy, comprises the following steps:
(1) measure the ethyl n-butyrate. in cigarette sample to be predicted, δ-dodecalactone, heliotropin, 4-methyl-2-phenyl- 1,3-dioxolanes, cinnamyl cinnamate, β-caryophyllene, isophorone, 5 methyl furfural, 4-hydroxyl-2,5-dimethyl-3 (2H)-furanone, hyacinthin, 1-Phenylethanone., γ-amyl group butyrolactone, δ-decalactone, ethyl isobutyrate, benzylalcohol, phenethanol, 2-second Acyl pyrroline, 2-methyltetrahydrofuran-3-ketone, furfuryl alcohol, fenchene, δ-caprolactone, benzaldehyde dimethyl acetal, Acacia farnesiana Willd. base third Ketone, alpha-angelica lactone, isobutyl acetate, D-menthol, linalool, δ-nonalactone, the quality of these 29 kinds of materials of ethyl phenylacetate Degree, respectively with X1To X29Represent；
(2) by X1To X29Substitute in following regression equation respectively, calculate YXin XiangNumerical value:
YXin Xiang=0.449X1+0.294X2+0.190X3+0.223X4+0.438X5+0.018X6+0.662X7+0.301X8+ 0.650X9+0.672X10+0.783X11+0.457X12+0.295X13+0.741X14+0.613X15+0.300X16-0.363X17– 0.417X18-0.412X19–0.583X20-0.443X21–0.571X22-0.494X23-0.583X24–0.261X25–0.735X26- 0.353X27–0.301X28-0.094X29-26.759；
(3) Y of gained is calculatedXin XiangNumerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette spicy, in the range from 0-10 divides.
Table 1 below list for above-mentioned 29 kinds of substance to be measured, its quantitative forecast score to Medicated cigarette spicy Regression equation coefficient.
Table 1 regression equation coefficient
Relative to prior art, the invention have the advantages that
1, the present invention 29 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, use the material of the plurality of classes such as aldehyde, ester, ketone, alcohol as depending on that the quantitative forecast score of Medicated cigarette spicy is predicted According to, more accurate than existing method.
3, use less material for modeling and Medicated cigarette spicy to be carried out quantitative forecast, 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 is the hyperbolic chart of 30 kinds of sample regression value of calculation and 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 pungent fragrant style and features sensory evaluating smoking's score range is that 0.5-3.0 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.
29 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):
C s = ( A s A i + a ) × C i × V k × m ... ( 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 ethyl n-butyrate. measured according to method described in a-c in cigarette sample to be predicted, δ-dodecalactone, heliotropin, 4-methyl-2-phenyl-1,3-dioxolanes, cinnamyl cinnamate, β-caryophyllene, isophorone, 5 methyl furfural, 4-hydroxyl- 2,5-dimethyl-3 (2H)-furanone, hyacinthin, 1-Phenylethanone., γ-amyl group butyrolactone, δ-decalactone, ethyl isobutyrate, benzylalcohol, Phenethanol, 2-acetyl pyrrole, 2-methyltetrahydrofuran-3-ketone, furfuryl alcohol, fenchene, δ-caprolactone, benzaldehyde dimethyl acetal, Farnesyl acetone, alpha-angelica lactone, isobutyl acetate, D-menthol, linalool, δ-nonalactone, ethyl phenylacetate etc. 29 kinds The content of material.The descriptive statistics of various content of material testing results is shown in Table 3.
The descriptive statistics of 29 kinds of volatile material testing results in table 3 tobacco shred
Note: statistical sample number is: 30
E, the content detecting obtained 29 kind material in d is brought in following regression equation respectively, calculates YXin XiangNumber Value:
YXin Xiang=0.449X1+0.294X2+0.190X3+0.223X4+0.438X5+0.018X6+0.662X7+0.301X8+ 0.650X9+0.672X10+0.783X11+0.457X12+0.295X13+0.741X14+0.613X15+0.300X16-0.363X17– 0.417X18-0.412X19–0.583X20-0.443X21–0.571X22-0.494X23-0.583X24–0.261X25–0.735X26- 0.353X27–0.301X28-0.094X29-26.759；
F, the Y of calculating gainedXin XiangNumerical value, be the quantitative forecast score of this kind of Medicated cigarette spicy.Calculate 30 kinds of samples respectively The Y of productXin XiangNumerical value, and with sensory evaluating smoking's result comparison, result is as shown in Figure 1.The curve of diamond indicia is that regression equation records in advance Point, and the square marks actual score of smokeing panel test that is sense organ.There it can be seen that use the Medicated cigarette pungent fragrant breeze lattice spy of forecast of regression model Levy sensory evaluating smoking's score preferable with the actual smoking result goodness of fit, it was predicted that average MAE (mean absolute error)=0.0920 point.

Claims (1)

1. a quantitative forecasting technique for Medicated cigarette spicy, comprises the following steps:
(1) ethyl n-butyrate. in cigarette sample to be predicted, δ-dodecalactone, heliotropin, 4-methyl-2-phenyl-1,3-are measured Dioxolanes, cinnamyl cinnamate, β-caryophyllene, isophorone, 5 methyl furfural, 4-hydroxyl-2,5-dimethyl-3 (2H)-furan Mutter ketone, hyacinthin, 1-Phenylethanone., γ-amyl group butyrolactone, δ-decalactone, ethyl isobutyrate, benzylalcohol, phenethanol, 2-acetyl group pyrrole Cough up, 2-methyltetrahydrofuran-3-ketone, furfuryl alcohol, fenchene, δ-caprolactone, benzaldehyde dimethyl acetal, farnesyl acetone, α-when Lactone, isobutyl acetate, D-menthol, linalool, δ-nonalactone, the mass percent of these 29 kinds of materials of ethyl phenylacetate is returned to contain Amount, respectively with X1To X29Represent；
(2) by X1To X29Substitute in following regression equation respectively, calculate YXin XiangNumerical value:
YXin Xiang=0.449X1+0.294X2+0.190X3+0.223X4+0.438X5+0.018X6+0.662X7+0.301X8+0.650X9 +0.672X10+0.783X11+0.457X12+0.295X13+0.741X14+0.613X15+0.300X16-0.363X17–0.417X18- 0.412X19–0.583X20-0.443X21–0.571X22-0.494X23-0.583X24–0.261X25–0.735X26-0.353X27– 0.301X28-0.094X29-26.759；
(3) Y of gained is calculatedXin XiangNumerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette spicy, in the range from 0-10 Point.
CN201610656099.XA 2016-08-11 2016-08-11 A kind of quantitative forecasting technique of Medicated cigarette spicy Pending CN106093246A (en)

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Publication number Priority date Publication date Assignee Title
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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
CN111289677A (en) * 2020-03-31 2020-06-16 中国烟草总公司郑州烟草研究院 Method for measuring spicy components in main stream smoke of cigarette
CN113376268A (en) * 2021-05-14 2021-09-10 河北中烟工业有限责任公司 Method for measuring spicy components in main stream smoke of cigarette

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