CN106338555A - Method for quantification prediction of cigarette baking incense type - Google Patents
Method for quantification prediction of cigarette baking incense type Download PDFInfo
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- CN106338555A CN106338555A CN201610657655.5A CN201610657655A CN106338555A CN 106338555 A CN106338555 A CN 106338555A CN 201610657655 A CN201610657655 A CN 201610657655A CN 106338555 A CN106338555 A CN 106338555A
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- 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
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Abstract
The invention discloses a method for quantification prediction of a cigarette baking incense type based on detected contents of 25 volatile components in cigarette. Firstly, according to an independently developed and established sample processing method and a GC-MS/MS analysis method, the contents of the 25 volatile components in cigarette shreds are determined, then the determined contents are introduced to a regression equation, and the numerical value of a Y baking incense is calculated, namely a scoring prediction value of the method for quantification prediction of the cigarette baking incense type, wherein the range is 0-10 points. The method for quantification prediction of the cigarette baking incense type has relatively good identical degree with a sensory actual smoking evaluation result, and the average absolute error of prediction is 0.0920 point. A beneficial technical support is provided for maintaining the stability of the cigarette sensory quality.
Description
Technical field
The invention belongs to the quantitative forecast of Medicated cigarette baking odor type and control field are and in particular to a kind of be based in cigarette shreds
The detection level of 25 kinds of volatile ingredients, and combine the quantitation that the method for regression coefficient structure regression model bakees odor type to Medicated cigarette
Forecasting Methodology.
Background technology
The stable and lifting of cigarette product quality, it is critical only that the stable of organoleptic quality and is lifted, how to set 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 carrying out, and issued and implemented concerned countries and industry standard.For example, gb 5606.4-2005 " Medicated cigarette the 4th
Part: sense organ technical requirements " and yc/t 497-2014 " Medicated cigarette Chinese-style cigarette style sensory evaluation method ".But due to the person of smokeing panel test
There is subjectivity in smokeing panel test, make the repeatability of smoking result and stability there is certain deficiency, so as to evaluation result
Reliability produce impact.
There is internal relation, different chemical group branches are special to Medicated cigarette sense organ between the organoleptic feature of Medicated cigarette and its chemical composition
Levy and produce different degrees of impact.In recent years, the Medicated cigarette sensory evaluation based on chemical composition and Study on Forecasting Method there has also been relatively
Many reports.For example, not magnificence of Harbin Engineering University etc. provides one kind and predicts volume by immune neural net algorithm
The method (cn 101419209 a) of cigarette sensory evaluating smoking and fume indication, but it is included the component substances of computation modeling and is only total
Sugar, total nicotine, reducing sugar etc. more than 10 plant routine chemical componentses index, and it cannot represent the overall permanence of Medicated cigarette sense organ.Yizhong cigarette
Hu Shengguo of careless (group) company limited etc. has invented a kind of bp neural network model of combination FUZZY SET APPROACH TO ENVIRONMENTAL, and uses this mould
Type is predicted to Medicated cigarette sensory evaluating smoking and fume indication (cn 1525394 a), but it is used for the chemical composition modeling and calculating
Up to 110 remainders, Indexs measure is qualitative, quantitation is loaded down with trivial details, and difficulty in computation is larger.In turn result in it to predict the outcome relatively low or not may be used
By the shortcomings of.
Content of the invention
Present invention aims to and overcome the deficiencies in the prior art, provide a kind of to Medicated cigarette bakee odor type quantitation
Forecasting Methodology, to simplify the flow process that Medicated cigarette bakees the quantitative forecast of odor type, thus fast and accurately complete to bakee odor type to Medicated cigarette
Quantitative forecast work.
The purpose of the present invention is achieved by the following technical programs.
A kind of Medicated cigarette bakees the quantitative forecasting technique of odor type, comprises the following steps:
(1) δ-decalactone in mensure cigarette sample to be predicted, δ-dodecalactone, vanillin, fenchene, γ-amyl group fourth
Lactone, β-caryophyllene, vanirom, γ-octalactone, 4- vinyl guaiacol, heliotropin, Fructus Crataegi
Flower ketone, dihydro tonquin butter, raspberry ketone, farnesyl acetone, gamma-undecalactone, eugenol, β-damascone, β-purple sieve
Blue ketone, benzyl cinnamate, delta-undeca lactone, γ-dodecalactone, cinnamyl cinnamate, benzyl benzoate, ethylmaltol,
The mass percentage content of this 25 kinds of materials of β-cyclocitral, respectively with x1To x25To represent;
(2) by x1To x25Substitute into respectively in following regression equation, calculate yBakee fragrantNumerical value:
yBakee fragrant=1.018x1+1.662x2+1.301x3+1.650x4+1.672x5+1.783x6+0.457x7+1.295x8+
1.741x9+0.613x10+1.300x11-0.363x12–1.417x13-1.412x14–1.583x15+0.443x16–1.571x17-
1.494x18-1.583x19–0.261x20–0.735x21-1.353x22–1.301x23-1.094x24–1.329x25-111.905;
(3) calculate the y of gainedBakee fragrantNumerical value, be the score value that this kind of Medicated cigarette bakees the quantitative forecast of odor type, its scope
Divide for 0-10.
List in table 1 below for above-mentioned 25 kinds of substance to be measured, the quantitative forecast that it bakees odor type to Medicated cigarette obtains
The regression equation coefficient dividing.
Table 1 regression equation coefficient
With respect to prior art, the invention has the advantages that
1st, the present invention 25 kinds of volatile component contents from cigarette shreds, can be given more than sensory evaluating smoking method
Objective, stable predicts the outcome, and eliminates the impact of the artificial difference in sensory evaluating smoking.
2nd, use the quantitative forecast score that the material of the plurality of classes such as ester, aldehyde, alkene, ketone, phenol bakees odor type as Medicated cigarette pre-
The foundation surveyed, more fully more accurate than existing method.
3rd, it is used for modeling and bakeing odor type to Medicated cigarette carrying out quantitative forecast using less material, have and detect speed faster
Degree, the quantitative flow process of relatively simplification, it is to avoid the problem of regression modeling overfitting, make the result of quantitative forecast accurately and reliable.
For the favourable technical support of the stable offer safeguarding Sensory Quality of Cigarette.
Brief description
Fig. 1 is the hyperbolic chart of 30 kinds of sample regression value of calculation and sensory evaluating smoking's result.
Specific embodiment
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 is purchased from the market such as Kunming, Shanghai City, Changsha respectively within 2015);Collected sample is according to yc/t
497-2014 carries out sensory evaluation, determines that it bakees fragrant style and features sensory evaluating smoking's score range and divides for 0.5-5.5.
A, sample treatment and analysis
The cigarette taking the same brand of Xin Kaibao at random carries out sample preparation, and sample preparation quick and precisely, and should guarantee sample
Product are not 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.It is separately added into the internal standard of 1ml 60 μ g/ml in ready sample
Naphthalene, 9ml ether, close the lid rapidly and shake up, and are placed in and shake 2h on concussion shaking table, take upper layer of extraction liquid through 0.22 μm with 10ml syringe
Filtering with microporous membrane, for gc-ms/ms (gas chromatography-mass spectrum/mass spectrograph) analysis.
B, gas chromatography-mass spectrum/mass spectral analyses 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, column flow 1ml/min, sample size: 1 μ l, shunting
Than: 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 monitors full scan
Pattern, sweep limitss: 10-500amu;Multiple-reaction monitoring mrm pattern, qualitative, quota ion pair selection parameter is shown in Table 2.
25 kinds of volatile components and interior target qualitative ion pair, quota ion pair and collision energy in table 2 tobacco shred
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 relative abundance standard suitable with concentration of each qualitative ion
The ion relative abundance of solution is consistent, then can determine whether to exist corresponding measured object in sample.Each sample parallel assay 3 times.Root
Content according to volatility and 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 sample in volatility or
The peak area of semi-volatile organic compounds, unit is u (integration unit);Ai is the peak area of internal standard substance, and unit is that u is (long-pending
Divide unit);Ci is the amount adding internal standard substance, and unit is μ g/ml;M is to weigh tobacco quality, and unit is g;K is each volatility
Or the standard working curve slope of semi-volatile organic compounds;A is each volatility or the standard of semi-volatile organic compounds
Working curve intercept.
D, the δ-decalactone being measured according to a-c methods described in cigarette sample to be predicted, δ-dodecalactone, vanillin, fennel
Fragrant alkene, γ-amyl group butyrolactone, β-caryophyllene, vanirom, γ-octalactone, 4- vinyl guaiacol,
Heliotropin, May bloom ketone, dihydro tonquin butter, raspberry ketone, farnesyl acetone, gamma-undecalactone, eugenol, β-dihydro
Damascenone, alpha, beta-lonone, benzyl cinnamate, delta-undeca lactone, γ-dodecalactone, cinnamyl cinnamate, phenylamino benzoic acid first
The content of 25 kinds of materials such as ester, ethylmaltol, β-cyclocitral.The descriptive statisticses of various content of material testing results are shown in Table 3.
The descriptive statisticses of 25 kinds of volatile material testing results in table 3 tobacco shred
Note: statistical sample number is: 30
E, the content of 25 kinds of materials obtained by detecting in d is brought in following regression equation respectively, calculates yBakee fragrant's
Numerical value:
yBakee fragrant=1.018x1+1.662x2+1.301x3+1.650x4+1.672x5+1.783x6+0.457x7+1.295x8+
1.741x9+0.613x10+1.300x11-0.363x12–1.417x13-1.412x14–1.583x15+0.443x16–1.571x17-
1.494x18-1.583x19–0.261x20–0.735x21-1.353x22–1.301x23-1.094x24–1.329x25-111.905;
F, the y of calculating gainedBakee fragrantNumerical value, be the quantitative forecast score that this kind of Medicated cigarette bakees odor type.Calculate 30 respectively
Plant the y of sampleBakee fragrantNumerical value, and compare with sensory evaluating smoking's result, result is as shown in Figure 1.The curve of diamond indicia is regression equation
Prediction score, and square marks are the actual score of smokeing panel test of sense organ.There it can be seen that being bakeed using the Medicated cigarette of forecast of regression model
Fragrant style and features sensory evaluating smoking's score and the actual smoking result goodness of fit are preferable, and the average mae (mean absolute error) of prediction=
0.0920 point.
Claims (1)
1. a kind of Medicated cigarette bakees the quantitative forecasting technique of odor type, comprises the following steps:
(1) measure cigarette sample to be predicted in δ-decalactone, δ-dodecalactone, vanillin, fenchene, γ-amyl group butyrolactone,
β-caryophyllene, vanirom, γ-octalactone, 4- vinyl guaiacol, heliotropin, May bloom ketone,
Dihydro tonquin butter, raspberry ketone, farnesyl acetone, gamma-undecalactone, eugenol, β-damascone, alpha, beta-lonone,
Benzyl cinnamate, delta-undeca lactone, γ-dodecalactone, cinnamyl cinnamate, benzyl benzoate, ethylmaltol, β-ring lemon
The mass percentage content of this 25 kinds of materials of lemon aldehyde, respectively with x1To x25To represent;
(2) by x1To x25Substitute into respectively in following regression equation, calculate yBakee fragrantNumerical value:
yBakee fragrant=1.018x1+1.662x2+1.301x3+1.650x4+1.672x5+1.783x6+0.457x7+1.295x8+
1.741x9+0.613x10+1.300x11-0.363x12–1.417x13-1.412x14–1.583x15+0.443x16–1.571x17-
1.494x18-1.583x19–0.261x20–0.735x21-1.353x22–1.301x23-1.094x24–1.329x25-111.905;
(3) calculate the y of gainedBakee fragrantNumerical value, be the score value that this kind of Medicated cigarette bakees the quantitative forecast of odor type, in the range from 0-
10 points.
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