CN106546699A - A kind of quantitative forecasting technique of Medicated cigarette dry in the sun cigarette perfume type - Google Patents

Abstract

The invention discloses a kind of detection level based on 21 kinds of volatile ingredients in Medicated cigarette is come the quantitative forecasting technique to Medicated cigarette dry in the sun cigarette perfume type.The sample treatment and GC MS/MS analysis methods first set up according to independent development is measured to the content of 21 kinds of volatile ingredients in tobacco shred, then the content of measure is brought in regression equation and calculates Y_{Dry in the sun cigarette perfume}Numerical value, be the predictive value of this kind of Medicated cigarette dry in the sun cigarette perfume type quantitative forecasting technique score, in the range from 0 10 points.With the actual smoking result goodness of fit of sense organ preferably, the mean absolute error of prediction is 0.1451 point to the quantitative forecasting technique of the Medicated cigarette dry in the sun cigarette perfume type of the present invention.The technical support favourable to safeguard the stable offer of Sensory Quality of Cigarette.

Description

A kind of quantitative forecasting technique of Medicated cigarette dry in the sun cigarette perfume type

Technical field

The invention belongs to the quantitative forecast and control field of Medicated cigarette dry in the sun cigarette perfume type, and in particular to a kind of to be based on cigarette shreds In 21 kinds of volatile ingredients detection level, and with reference to regression coefficient build regression model method to Medicated cigarette dry in the sun cigarette perfume type Quantitative forecasting technique.

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, the evaluation of cigarette sensory quality is mainly by expert 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》With 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, the repeatability and stability for making smoking result has certain deficiency, so as to evaluation result Reliability produce impact.

There is internal relation between the organoleptic feature of Medicated cigarette and its chemical composition, different chemical constituents can be special to Medicated cigarette sense organ Levy and produce different degrees of impact.In recent years, based on chemical composition Medicated cigarette sensory evaluation and Study on Forecasting Method there has also been compared with Many reports.For example, not grand grade of Harbin Engineering University provides one kind by immune neural net algorithm to predict volume The method (101419209 A of CN) of cigarette sensory evaluating smoking and fume indication, but its component substances for including computation modeling is only total Sugar, total nicotine, reducing sugar etc. more than 10 plant routine chemical componentses index, and which 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 the mould Type is predicted to Medicated cigarette sensory evaluating smoking and fume indication (CN 1525394A), but which is used for the chemical composition that models and calculate Up to 110 remainders, Indexs measure are qualitative, quantitative loaded down with trivial details, and difficulty in computation is larger.In turn result in which to predict the outcome relatively low or not enough may be used By the shortcomings of.

The content of the invention

Present invention aims to and overcome the deficiencies in the prior art, there is provided it is a kind of that Medicated cigarette dry in the sun cigarette perfume type is determined Amount Forecasting Methodology, to simplify the flow process of the quantitative forecast of Medicated cigarette dry in the sun cigarette perfume type, so as to fast and accurately complete to Medicated cigarette dry in the sun The quantitative forecast work of cigarette perfume type.

The purpose of the present invention is achieved by the following technical programs.

A kind of quantitative forecasting technique of Medicated cigarette dry in the sun cigarette perfume type, comprises the following steps：

(1) determine delta-undeca lactone in cigarette sample to be predicted, γ-dodecalactone, gamma-undecalactone, δ-decalactone, In γ-decalactone, alpha, beta-lonone, benzyl benzoate, δ-dodecalactone, cinnamyl cinnamate, benzyl cinnamate, δ-nonyl Ester, γ-amyl group butyrolactone, β-caryophyllene, dihydro tonquin butter, eugenol, farnesyl acetone, 3- ethyoxyl -4- hydroxy benzeness first Aldehyde, vanillin, phenethyl acetate, fenchene, the mass percentage content of 4- vinyl guaiacols this 21 kinds of materials, respectively with X₁To X₂₁To represent；

(2) by X₁To X₂₁Substituted in following regression equation respectively, calculate Y_{Dry in the sun cigarette perfume}Numerical value：

Y_{Dry in the sun cigarette perfume}=11.779X₁+11.659X₂+11.439X₃+11.216X₄+10.789X₅+10.635X₆+10.453X₇+ 10.336X₈+8.974X₉+8.515X₁₀+8.329X₁₁+8.298X₁₂-5.619X₁₃+7.118X₁₄-5.221X₁₅-4.965X₁₆+ 7.451X₁₇+7.092X₁₈-5.336X₁₉+5.291X₂₀+4.807X₂₁-428.317；

(3) calculate the Y of gained_{Dry in the sun cigarette perfume}Numerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette dry in the sun cigarette perfume type, its Scope is 0-10 point.

List in table 1 below for above-mentioned 21 kinds of substance to be measured, its quantitative forecast to Medicated cigarette dry in the sun cigarette perfume type The regression equation coefficient of score.

1 regression equation coefficient of table

Relative to prior art, the present invention has advantages below：

1st, the present invention can be given more than sensory evaluating smoking method from 21 kinds of volatile component contents in cigarette shreds Objective, stable result of determination, eliminates the impact of the artificial difference in sensory evaluating smoking.

2nd, with the plurality of classes such as ester, ketone, alkene, phenol material as Medicated cigarette dry in the sun cigarette perfume type quantitative forecast score predict Foundation, it is more fully more accurate than existing method.

3rd, modeling quantitative forecast to Medicated cigarette dry in the sun cigarette perfume type are used for using less material, with detecting speed faster Degree, the quantitative flow process for relatively simplifying, it is to avoid the problem of regression modeling overfitting make the result of quantitative forecast accurately and reliable. The technical support favourable to safeguard the stable offer of Sensory Quality of Cigarette.

Description of the drawings

The hyperbolic chart of 30 kinds of sample regression value of calculation of Fig. 1 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

The commercially available finished cigarettes in 30 kinds of country of purchase (box mark tar 8-12mg/, box mark nicotine 0.6-1.2mg/, box mark CO 9-13mg/, 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 its dry in the sun cigarette perfume style and features sensory evaluating smoking score range for 0.5-2.5 point.

A, sample treatment and analysis

The cigarette for taking the same brand of Xin Kaibao at random carries out sample preparation, and prepared by sample quick and precisely, and should guarantee sample Product are not contaminated, and each laboratory sample prepares three parallel samples.Cigarette paper and filter tip are peelled off, tobacco shred is taken out, weight is recorded, then It is respectively put in 3 100ml conical flasks, as sample.The internal standard of 60 μ g/mL of 1mL is separately added in ready sample Naphthalene, 9mL ether, close the lid rapidly and shake up, and are placed on concussion shaking table and shake 2h, take 0.22 μm of upper layer of extraction liquid Jing with 10ml syringes Filtering with microporous membrane, analyzes for GC-MS/MS (gas chromatography-mass spectrum/mass spectrograph).

B, gas chromatography-mass spectrum/mass spectral analyses condition

Chromatographic column：DB-5MS (30m × 0.25mm i.d. × 0.25 μm d.f., Agilent companies of the U.S.) elastic quartz Capillary chromatographic column；Injector temperature：250℃；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℃；Ionization energy 70eV；Heater current：80μA；Full scan monitors Full scan Pattern, sweep limitss：10-500amu；Multiple-reaction monitoring MRM patterns, qualitative, quota ion pair selection parameter are shown in Table 2.

21 kinds of volatile components and interior target qualitative ion pair, quota ion pair and collision energy in 2 tobacco shred of table

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 the 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 there is corresponding measured object in can determine whether sample.Each sample parallel assay 3 times.Root According to the content of 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 are U (integration unit)；Peak areas of the Ai for internal standard substance, unit are U (products Divide unit)；Ci is the amount for adding internal standard substance, and unit is μ g/mL；To weigh tobacco quality, unit is g to m；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 delta-undeca lactone determined according to a-c methods describeds in cigarette sample to be predicted, γ-dodecalactone, γ-ten one Lactone, δ-decalactone, γ-decalactone, alpha, beta-lonone, benzyl benzoate, δ-dodecalactone, cinnamyl cinnamate, Cortex Cinnamomi Acid benzyl ester, δ-nonalactone, γ-amyl group butyrolactone, β-caryophyllene, dihydro tonquin butter, eugenol, farnesyl acetone, 3- ethoxies The content of 21 kinds of materials such as base -4- hydroxy benzaldehydes, vanillin, phenethyl acetate, fenchene, 4- vinyl guaiacols.Respectively The descriptive statisticses for planting content of material testing result are shown in Table 3.

The descriptive statisticses of 21 kinds of volatile material testing results in 3 tobacco shred of table

Note：Statistical sample number is：30

E, the content of 21 kinds of materials obtained by detecting in d is brought in following regression equation respectively, calculates Y_{Dry in the sun cigarette perfume}'s Numerical value：

Y_{Dry in the sun cigarette perfume}=11.779X₁+11.659X₂+11.439X₃+11.216X₄+10.789X₅+10.635X₆+10.453X₇+ 10.336X₈+8.974X₉+8.515X₁₀+8.329X₁₁+8.298X₁₂-5.619X₁₃+7.118X₁₄-5.221X₁₅-4.965X₁₆+ 7.451X₁₇+7.092X₁₈-5.336X₁₉+5.291X₂₀+4.807X₂₁-428.317；

F, the Y for calculating gained_{Dry in the sun cigarette perfume}Numerical value, be the quantitative forecast score of this kind of Medicated cigarette dry in the sun cigarette perfume type.Calculate respectively The Y of 30 kinds of samples_{Dry in the sun cigarette perfume}Numerical value, and compare with sensory evaluating smoking's result, as a result as shown in Figure 1.The curve of diamond indicia is recurrence side Journey predicts score, and square marks are the actual score of smokeing panel test of sense organ.There it can be seen that the Medicated cigarette using forecast of regression model dries in the air The fragrant style and features sensory evaluating smoking score of suncured tabacco with the actual smoking result goodness of fit preferably, (miss the average MAE of prediction by average absolute Difference)=0.1451 point.

Claims (1)

1. a kind of quantitative forecasting technique of Medicated cigarette dry in the sun cigarette perfume type, comprises the following steps：

(1) determine delta-undeca lactone in cigarette sample to be predicted, γ-dodecalactone, gamma-undecalactone, δ-decalactone, γ- Decalactone, alpha, beta-lonone, benzyl benzoate, δ-dodecalactone, cinnamyl cinnamate, benzyl cinnamate, δ-nonalactone, γ-amyl group butyrolactone, β-caryophyllene, dihydro tonquin butter, eugenol, farnesyl acetone, vanirom, Vanillin, phenethyl acetate, fenchene, the mass percentage content of 4- vinyl guaiacols this 21 kinds of materials, respectively with X₁ To X₂₁To represent；

(2) by X₁To X₂₁Substituted in following regression equation respectively, calculate Y_{Dry in the sun cigarette perfume}Numerical value：

Y_{Dry in the sun cigarette perfume}=11.779X₁+11.659X₂+11.439X₃+11.216X₄+10.789X₅+10.635X₆+10.453X₇+ 10.336X₈+8.974X₉+8.515X₁₀+8.329X₁₁+8.298X₁₂-5.619X₁₃+7.118X₁₄-5.221X₁₅-4.965X₁₆+ 7.451X₁₇+7.092X₁₈-5.336X₁₉+5.291X₂₀+4.807X₂₁-428.317；

(3) calculate the Y of gained_{Dry in the sun cigarette perfume}Numerical value, be the score value of the quantitative forecast of this kind of Medicated cigarette dry in the sun cigarette perfume type, its scope For 0-10 point.