CN106442768A - Quantitative forecasting method for fresh and sweet aroma type of cigarettes - Google Patents

Abstract

The invention discloses a quantitative forecasting method for the fresh and sweet aroma type of cigarettes on the basis of detection of content of 17 volatile components in cigarettes. Firstly, the content of the 17 volatile components in the cigarettes is measured with an independently developed and established sample treatment method and a GC-MS/MS analysis method, and the measured content is introduced into a regression equation, the value of Y fresh and sweet aroma is calculated, that is, the forecasted value of the score of the quantitative forecasting method for the green aroma type of the cigarettes is calculated and ranges from 0 to 10. The quantitative forecasting method for the fresh and sweet aroma type of the cigarettes is better fit with sensory actual smoke panel test results, the forecasted mean absolute error is 0.1329 scores, and favorable technical support is provided for keeping the sensory quality of the cigarettes stable.

Description

The blue or green quantitative forecasting technique growing odor type of a kind of cigarette

Technical field

The invention belongs to the blue or green quantitative forecast growing odor type of cigarette and control field, be specifically related to a kind of based in cigarette shreds The detection of 17 kinds of volatile component contents, and the method combining regression coefficient structure regression model is quantitatively pre-to cigarette blue or green taste odor type The method surveyed.

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 cigarette sense The evaluation method 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 professional standard.For example, GB 5606.4-2005《Cigarette the 4th Part:Sense organ technology requires》With YC/T 497-2014《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 reappearance of smoking result and stability there is certain deficiency, to evaluation result Reliability produce impact.

There is inner link between the organoleptic feature of cigarette and its chemical composition, different chemical component can be special to cigarette sense organ Levy the impact producing in various degree.In recent years, there has also been relatively based on the cigarette sensory evaluation and Study on Forecasting Method of chemical composition Many reports.For example, 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, reduced sugars etc. more than 10 plant routine chemical components index, and it cannot represent the overall permanence of cigarette sense organ.Yizhong cigarette The Hu Shengguo etc. of grass (group) Co., Ltd has invented the BP neural network model of a kind of combination FUZZY SET APPROACH TO ENVIRONMENTAL, and uses this mould Cigarette sensory evaluating smoking and fume indication are predicted (CN 1525394 A) by type, but it is for modeling the chemical composition calculating Up to 110 remainders, Indexs measure is qualitative, quantitatively loaded down with trivial details, and difficulty in computation is relatively big, in turn results in it and predicts the outcome relatively low or not may be used The shortcoming such as lean on.

Content of the invention

Present invention aims to and overcome the deficiencies in the prior art, providing and a kind of grow the quantitative of odor type to cigarette is blue or green Forecasting Methodology, simplifying the flow process of the blue or green quantitative forecast growing odor type of cigarette, thus completes to grow odor type to cigarette is blue or green fast and accurately Quantitative forecast work.

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

The blue or green quantitative forecasting technique growing odor type of a kind of cigarette, comprises the following steps：

(1) benzyl cinnamate in cigarette sample to be predicted, cinnamyl cinnamate, γ-decalactone, phenylamino benzoic acid first are measured Ester, alpha, beta-lonone, farnesyl acetone, dihydro tonquin butter, δ-nonalactone, β-damascone, γ-dodecalactone, benzene second Acetoacetic ester, phenethyl acetate, eugenol, 4-vinyl guaiacol, vanillic aldehyde, p-anisaldehyde, anethene this 17 kinds of materials Mass percentage content, respectively with X₁To X₁₇Represent；

(2) by X₁To X₁₇Substitute in following regression equation respectively, calculate Y_{Blue or green taste perfume}Numerical value：

Y_{Blue or green taste perfume}=7.329X₁+6.428X₂-4.929X₃+6.157X₄+4.608X₅-4.525X₆+3.433X₇+3.216X₈- 4.020X₉+2.036X₁₀-3.071X₁₁+4.235X₁₂+3.053X₁₃+3.036X₁₄-3.071X₁₅-5.235X₁₆+5.053X₁₇- 269.045；

(3) Y of gained is calculated_{Blue or green taste perfume}Numerical value, be the score value of the blue or green quantitative forecast growing odor type of this kind of cigarette, its scope Divide for 0-10.

Listing in table 1 below for above-mentioned 17 kinds of substance to be measured, to cigarette, the blue or green quantitative forecast growing odor type obtains for it The regression equation coefficient dividing.

Table 1 regression equation coefficient

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

1st, the present invention 17 kinds of volatile component contents from cigarette shreds, can be given more than sensory evaluating smoking method Objective, stable result of determination, eliminates the impact of artificial difference in sensory evaluating smoking.

2nd, the material using the plurality of classes such as ester, ketone, phenol, aldehyde, alkene is pre-as the quantitative forecast score of cigarette blue or green taste odor type The foundation surveyed, more fully more accurate than existing method.

3rd, use the quantitative forecast for modeling and to cigarette blue or green taste odor type for the less material, there is detection speed faster Degree, the quantitative flow process relatively simplifying, it is to avoid the problem of regression modeling overfitting, the result making quantitative forecast is accurate and reliable, For the favourable technical support of the stable offer safeguarding Sensory Quality of Cigarette.

Brief description

30 kinds of sample regression calculated values of Fig. 1 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 blue or green perfume style and features sensory evaluating smoking's score range of growing is that 0.5-3.5 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 not contaminated, and each laboratory sample prepares three parallel samples.Peel off cigarette paper and filter tip, take out pipe tobacco, 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 is placed in concussion 2h on concussion shaking table, 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℃；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℃；Ionization energy 70eV；Heater current：80μA；Full scan monitors Full scan Pattern, sweep limits：10-500amu；Multiple-reaction monitoring MRM pattern, qualitative, quota ion is shown in Table 2 to Selection parameter.

17 kinds of volatile components and the qualitative ion pair of interior target in table 2 pipe tobacco, quota ion to and collision energy

C, index assay

The retention time of comparison standard specimen, 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 corresponding measured object.Each sample parallel measures 3 times.Root Content according to volatility in the quota ion calculated by peak area sample of target compound in sample and semi-volatile organic compounds. 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 for adding the amount of 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, method according to a-c measure the benzyl cinnamate in cigarette sample to be predicted, cinnamyl cinnamate, γ-last of the ten Heavenly stems Lactone, benzyl benzoate, alpha, beta-lonone, farnesyl acetone, dihydro tonquin butter, δ-nonalactone, β-damascone, γ-dodecalactone, ethyl phenylacetate, phenethyl acetate, eugenol, 4-vinyl guaiacol, vanillic aldehyde, p-anisaldehyde, fennel The content of 17 kinds of materials such as fragrant alkene.The descriptive statistics of various content of material testing results is shown in Table 3.

The descriptive statistics of 17 kinds of volatile materials testing results in table 3 pipe tobacco

Note：Statistical sample number is：30

E, d will detect obtained by the content of 17 kinds of materials be brought into respectively in following regression equation, calculate Y_{Blue or green taste perfume}'s Numerical value：

Y_{Blue or green taste perfume}=7.329X₁+6.428X₂-6.428X₃+6.157X₄+4.608X₅-4.525X₆+3.433X₇+3.216X₈- 4.020X₉+2.036X₁₀-3.071X₁₁+4.235X₁₂+3.053X₁₃+3.036X₁₄-3.071X₁₅-5.235X₁₆+5.053X₁₇- 269.045；

F, the Y calculating gained_{Blue or green taste perfume}Numerical value, be the blue or green quantitative forecast score growing odor type of this kind of cigarette.Calculate 30 respectively Plant the Y of sample_{Blue or green taste perfume}Numerical 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 blue or green taste of cigarette 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)= 0.1329 point.

Claims (1)

1. the blue or green quantitative forecasting technique growing odor type of cigarette, comprises the following steps：

(1) measure the benzyl cinnamate in cigarette sample to be predicted, cinnamyl cinnamate, γ-decalactone, benzyl benzoate, Alpha, beta-lonone, farnesyl acetone, dihydro tonquin butter, δ-nonalactone, β-damascone, γ-dodecalactone, phenylacetic acid second Ester, phenethyl acetate, eugenol, 4-vinyl guaiacol, vanillic aldehyde, p-anisaldehyde, the quality of this 17 kinds of materials of anethene Degree, respectively with X₁To X₁₇Represent；

(2) by X₁To X₁₇Substitute in following regression equation respectively, calculate Y_{Blue or green taste perfume}Numerical value：

Y_{Blue or green taste perfume}=7.329X₁+6.428X₂-6.428X₃+6.157X₄+4.608X₅-4.525X₆+3.433X₇+3.216X₈- 4.020X₉+2.036X₁₀-3.071X₁₁+4.235X₁₂+3.053X₁₃+3.036X₁₄-3.071X₁₅-5.235X₁₆+5.053X₁₇- 269.045；

(3) Y of gained is calculated_{Blue or green taste perfume}Numerical value, be the score value of the blue or green quantitative forecast growing odor type of this kind of cigarette, in the range from 0- 10 points.