CN104237420A - Method for building cigarette bitter taste index evaluation model based on taste activity value - Google Patents
Method for building cigarette bitter taste index evaluation model based on taste activity value Download PDFInfo
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Abstract
The invention relates to a method for building a cigarette bitter taste index evaluation model based on a taste activity value. The method for building the model comprises the steps of 1) selecting a representative substance of which the alkaloids are the cigarette bitter taste and performing quantitative analysis by gas chromatography-mass spectrometry to obtain a free alkaloid detection result, 2) measuring the bitter taste threshold of each alkaloid in water medium by 3-AFC, calculating the alkaloid taste activity value (TAV) and identifying cigarette key bitter taste substances, 3) building the cigarette bitter taste index evaluation model based on the cigarette key bitter taste substances, and 4) performing fitting effect and model verification analysis on the cigarette bitter taste index and a human body sensory evaluation score by use of Origin 8.5 statistical software. A relatively ideal fitting effect of the built cigarette bitter taste index evaluation model and the human body sensory evaluation is achieved, objective evaluation on the cigarette bitter taste intensity is realized, and technical support can be provided for cigarette bitter taste mechanism revealing, bitter inhibitor development and cigarette bitter taste evaluation.
Description
Technical field
The invention belongs to cigarette evaluation and test technical field, be specifically related to a kind of flue gas bitter taste index assessment method for establishing model based on sense of taste energy value.
Background technology
Cigarette product style and features is the soul of cigarette product, through cigarette product life cycle all the time.The evaluation of tobacco and tobacco product comprises the aspects such as vision, the sense of hearing, sense of smell, the sense of taste and sense of touch, vision is how relevant with appearance factor with hearing evaluation, sense of smell, the sense of taste and sense of touch evaluation are then closely related with style and features, only have the common impression by sense of smell, the sense of taste and sense of touch, could comprehensive, objective, evaluating cigarette product style feature exactly.
Scientific research personnel has carried out a large amount of exploratory development to flue gas aromatic style feature, but is still in the starting stage to the research of flue gas sense of taste style and features evaluation method.Have the special project evaluation for flue gas tart flavour in the Chinese-style cigarette style and features sensory evaluation method set up at present, but it is still smoked panel test based on human body, process difficult of smokeing panel test gets rid of artificial subjectivity and consequent uncertainty.
Natural numerous food product and spices, as Radix Angelicae Sinensis, mango, banana, cucumber and coriander etc., it is not principal ingredient with causing taste composition that its key causes fragrant, micro constitutent often, and its profoundness is that compound is except content height, also has threshold properties.
At present, domestic tobacco business dissects in material base that quality or style and features formed in threshold application technological means and is also in blank; Applying electronic tongue bionics techniques differentiates that flue gas tart flavour, sweet taste, bitter taste and saline taste intensity are emerging a kind of objective quantification characterizing methods, but the method exists testing result is subject to the factor such as artificial saliva, flue gas complex sample contaminant sensor and occurs unstable shortcoming.Bitter taste index is one of key factor affecting cigarette quality, and how quantization signifying is the gordian technique that cigarette product research staff faces with regulation and control flue gas bitter taste.
Summary of the invention
The object of the invention is to the deficiency for existing flue gas bitter taste estimate method, a kind of flue gas bitter taste index assessment method for establishing model based on sense of taste energy value is provided, desirable fitting effect can be obtained with human body evaluation by the method, realize the objective evaluation of flue gas bitterness intensity, for the research of flue gas bitter taste characteristic evaluating, material base and control technique provides support support.
The object of the invention is to be achieved through the following technical solutions:
Based on the flue gas bitter taste index assessment method for establishing model of sense of taste energy value, comprise the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is the bitter substance of representative, adopt in excess sodium hydroxide solution and total particulate matter in mainstream smoke, then with this granule phase substance of methylene chloride-methanol mixed solvent ultrasonic extraction, and carry out Gc/ms Analyser quantitative test, obtain each drifting alkaloids testing result, namely obtain each drifting alkaloids content of total particulate matter in mainstream smoke;
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedure 3-AFC, measure each alkaloidal bitter threshold, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke; Because alkaloid has strong physiologically active, consumption and experimental subjects need strictly to control: experimenter need possess by degree of having a sharp sense of taste, cigarette sensory evaluating smoking qualification test, and alkaloid consumption will control under the low-level of pole;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
In technical solution of the present invention, based food local flavor sense of taste theory described in step (1) is R.S.Shallenberger, Taste Chemistry [M] .New York:Springer-Verlag New York Inc., 2012, filtering out the bitter substance that may exist will comprise containing alkaloid and relevant alkaline matter, some terpene substances, some amino acid and part metals salt compounds, in conjunction with the actual conditions of total particulate matter in mainstream smoke composition, specifically see Rodgman A, Perfetti T A.The chemical components of tobacco and tobacco smoke [M] .Boca Raton:CRC press, 2009, in flue gas, alkaloid and relevant alkaline substance classes are enriched, bitterness intensity is large, be defined as the representative substances of bitter taste in flue gas.
Total particulate matter in mainstream smoke alkaloid described in step (1) carries out rolling of sample according to the method for GB/T 5606.3-2005.
Main flume described in technique scheme step (1) is the main flume that flammable suction tobacco and tobacco product produce through burning.
Further, preferably main flume described in step (1) is the main flume that cigarette, cigar, pipe tobacco, redried leaf tobacco, stem or reconstituted tobacoo produce through burning.
It is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2,3'-dipyridines, anatabine, anabasine, myosmine and nornicotine that technique scheme step (1) filters out alkaloid in flue gas.Excess sodium hydroxide solution described in technique scheme step (1) is 10% sodium hydrate aqueous solution, and in methylene chloride-methanol mixed solvent, methylene chloride and methyl alcohol volume ratio are 3:1.
The mass analyzer of the Gc/ms Analyser described in technique scheme step (1) is any one in commercially available quadrupole rod mass analyzer, ion strap mass analyzer and time of flight mass analyzer, without particular/special requirement.
In step (2), 3 trail and error procedure 3-AFC are specifically see GB/T 12312-2012 organoleptic analysis, the assay method of sense of taste susceptibility.
Further, preferably each alkaloid bitter threshold adopts the medium of 3 trail and error procedures to be water in step (2).
Further, the preferably described flue gas bitter taste index assessment method for establishing model based on sense of taste energy value, comprises the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2, 3'-dipyridine, anatabine, anabasine, myosmine and nornicotine are with the bitter substance of representative, prepare the standard reserving solution that these 13 kinds of alkaloid mass concentrations are 100mg/mL respectively, solvent is the methylene chloride of volume ratio 3:1 and the mixed solution of methyl alcohol, prepare the hybrid standard working solution of series mass concentration as required, according to GB/T19609-2004 defined terms smoking cigarette, total particulate matter in mainstream smoke is trapped with cambridge filter, put into 250mL ground triangular flask by folding for filter disc after trapping, add 8-20mL10% sodium hydrate aqueous solution, after leaving standstill 20min, add methylene chloride and the methanol mixed solvent of 30-60mL volume ratio 3:1 again, ultrasonic extraction 20min, separate dichloromethane layer, adds 100 μ L internal standard compound heptadecanes, under 25 DEG C and 0.04mPa, rotate evaporation and concentration analyze to 1mL, GC/MS, chromatographic column: HP-INNOWAX capillary column, length × internal diameter × thickness is 60m × 0.32mm × 0.25 μm, temperature programme: after 60 DEG C of maintenance 2min, with 20 DEG C/min ramp to 180 DEG C, then with 5 DEG C/min ramp to 230 DEG C, keep 40min, carrier gas is He, post flow 1mL/min, injector temperature 250 DEG C, sample size 1 μ L, split ratio 50:1, solvent delay 3min, ion gun is EI, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, mass scan range 35 ~ 350amu, scan mode SCAN+SIM, qualitative-and-quantitative method: adopt n-compound retention time qualitative, and adopt the qualitative checking of NIST mass spectral database further, adopt 13 kinds of alkaloid standard models to carry out inner mark method ration, obtain each drifting alkaloids content of total particulate matter in mainstream smoke,
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedures, measure the bitter threshold of each alkaloid in aqueous medium, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
Further, preferably the consumption of 10% sodium hydrate aqueous solution is 10mL.
Further, the methylene chloride of the volume ratio 3:1 of preferably ultrasonic extraction and the amount of methanol mixed solvent are 40mL.
In the present invention, 2,3'-dipyridines are the important alkaloids of tobacco, are not 2,2'-dipyridines; When the blending council of State Bureau investigation project in 2013, once pointed out that 2,2'-dipyridine was not the principal ingredient of tobacco specially, but 2,3'-dipyridine.
The present invention compared with prior art, its beneficial effect is: the invention provides a kind of flue gas bitter taste index assessment model set up based on sense of taste energy value, objective quantification can characterize flue gas bitterness intensity, and achieve desirable fitting effect with human body evaluation assessment, solve in sensory evaluation flue gas bitterness intensity process by the problem such as artificial subjectivity and consequent uncertainty; The present invention is that cigarette bitterness mechanism discloses, presses down bitter agent exploitation and flue gas bitter taste estimate and provide technical support.
Accompanying drawing explanation
Fig. 1 is that exponential model method of the present invention and sensory evaluation method are to the correlation test figure of 51 parts of flue gas sample bitter taste estimates.
Embodiment
Below in conjunction with the present invention will be further described by reference to the accompanying drawings.
Reagent required for the present invention, material and instrument:
11 raw tobacco material main producing regions such as Yunnan, Fujian, Guizhou, Hunan, Jiangxi, Sichuan, Heilungkiang, Hubei, Brazil, the U.S. and Zimbabwe amount to 51 parts of tobacco leaf samples, wherein, and burley tobacco leaf 5 parts, 1 part, suncured tabacco, stem 1 part, flue-cured tobacco 44 parts; Upper tobacco leaf 25 parts, 18 parts, middle part tobacco leaf, lower tobacco leaf 8 parts; 9 parts, external tobacco leaf, wherein, 3 parts, Zimbabwe, Brazil 4 parts, 2 parts, U.S., 42 parts, domestic tobacco leaf.
Cigarette is rolled by GB56063-1996 method, more than 48h is balanced under being positioned over temperature 22 ± 1 DEG C, relative humidity 60 ± 3% environment, select cigarette within the scope of average quality ± 0.020g and average resistance to suction ± 49Pa for experiment cigarette, detect for flue gas alkaloid and the sensory evaluation of bitter taste.
Methyl alcohol, chromatographically pure, Shanghai ANPEL Scientific Instrument Co., Ltd.; Methylene chloride, analyzes pure, traditional Chinese medicines group chemical reagent Beijing company limited; NaOH top grade is pure, traditional Chinese medicines group chemical reagent Beijing company limited; N-heptadecane (>=99.5%), 3-ethylpyridine (>=98%), isoquinoline (>=97%), cotinine (>=98%), myosmine (>=98%), nornicotine (>=98%), anabasine (>=97%), nicotine (>=99%), indoles (>=99%), pyridine (>=99%) and quinoline (>=97%) are Sigma-Aidrich company); Nicotryin (>=97%), 2,3'-dipyridines (>=97%) and anatabine (>=95%) are Ling Wei Science and Technology Ltd..All samples is all kept at lower than in 4 DEG C of refrigerators.
The semi-automatic 20 duct smoking machines of RM20H, German Borgwaldt company;
7890GC/5973MS gas chromatograph-mass spectrometer (GCMS), Agilent company of the U.S.;
Jy92-2D ultrasonic cell disrupte instrument, NingBo XinZhi Biology Science Co., Ltd;
RE-52A Rotary Evaporators, Shanghai Yarong Biochemical Instrument Plant;
Elma company of E100H Ultrasound Instrument Germany;
Binder company of KBF240 climatic chamber Germany.
Main flume described in embodiment is the main flume that flammable suction tobacco and tobacco product produce through burning, is specially the main flume that cigarette, cigar, pipe tobacco, redried leaf tobacco, stem or reconstituted tobacoo produce through burning.
Embodiment 1
Based on the flue gas bitter taste index assessment method for establishing model of sense of taste energy value, comprise the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: prepare pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2 respectively, 3'-dipyridine, anatabine, anabasine, myosmine and nornicotine 13 kinds of alkaloid mass concentrations are the standard reserving solution of 100mg/mL, solvent is the methylene chloride of volume ratio 3:1 and the mixed solution of methyl alcohol, prepares the hybrid standard working solution of series mass concentration as required; Carry out tobacco sample according to the method for GB/T5606.3-2005 to roll, rolled sample balances 48h in the climatic chamber of temperature 22 ± 1 DEG C, relative humidity 60 ± 3%, and the cigarette selected within the scope of average quality ± 0.020g and average resistance to suction ± 49Pa is experiment cigarette; According to GB/T19609-2004 defined terms smoking cigarette, trap total particulate matter in mainstream smoke with cambridge filter.Put into 250mL ground triangular flask by folding for filter disc after trapping, add 10mL10% sodium hydrate aqueous solution, after leaving standstill 20min, add the methylene chloride of 40mL volume ratio 3:1 and the mixed solution of methyl alcohol again, ultrasonic extraction 20min, separate dichloromethane layer, adds 100 μ L internal standard compound heptadecanes; Under 25 DEG C and 0.04mPa, rotate evaporation and concentration to 1mL, mass analyzer is commercially available quadrupole rod mass analyzer, and GC/MS analyzes; Chromatographic column: HP-INNOWAX capillary column, length × internal diameter × thickness is 60m × 0.32mm × 0.25 μm; Temperature programme: after 60 DEG C of maintenance 2min, with 20 DEG C/min ramp to 180 DEG C, then with 5 DEG C/min ramp to 230 DEG C, keep 40min; Carrier gas He, post flow 1mL/min, injector temperature 250 DEG C, sample size 1 μ L, split ratio 50:1, solvent delay 3min, ion gun is EI, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, mass scan range 35 ~ 350amu, scan mode SCAN+SIM, qualitative-and-quantitative method: adopt n-compound retention time qualitative, and adopt the qualitative checking of NIST mass spectral database further, adopt 13 kinds of alkaloid standard models to carry out inner mark method ration, n-heptadecane is interior mark.Linear, reappearance, the recovery and the detectability of method are in table 1, and 51 tobacco samples, 13 kinds of flue gas analysis of alkaloids the results are shown in Table 2.13 kinds of alkaloidal coefficient R 2 are between 0.9955 ~ 0.9988, all be greater than 0.99, linear relationship is good, and the range of linearity is between 0.002 ~ 100.000mg/mL, and the standard specimen recovery is between 79.51% ~ 94.80%, except nornicotine, all between 80% ~ 120%, relative standard deviation between 0.42% ~ 8.86%, except anatabine, all be less than 5%, this analysis method can meet the actual requirement of alkaloid quantitative test in flue gas.In 51 tobacco samples, nicotine and nornicotine are alkaloidal principal ingredients, quinoline and isoquinoline content minimum, all the other alkaloids are placed in the middle.
Linear, reappearance, the recovery and the detectability of table 1 method
Table 2 51 tobacco samples 13 kinds of flue gas analysis of alkaloids results (unit: μ g/ props up)
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: alkaloid has strong physiologically active, and consumption and experimental subjects need strictly to control, otherwise, physiology or pharmacology spinoff can be brought.This experiment is chosen to be had long-term smoking cigarette and possesses resistance to alkaloid ability, tested and obtained 30 volunteers of cigarette sensory evaluating smoking technical qualification card by sense of taste susceptibility for experimental subjects, and the alkaloidal research on maximum utilized quantity of oral contact strict control and suck a bite cigarette discharges under alkaloidal level.In 13 alkaloids, pyridine, quinoline, nicotryin, indoles and the taste of anabasine 5 compounds in water are bitter taste, the taste threshold of its open report is 2.00 respectively, 0.95, 0.50, 0.50 and 0.10mg/kg, 3-ethylpyridine, nicotine, isoquinoline, cotinine, 2, 3'-dipyridine, anatabine, 8 kinds of alkaloids such as myosmine and nornicotine are according to GB/T12312-2012 standard method, (1# or 2# cup is containing the material recognized to some extent to prepare each 3 glasss of the alkaloid aqueous solution of 6 concentration gradients respectively, not containing this material in remaining cup, for contrast), be distributed to the volunteer participating in experiment, identification is carried out from low to high by concentration, until taster feels flavoursome, the number of taste can be perceiveed under writing down each concentration, everyone taste threshold is calculated by logistic data model, calculate average taste threshold, the results are shown in Table 3.
Table 38 kinds of alkaloid sense of taste sensory evaluation and taste threshold
Step (3), the foundation of flue gas bitter taste index assessment model: the total particulate matter in mainstream smoke alkaloid testing result table 2 obtained according to step (1) and the alkaloidal taste threshold table 3 of step (2), calculate each alkaloid to flue gas bitter taste contribution rate by sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, the results are shown in Table 4.51 samples, 13 kinds of alkaloidal TAV values are almost all greater than 0.2, show that these alkaloids are all key substance of flue gas bitter taste: myosmine, anabasine and nicotine contribution rate are larger, maximum with the contribution of myosmine, its TAV value is all greater than 20 in all samples, the TAV value of cotinine, nornicotine, nicotryin, indoles and pyridine is between 2 ~ 20 in most sample, and 3-ethylpyridine, quinoline, isoquinoline, anatabine and 2,3'-dipyridine is less than 2 in most sample, minimum to the contribution of flue gas bitter taste.Add by flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value and, because bitter threshold is very low, need for ease of step (4) matching, the index calculated is revised divided by 100, flue gas bitter taste index=(pyridine content/2+3-ethylpyridine content/4+ nicotine content/50+ isoquinoline level/0.95+ isoquinoline content+indoles content/0.5+ nicotryin content/0.5+ anabasine content/0.1+ Mai Siming content/0.05+ anatabine content/2+2, 3'-dipyridine content/7+ cotinine content+nornicotine content/5)/100, 51 sample revised flue gas bitter taste indexes are in table 4.
Table 4 51 tobacco samples 13 kinds of alkaloidal sense of taste energy values and flue gas bitter taste index
Step (4), the checking of flue gas bitter taste index assessment model: organize cigarette sensory evaluating smoking technician, carries out the human body evaluation of flue gas bitterness intensity, obtains the sensory evaluation score value of 51 sample flue gas bitter tastes, in table 5.With Origin8.5 statistical software, linear fit analysis is carried out to flue gas bitter taste exponential sum sensory evaluation score value two column data.Fig. 1 is the correlation test figure of two column datas.As can be seen here, only study with the correlativity effect of flue gas bitter taste unsatisfactory with a certain or certain several alkaloid, and the sense of taste energy value sum set up based on 13 kinds of alkaloids and taste threshold and flue gas bitter taste exponential model, in flue gas bitter taste estimate, desirable fitting effect is achieved with human body, relative coefficient reaches 0.86, two groups of data height correlations are described, demonstrate the correctness that this model is set up from the side.Flue gas bitter taste exponential model is a kind of new way of flue gas bitter taste quantization signifying, for cigarette bitterness mechanism discloses, presses down bitter agent exploitation and flue gas bitter taste estimate and provide technical support.
Table 5 51 tobacco sample flue gas bitter taste indexes and sensory evaluation score value comparison sheet
| Sequence number | Flue gas bitter taste index | Sensory evaluation score value | Sequence number | Flue gas bitter taste index | Sensory evaluation score value |
| 1 | 2.03 | 1.47 | 27 | 5.08 | 6.15 |
| 2 | 0.69 | 0.66 | 28 | 5.67 | 6.68 |
| 3 | 2.98 | 2.96 | 29 | 3.14 | 3.00 |
| 4 | 1.75 | 1.10 | 30 | 2.89 | 2.86 |
| 5 | 1.23 | 0.67 | 31 | 2.00 | 1.55 |
| 6 | 2.80 | 2.50 | 32 | 1.88 | 1.18 |
| 7 | 1.56 | 0.70 | 33 | 2.91 | 2.87 |
| 8 | 2.07 | 1.50 | 34 | 2.12 | 1.54 |
| 9 | 2.15 | 1.60 | 35 | 2.95 | 2.95 |
| 10 | 0.60 | 0.72 | 36 | 2.48 | 2.00 |
| 11 | 1.49 | 0.72 | 37 | 2.71 | 2.40 |
| 12 | 2.24 | 1.63 | 38 | 1.85 | 1.10 |
| 13 | 3.51 | 3.42 | 39 | 1.94 | 1.42 |
| 14 | 2.34 | 1.79 | 40 | 2.66 | 2.37 |
| 15 | 0.79 | 0.71 | 41 | 1.94 | 1.38 |
| 16 | 0.62 | 0.70 | 42 | 1.59 | 0.74 |
| 17 | 1.90 | 1.22 | 43 | 2.39 | 1.87 |
| 18 | 2.78 | 2.45 | 44 | 3.16 | 3.07 |
| 19 | 1.94 | 1.43 | 45 | 1.97 | 1.46 |
| 20 | 1.61 | 0.83 | 46 | 2.4 | 1.90 |
| 21 | 1.77 | 1.11 | 47 | 2.59 | 2.21 |
| 22 | 3.41 | 3.33 | 48 | 4.23 | 3.95 |
| 23 | 4.81 | 5.76 | 49 | 1.74 | 0.98 |
| 24 | 4.48 | 5.45 | 50 | 0.91 | 0.70 |
| 25 | 14.38 | 7.46 | 51 | 1.75 | 0.95 |
| 26 | 5.31 | 6.20 |
Embodiment 2
Based on the flue gas bitter taste index assessment method for establishing model of sense of taste energy value, comprise the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2, 3'-dipyridine, anatabine, anabasine, myosmine and nornicotine are with the bitter substance of representative, prepare the standard reserving solution that these 13 kinds of alkaloid mass concentrations are 100mg/mL respectively, solvent is the methylene chloride of volume ratio 3:1 and the mixed solution of methyl alcohol, prepare the hybrid standard working solution of series mass concentration as required, according to GB/T19609-2004 defined terms smoking cigarette, total particulate matter in mainstream smoke is trapped with cambridge filter, put into 250mL ground triangular flask by folding for filter disc after trapping, add 8mL10% sodium hydrate aqueous solution, after leaving standstill 20min, add methylene chloride and the methanol mixed solvent of 30mL volume ratio 3:1 again, ultrasonic extraction 20min, separate dichloromethane layer, adds 100 μ L internal standard compound heptadecanes, under 25 DEG C and 0.04mPa, rotate evaporation and concentration analyze to 1mL, GC/MS, chromatographic column: HP-INNOWAX capillary column, length × internal diameter × thickness is 60m × 0.32mm × 0.25 μm, temperature programme: after 60 DEG C of maintenance 2min, with 20 DEG C/min ramp to 180 DEG C, then with 5 DEG C/min ramp to 230 DEG C, keep 40min, carrier gas is He, post flow 1mL/min, injector temperature 250 DEG C, sample size 1 μ L, split ratio 50:1, solvent delay 3min, ion gun is EI, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, mass scan range 35 ~ 350amu, scan mode SCAN+SIM, qualitative-and-quantitative method: adopt n-compound retention time qualitative, and adopt the qualitative checking of NIST mass spectral database further, adopt 13 kinds of alkaloid standard models to carry out inner mark method ration, obtain each drifting alkaloids content of total particulate matter in mainstream smoke,
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedures, measure the bitter threshold of each alkaloid in aqueous medium, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
Wherein, mass analyzer is ion strap mass analyzer.
Embodiment 3
Based on the flue gas bitter taste index assessment method for establishing model of sense of taste energy value, comprise the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2, 3'-dipyridine, anatabine, anabasine, myosmine and nornicotine are with the bitter substance of representative, prepare the standard reserving solution that these 13 kinds of alkaloid mass concentrations are 100mg/mL respectively, solvent is the methylene chloride of volume ratio 3:1 and the mixed solution of methyl alcohol, prepare the hybrid standard working solution of series mass concentration as required, according to GB/T19609-2004 defined terms smoking cigarette, total particulate matter in mainstream smoke is trapped with cambridge filter, put into 250mL ground triangular flask by folding for filter disc after trapping, add 20mL10% sodium hydrate aqueous solution, after leaving standstill 20min, add methylene chloride and the methanol mixed solvent of 60mL volume ratio 3:1 again, ultrasonic extraction 20min, separate dichloromethane layer, adds 100 μ L internal standard compound heptadecanes, under 25 DEG C and 0.04mPa, rotate evaporation and concentration analyze to 1mL, GC/MS, chromatographic column: HP-INNOWAX capillary column, length × internal diameter × thickness is 60m × 0.32mm × 0.25 μm, temperature programme: after 60 DEG C of maintenance 2min, with 20 DEG C/min ramp to 180 DEG C, then with 5 DEG C/min ramp to 230 DEG C, keep 40min, carrier gas is He, post flow 1mL/min, injector temperature 250 DEG C, sample size 1 μ L, split ratio 50:1, solvent delay 3min, ion gun is EI, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, mass scan range 35 ~ 350amu, scan mode SCAN+SIM, qualitative-and-quantitative method: adopt n-compound retention time qualitative, and adopt the qualitative checking of NIST mass spectral database further, adopt 13 kinds of alkaloid standard models to carry out inner mark method ration, obtain each drifting alkaloids content of total particulate matter in mainstream smoke,
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedures, measure the bitter threshold of each alkaloid in aqueous medium, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
Wherein, mass analyzer is time of flight mass analyzer.
Claims (10)
1., based on the flue gas bitter taste index assessment method for establishing model of sense of taste energy value, it is characterized in that comprising the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is the bitter substance of representative, adopt in excess sodium hydroxide solution and total particulate matter in mainstream smoke, then with this granule phase substance of methylene chloride-methanol mixed solvent ultrasonic extraction, and carry out Gc/ms Analyser quantitative test, obtain each drifting alkaloids testing result, namely obtain each drifting alkaloids content of total particulate matter in mainstream smoke;
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedures, measure each alkaloid bitter threshold, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
2. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: the main flume described in step (1) is the main flume that flammable suction tobacco and tobacco product produce through burning.
3. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: main flume described in step (1) is the main flume that cigarette, cigar, pipe tobacco, redried leaf tobacco, stem or reconstituted tobacoo produce through burning.
4. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, it is characterized in that: it is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2,3'-dipyridines, anatabine, anabasine, myosmine and nornicotine that step (1) filters out alkaloid in flue gas.
5. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, it is characterized in that: the excess sodium hydroxide solution described in step (1) is 10% sodium hydrate aqueous solution, in methylene chloride-methanol mixed solvent, methylene chloride and methyl alcohol volume ratio are 3:1.
6. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: the mass analyzer of the Gc/ms Analyser described in step (1) is any one in commercially available quadrupole rod mass analyzer, ion strap mass analyzer and time of flight mass analyzer.
7. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: in step (2), each alkaloid bitter threshold adopts the medium of 3 trail and error procedures to be water.
8. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 1, is characterized in that: comprise the steps:
Step (1), the detection of total particulate matter in mainstream smoke bitter substance content: based food local flavor theory, filtering out alkaloid in flue gas is pyridine, 3-ethylpyridine, nicotine, quinoline, isoquinoline, nicotryin, indoles, cotinine, 2, 3'-dipyridine, anatabine, anabasine, myosmine and nornicotine are with the bitter substance of representative, prepare the standard reserving solution that these 13 kinds of alkaloid mass concentrations are 100mg/mL respectively, solvent is the methylene chloride of volume ratio 3:1 and the mixed solution of methyl alcohol, prepare the hybrid standard working solution of series mass concentration as required, according to GB/T19609-2004 defined terms smoking cigarette, total particulate matter in mainstream smoke is trapped with cambridge filter, put into 250mL ground triangular flask by folding for filter disc after trapping, add 8-20mL10% sodium hydrate aqueous solution, after leaving standstill 20min, add methylene chloride and the methanol mixed solvent of 30-60mL volume ratio 3:1 again, ultrasonic extraction 20min, separate dichloromethane layer, adds 100 μ L internal standard compound heptadecanes, under 25 DEG C and 0.04mPa, rotate evaporation and concentration analyze to 1mL, GC/MS, chromatographic column: HP-INNOWAX capillary column, length × internal diameter × thickness is 60m × 0.32mm × 0.25 μm, temperature programme: after 60 DEG C of maintenance 2min, with 20 DEG C/min ramp to 180 DEG C, then with 5 DEG C/min ramp to 230 DEG C, keep 40min, carrier gas is He, post flow 1mL/min, injector temperature 250 DEG C, sample size 1 μ L, split ratio 50:1, solvent delay 3min, ion gun is EI, electron energy 70eV, transmission line temperature 280 DEG C, ion source temperature 230 DEG C, level Four bar temperature 150 DEG C, mass scan range 35 ~ 350amu, scan mode SCAN+SIM, qualitative-and-quantitative method: adopt n-compound retention time qualitative, and adopt the qualitative checking of NIST mass spectral database further, adopt 13 kinds of alkaloid standard models to carry out inner mark method ration, obtain each drifting alkaloids content of total particulate matter in mainstream smoke,
Step (2), the identification of the crucial bitter substance of total particulate matter in mainstream smoke: utilize 3 trail and error procedures, measure the bitter threshold of each alkaloid in aqueous medium, integrating step (1) drifting alkaloids testing result, calculate each alkaloid to flue gas bitter taste contribution rate, i.e. sense of taste energy value; Sense of taste energy value TAV=total particulate matter in mainstream smoke drifting alkaloids content/taste threshold, if during certain alkaloid TAV >=0.1, is then identified as the crucial bitter substance of total particulate matter in mainstream smoke;
Step (3), the foundation of flue gas bitter taste index assessment model: the crucial bitter substance TAV of total particulate matter in mainstream smoke that step (2) obtains is sued for peace, sets up flue gas bitter taste index assessment model: flue gas bitter taste index=total particulate matter in mainstream smoke key organism alkali sense of taste energy value sum;
Step (4), flue gas bitter taste index assessment models fitting effect and modelling verification analysis: organize cigarette sensory evaluating smoking technician, carry out the human body evaluation of flue gas bitterness intensity, and adopt Origin8.5 statistical software, score value is evaluated to flue gas bitter taste index and human body and carries out fitting effect and modelling verification analysis.
9. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 8, is characterized in that: the consumption of 10% sodium hydrate aqueous solution is 10mL.
10. the flue gas bitter taste index assessment method for establishing model based on sense of taste energy value according to claim 8, is characterized in that: the methylene chloride of the volume ratio 3:1 of ultrasonic extraction and the amount of methanol mixed solvent are 40mL.
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