CN105004827A - Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance - Google Patents

Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance Download PDF

Info

Publication number
CN105004827A
CN105004827A CN201510404205.0A CN201510404205A CN105004827A CN 105004827 A CN105004827 A CN 105004827A CN 201510404205 A CN201510404205 A CN 201510404205A CN 105004827 A CN105004827 A CN 105004827A
Authority
CN
China
Prior art keywords
cigarette
property material
pungent
sample
testing sample
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510404205.0A
Other languages
Chinese (zh)
Inventor
李超
张承明
吴亿勤
许�永
邹楠
蒋薇
蒋茨清
秦云华
杨光宇
缪明明
陈章玉
张建华
李劲竹
鲁媛
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Yunnan Industrial Co Ltd
Original Assignee
China Tobacco Yunnan Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Yunnan Industrial Co Ltd filed Critical China Tobacco Yunnan Industrial Co Ltd
Priority to CN201510404205.0A priority Critical patent/CN105004827A/en
Publication of CN105004827A publication Critical patent/CN105004827A/en
Pending legal-status Critical Current

Links

Landscapes

  • Fats And Perfumes (AREA)

Abstract

The invention discloses a method for accurately characterizing and evaluating spicy characteristics of a cigarette fragrance. Through a HS-GC-MS/MS detection method, fragrant substance quantification data is obtained and through a corresponding fragrant substance threshold, a cigarette spicy fragrance index S is calculated and constructed. The method can be operated simply, is not interfered by impurities and has accurate detection results. GC-MS/MS selectivity and sensitivity are higher than those of GC-MS so that the problem that the GC-MS has low sensitivity, a poor resolution ratio and poor selectivity, can easily produce false positive results and cannot provide enough qualitative/quantitative information is solved. From a substance base perspective, the method provides corresponding description and expression of cigarette spicy fragrant characteristics, prevents sensorial rating subjectivity and realizes objective and comprehensive characterization and evaluation of a spicy fragrance style of a cigarette product.

Description

A kind of method of pungent fragrant feature in accurate characterization and evaluating cigarette fragrance
Technical field
The invention belongs to Sensory Quality of Cigarette evaluate and analyze technical field, specifically relate to a kind of can the method for pungent fragrant feature in accurate characterization and evaluating cigarette fragrance.
Background technology
Burn and suck the consumer goods as one, the aesthetic quality of cigarette is its core and soul, is therefore one of of paramount importance content in cigarette technical work to the evaluate and analyze of Sensory Quality of Cigarette always.Literature survey shows, has carried out a large amount of technical researches in recent years around Sensory Quality of Cigarette, sums up and gets up can be divided into Sensory Quality of Cigarette evaluation, species analysis two type relevant to aesthetic quality.
1, Sensory Quality of Cigarette evaluation
Existing Sensory Quality of Cigarette evaluation method has two kinds, and a kind of is comprehensive evaluation to cigarette sensory quality, and another kind is the evaluation to cigarette sense organ style and features and qualitative characteristics.
The middle defined of the integrated evaluating method of cigarette sensory quality: GB 5606.4-2005 " cigarette the 4th part: sense organ technical requirement ", six judgment criteria of sensory evaluating smoking, comprise gloss, fragrance, harmony, assorted gas, pungency and pleasant impression;
Cigarette sense organ style and features and qualitative characteristics evaluation method: in YC/T 497-2014 " cigarette Chinese-style cigarette style sensory evaluation method ", cigarette sense organ aromatic style is further subdivided into: delicate fragrance, fruital, Xin Xiang, the banksia rose, blue or green grow perfume, the fragrance of a flower, herbal, beans are fragrant, cocoa is fragrant, milk, cream are fragrant, cure perfume (or spice), fragrant and sweet, Flue-cured Tobacco is fragrant and 15 note indexs such as airing cigarette cigarette perfume;
Above-mentioned two kinds of existing evaluation methods are all the evaluate and analyze methods set up from subjective experience impressions such as the person's of smokeing panel test vision, sense of smell, the sense of taste, wherein GB 5606.4-2005 is mainly used in the accordance inspection of cigarette product aesthetic quality, and YC/T 497-2014 is then applied to the consistency check of cigarette product aesthetic quality.But the impact of the many factors such as these two kinds of methods need the experience relying on Sensory Quality of Cigarette judging panel to carry out, and are easily subject to the professional standards of judging panel, technical ability of smokeing panel test, subjective hobby, likely there is larger difference in the evaluation result of different judging panel.
2, relevant to Sensory Quality of Cigarette species analysis
Along with the continuous progress of detection technique, researchist adopts the technological means pair flavor matters relevant to Sensory Quality of Cigarette such as headspace solid-phase microextraction-GC/MS, LC-MS, sensor, Electronic Nose, near infrared to detect, and to flavor matter concentration and cause fragrant contribution and carry out multiple regression, find the material of variable concentrations to the impact of cigarette sense organ fragrance by setting up corresponding regression equation.The such as detection decision method of a CN201210388661 flavor type of cigarette.Although regression equation can explain the correlativity between the concentration of flavor matter and cigarette flavor to a certain extent.But GC-MS method also exists on material qualitative/quantitative, and sensitivity is low, lack of resolution, poor selectivity, easily produce false positive results and can not provide the problems such as enough qualitative/quantitative information, qualitative/quantitative result is caused to there is very large uncertainty.Meanwhile, relevant research work also cannot explain that eugenol equal size is low, but contributes the material of large (namely threshold value is low) to the remarkable effect of the pungent fragrant aromatic style of cigarette to sense organ fragrance; Lack to cigarette quality feature and style and features based on the corresponding description of material base and expression, many sensory evaluating smoking's features also cannot make an explanation from material base.
3, brief summary
All there is certain defect in existing evaluation and application method.How by chemical analysis technology means, accurate evaluation and analysis are carried out to " cigarette style characteristic and qualitative characteristics ", just become tobacco business scientific workers face one of key subjects urgently to be resolved hurrily.But there is not yet solution well in prior art.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of can the method for pungent fragrant feature in accurate characterization and evaluating cigarette fragrance.Detected by HS-GC-MS/MS (HS GC-tandem mass spectrometry) and obtain flavor matter quantitative data, and calculated by the threshold value of corresponding flavor matter and build the pungent note index S obtaining cigarette, the pungent fragrant aromatic style feature of cigarette is passed judgment on, the subjective error caused to avoid sensory evaluating smoking.
Object of the present invention is achieved through the following technical solutions.
Except as otherwise noted, percentage of the present invention is mass percent.
A method for pungent fragrant feature in accurate characterization and evaluating cigarette fragrance, comprises the following steps:
(1) with γ-hexalactone, styracine, heliotropin, 4-vinyl guaiacol, eugenol, 3,4-dihydrocoumarin and isoeugenol 7 kinds of property materials as the pungent fragrant aromatic style of appreciable impact cigarette;
(2) foundation of property material standard working curve:
1. standard reserving solution: each property material accurately takes the standard items of 10.0mg respectively, be placed in same 100mL volumetric flask, dissolve with methylene chloride and dilute constant volume, being mixed with the standard reserving solution that mass concentration is 100 μ g/mL, being stored in 4 DEG C of refrigerators for subsequent use;
2. internal standard compound naphthalene is dissolved in absolute ethyl alcohol, and concentration is 100 μ g/mL;
3. 1. gained standard reserving solution 0.1mL, 0.5mL, 1mL, 5mL, 10mL is pipetted respectively, be placed in 5 100mL volumetric flasks respectively, add 1mL inner mark solution respectively, the compound solution that concentration is followed successively by 0.1 μ g/mL, 0.5 μ g/mL, 1 μ g/mL, 5 μ g/mL, 10 μ g/mL is obtained with dchloromethane, wherein, mark naphthalene concentration is 1 μ g/mL, as Working Standard Solution;
4. carry out linear regression with the standard model of 7 property materials and interior target response ratio and its concentration proportion respectively, obtain the standard working curve of each property material, curve forces zero, linearly dependent coefficient R 2must 0.999 be greater than;
(3) pre-treatment of testing sample:
A, get the pipe tobacco of testing sample, carry out determination of moisture according to " preparation of YC/T 31 tobacco and tobacco product sample and determination of moisture Oven Method ";
B, take the pipe tobacco of 1.000g testing sample, be placed in 20mL ml headspace bottle, add 1mL inner mark solution, compress bottle cap rapidly, jolting makes pipe tobacco evenly and at the bottom of loosely is laid in bottle;
(4) carry out analysis and determination by HS-GC-MS/MS method to testing sample, instrumental conditions is as follows:
1. head space instrument analysis condition:
Ml headspace bottle capacity: 20mL, sample loop capacity: 3mL, Sample equilibration temperature: 100 DEG C, sample loop temperature: 120 DEG C, transmission line temperature: 160 DEG C, Sample equilibration time: 45min, GC cycling time: 42min, sample bottle moulding pressure: 138KPa, pressing time: 0.20min, inflationtime: 0.20min, sample loop equilibration time: 0.05min, sample injection time: 0.50min;
2. chromatographiccondition:
DB-5MS capillary column; Injector temperature: 250 DEG C; Constant current mode, post flow 1mL/min; Split ratio: 20:1; Heating schedule: initial temperature 80 DEG C, keeps 1min, with the ramp to 150 DEG C of 8 DEG C/min, keeps 3min; Again with the ramp to 250 DEG C of 15 DEG C/min, keep 20min;
3. mass spectrophotometry condition:
EI ionizes pattern, ionization energy 70ev; Filament current: 80 μ A; Ion source temperature: 170 DEG C; Transmission line temperature: 250 DEG C; Q2 collides gas: purity of argon 99.999%, CID gaseous tension is 1.5mtorr; Scan mode: multiple-reaction monitoring MRM pattern is 150ms to the detection time of each ion;
About qualitative ion pair, quota ion to and optimize after collision energy (CE) value as shown in table 1:
Table 1:
(5) read the response of each property material of testing sample, the typical curve set up by step (2) corrects property material primary data each in testing sample, namely obtains the content C of a certain property material in testing sample i:
C i = A i m s A s K i × 1 m × ( 1 - w ) ………………①
Wherein, C irepresent the content of a certain property material in testing sample, unit is ug/g;
A ifor the peak area of property material a certain in testing sample, unit is U (integration unit);
A sfor the peak area of internal standard compound matter, unit is U (integration unit);
M sfor adding the amount of internal standard compound matter, unit is ug;
M is for taking tobacco quality, and unit is g;
W is moisture in cut tobacco content to be measured, and unit is %;
K ifor the standard working curve slope of each property material;
(6) calculating of cigarette pungent note index S:
7 kinds of property materials all have contribution to the pungent perfume (or spice) of cigarette smoke, evaluate the percentage contribution of a certain property material to the pungent perfume (or spice) of cigarette by smell activity value OAV, the pungent note index of cigarette be 7 kinds of property material smell activity values adding and:
The pungent note index of cigarette 2.
In formula: C ifor the content of i kind property material in testing sample; t ifor the fragrance threshold value of i kind property material; O ifor the OAV value of i kind property material, namely n is the number of property material; Because Low Flavour Threshold is very low, for ease of comparing with Analyses Methods for Sensory Evaluation Results, the OAV value of each property material is multiplied by a coefficient, f ifor the correction factor of each property material, specifically as shown in table 2;
Table 2
Property material Correction factor f i
γ-hexalactone 1
Styracine 10 -1
Heliotropin 10 -3
4-vinyl guaiacol 10 -1
Eugenol 10 -3
3,4-dihydrocoumarin 10 -2
Isoeugenol 10 -2
(7) the pungent fragrant aromatic style feature evaluation of cigarette:
According to the standards of grading of table 3, the pungent fragrant aromatic style of cigarette is passed judgment on;
The pungent fragrant aromatic style judgment criteria of table 3 cigarette
Index Pungent note index (S)
6≤S≤10 3≤S<6 2≤S<3 1≤S<2 S<1
Xin Xiang Strongly Stronger Have Micro-have Nothing
Pungent fragrant feature in cigarette flavor and cigarette pungent note index S correlation, namely cigarette pungent note index S value is higher, then show that the pungent fragrant aromatic style of this cigarette is more remarkable.
Relative to prior art, the present invention has the following advantages:
1, the present invention is with cigarette style characteristic index---and pungent note is guiding, adopts HS-GC-MS/MS technological means, on the basis setting up qualitative characteristics and style and features thing mass spectral database, carries out qualitative and quantitative analysis to cigarette quality, style related substances; Testing result is utilized to adopt statistical model to set up the mathematic(al) representation of pungent note index, this expression formula comprehensively also builds the index (pungent note index S) characterizing the pungent fragrant aromatic style of cigarette with corresponding threshold calculations, carry out the pungent fragrant aromatic style of comprehensive characterization and evaluating cigarette product.The proposition of pungent note index S model has carried out corresponding description and expression from the angle of material base to the pungent fragrant feature of cigarette, many sensory evaluating smoking's features are explained from material base, explain eugenol equal size low, but contribute the material of large (namely threshold value is low) to the remarkable effect of the pungent fragrant aromatic style of cigarette to sense organ fragrance.And avoid the subjectivity of sensory evaluating smoking, the pungent fragrant aromatic style of objective comprehensive characterization and evaluating cigarette product.
2, HS-GC-MS/MS (HS GC-tandem mass spectrometry) easy and simple to handle, be not subject to impurity interference, testing result is more accurate.The selectivity of GC-MS/MS (gas chromatography tandem mass spectrometry method) and remolding sensitivity GC-MS (gas chromatography mass spectrometry method) are high, avoid that GC-MS sensitivity is low, lack of resolution, poor selectivity, easily produce false positive results and can not provide the problems such as enough qualitative/quantitative information.
Embodiment
In order to understand the present invention better, below by embodiment the present invention done and describe in detail further, but embodiment being not limited to the technical solution.
Embodiment 1:
(1) material and instrument:
(1) material: certain brand cigarette A;
Reagent: methylene chloride (AR, Shanghai ANPEL Scientific Instrument Co., Ltd.); Absolute ethyl alcohol (AR, Shanghai reagent one factory); γ-hexalactone, styracine, heliotropin, 4-vinyl guaiacol, eugenol, 3,4-dihydrocoumarin, isoeugenol, naphthalene (purity is all greater than 98%, all purchased from lark prestige).
(2) instrument: AG204 electronic balance (sensibility reciprocal: 0.0001g, METTLER TOLEDO company of Switzerland); Air blast thermostatic drying chamber (101A-2, Shanghai City experimental apparatus head factory); Head space instrument (G1888, Agilent); GC-MS/MS (SCION 456GC-TQ, Bruker company); Liquid-transfering gun (Tripette company).
(2) preparation of sample and the mensuration of property material:
(1) HS-GC-MS/MS method measures 7 kinds of property materials
A, sample preparation: finished cigarettes A is removed filter tip, divests tipping paper, carry out determination of moisture according to " preparation of YC/T 31 tobacco and tobacco product sample and determination of moisture Oven Method "; Use analytical balance to take 1.000g pipe tobacco (being accurate to 0.1mg) in 20mL ml headspace bottle, add 1mL inner mark solution, compress bottle cap rapidly, suitable jolting make pipe tobacco even and loose to be laid in bottle at the bottom of.
B, Static Headspace condition are: ml headspace bottle capacity: 20mL, sample loop capacity: 3mL, Sample equilibration temperature: 100 DEG C, sample loop temperature: 120 DEG C, transmission line temperature: 160 DEG C, Sample equilibration time: 45min, GC cycling time: 42min, sample bottle moulding pressure: 138KPa, pressing time: 0.20min, inflationtime: 0.20min, sample loop equilibration time: 0.05min, sample injection time: 0.50min; According to selected temperature programme condition, can suitably adjust GC cycling time;
C, when GC-MS/MS measures, the chromatographic condition of employing is specific as follows:
A) chromatographic column: DB-5MS quartz capillary column (30m × 0.25mm × 0.25 μm, Agilent company of the U.S.); Or other equivalent chromatographic columns, as HP-5MS quartz capillary column (30m × 0.25mm × 0.25 μm), mS (30m × 0.25mm × 0.25 μm) etc.;
B) injector temperature: 250 DEG C;
C) temperature programme condition: initial temperature 80 DEG C, keeps 1min, with the ramp to 150 DEG C of 8 DEG C/min, keeps 3min; Again with the ramp to 250 DEG C of 15 DEG C/min, keep 20min; Can concrete condition per sample, the temperature programme condition selecting other suitable;
D) carrier gas: He (purity >=99.99%); Q2 collides gas: argon gas (purity 99.999%);
E) mode is ionized: EI source; Ionization energy 70ev; Filament current: 80 μ A; Ion source temperature: 170 DEG C; Transmission line temperature: 250 DEG C;
F) scan mode: multiple-reaction monitoring MRM pattern, CID gaseous tension is 1.5mtorr; Be 150ms to the detection time of each ion.
The calculating of D, measurement result: measure series of features standard of physical solution by HS-GC-MS/MS method, with the ratio of property material and interior mark peak area as ordinate, the concentration of property material and the ratio of interior mark concentration are as horizontal ordinate, set up the standard working curve of 7 kinds of property materials respectively, curve forces zero.Linear regression is carried out to correction data, linearly dependent coefficient R 2must 0.999 be greater than.
Working sample, the content of the calculated by peak area 7 kinds of property materials per sample, calculates the content of wherein a certain property material:
C i = A i m s A s K i &times; 1 m &times; ( 1 - w ) ………………①
Wherein, C irepresent the content detecting and analyze the fragrance characteristic material obtained, unit is ug/g;
A ifor the peak area of fragrance characteristic material in sample, unit is U (integration unit);
A sfor the peak area of internal standard compound matter, unit is U (integration unit);
M sfor adding the amount of internal standard compound matter, unit is ug;
M is for taking tobacco quality, and unit is g;
W is moisture in cut tobacco content to be measured, and unit is %;
K ifor the standard working curve slope of each property material;
E, measurement result:
(1) certain brand tobacco sample A carries out sample preparation according to described method, measures its 7 kinds of property material content by HS-GC-MS/MS method.The results are shown in Table 4:
Table 4 HS-GC-MS/MS method measures the result of 7 kinds of property materials (ug/g) in A brand cigarette
Sequence number Title The content (ug/g) of object
1 γ-hexalactone 0.127
2 Styracine 3.056
3 Heliotropin 0.990
4 4-vinyl guaiacol 1.096
5 Eugenol 1.181
6 3,4-dihydrocoumarin 0.229
7 Isoeugenol 1.056
(2) the pungent note index of A brand cigarette (S a) calculating:
Based on said determination result, bring formula below into:
………………②
In formula: C ifor the content of i kind fragrance characteristic material; t ifor the fragrance threshold value of i kind property material; O ifor the OAV value of i kind fragrance characteristic material, namely n is the number of fragrance characteristic material; For ease of comparing with Analyses Methods for Sensory Evaluation Results, the OAV value of each property material is multiplied by a coefficient, f ifor the OAV correction factor of each material.The smell activity value of 7 kinds of property materials is as shown in table 5.
The smell activity value (O of 7 kinds of property materials in table 5 A brand cigarette pipe tobacco i)
Sequence number Title Fragrance threshold value (ug/g) O i f i
1 γ-hexalactone 1.6 0.079 1
2 Styracine 0.1 30.56 10 -1
3 Heliotropin 0.004 247.5 10 -3
4 4-vinyl guaiacol 0.3 3.653 10 -1
5 Eugenol 0.006 196.833 10 -3
6 3,4-dihydrocoumarin 0.07 3.271 10 -2
7 Isoeugenol 0.059 17.898 10 -2
The pungent note index of A brand cigarette (S a)=4.16, show that the pungent fragrant aromatic style of this brand cigarette is comparatively strong, but do not reach strong degree.
Embodiment 2:
Repeat the process of embodiment 1, select another brand cigarette B, measure its 7 kinds of property material content by HS-GC-MS/MS method, measured value is as shown in table 6, and the smell activity value of 7 kinds of property materials is as shown in table 7.
Table 6 HS-GC-MS/MS method measures the result of 7 kinds of property materials (ug/g) in B brand cigarette
Sequence number Title The content (ug/g) of object
1 γ-hexalactone 0.127
2 Styracine 2.529
3 Heliotropin 1.089
4 4-vinyl guaiacol 1.131
5 Eugenol 0.317
6 3,4-dihydrocoumarin 0.265
7 Isoeugenol 1.008
The smell activity value (O of 7 kinds of property materials in table 7 B brand cigarette pipe tobacco i)
The pungent note index of B brand cigarette (S b)=3.52.Show that the pungent fragrant aromatic style of this brand cigarette cigarette is comparatively strong, but fragrant aromatic style more pungent than A brand cigarette is more weak.
Embodiment 3:
The technician organizing 14 to have a national cigarette sensory evaluating smoking qualification certificate to A, B two the aromatic style index (Flue-cured Tobacco perfume, airing cigarette cigarette perfume, delicate fragrance, fruital, Xin Xiang, the banksia rose, blue or greenly grow perfume, the fragrance of a flower, herbal etc.) of brand cigarette sample evaluate, obtain pungent fragrant index judge score value.Result is as shown in table 8.
The pungent note exponential sum sensory evaluation contrast of table 8 A and B two brand cigarettes
Brand Pungent note index Pungent fragrant index sensory evaluation score value
A 4.16 4
B 3.52 4
As known from Table 8, the pungent note index that embodiment 1-2 draws and pungent fragrant index sensory evaluation score value do not have significant difference, demonstrate the accurate feasibility of the method for pungent fragrant feature in sign proposed by the invention and evaluating cigarette fragrance.And in implementation process, the subjectivity of conventional sensory evaluation method can be avoided, more objective the pungent fragrant aromatic style of cigarette can be characterized and passed judgment on.

Claims (1)

1. the method for pungent fragrant feature in accurate characterization and evaluating cigarette fragrance, comprises the following steps:
(1) with γ-hexalactone, styracine, heliotropin, 4-vinyl guaiacol, eugenol, 3,4-dihydrocoumarin and isoeugenol 7 kinds of property materials as the pungent fragrant aromatic style of appreciable impact cigarette;
(2) foundation of property material standard working curve:
1. standard reserving solution: each property material accurately takes the standard items of 10.0mg respectively, be placed in same 100mL volumetric flask, dissolve with methylene chloride and dilute constant volume, being mixed with the standard reserving solution that mass concentration is 100 μ g/mL, being stored in 4 DEG C of refrigerators for subsequent use;
2. internal standard compound naphthalene is dissolved in absolute ethyl alcohol, and concentration is 100 μ g/mL;
3. 1. gained standard reserving solution 0.1mL, 0.5mL, 1mL, 5mL, 10mL is pipetted respectively, be placed in 5 100mL volumetric flasks respectively, add 1mL inner mark solution respectively, the compound solution that concentration is followed successively by 0.1 μ g/mL, 0.5 μ g/mL, 1 μ g/mL, 5 μ g/mL, 10 μ g/mL is obtained with dchloromethane, wherein, mark naphthalene concentration is 1 μ g/mL, as Working Standard Solution;
4. carry out linear regression with the standard model of 7 property materials and interior target response ratio and its concentration proportion respectively, obtain the standard working curve of each property material, curve forces zero, linearly dependent coefficient R 2must 0.999 be greater than;
(3) pre-treatment of testing sample:
A, get the pipe tobacco of testing sample, carry out determination of moisture according to " preparation of YC/T 31 tobacco and tobacco product sample and determination of moisture Oven Method ";
B, take the pipe tobacco of 1.000g testing sample, be placed in 20mL ml headspace bottle, add 1mL inner mark solution, compress bottle cap rapidly, jolting makes pipe tobacco evenly and at the bottom of loosely is laid in bottle;
(4) carry out analysis and determination by HS-GC-MS/MS method to testing sample, instrumental conditions is as follows:
1. head space instrument analysis condition:
Ml headspace bottle capacity: 20mL, sample loop capacity: 3mL, Sample equilibration temperature: 100 DEG C, sample loop temperature: 120 DEG C, transmission line temperature: 160 DEG C, Sample equilibration time: 45min, GC cycling time: 42min, sample bottle moulding pressure: 138KPa, pressing time: 0.20min, inflationtime: 0.20min, sample loop equilibration time: 0.05min, sample injection time: 0.50min;
2. chromatographiccondition:
DB-5MS capillary column; Injector temperature: 250 DEG C; Constant current mode, post flow 1mL/min; Split ratio: 20:1; Heating schedule: initial temperature 80 DEG C, keeps 1min, with the ramp to 150 DEG C of 8 DEG C/min, keeps 3min; Again with the ramp to 250 DEG C of 15 DEG C/min, keep 20min;
3. mass spectrophotometry condition:
EI ionizes pattern, ionization energy 70ev; Filament current: 80 μ A; Ion source temperature: 170 DEG C; Transmission line temperature: 250 DEG C; Q2 collides gas: purity of argon 99.999%, CID gaseous tension is 1.5mtorr; Scan mode: multiple-reaction monitoring MRM pattern is 150ms to the detection time of each ion;
About qualitative ion pair, quota ion to and optimize after collision energy CE value as shown in table 1:
Table 1:
(5) read the response of each property material of testing sample, the typical curve set up by step (2) corrects property material primary data each in testing sample, namely obtains the content C of a certain property material in testing sample i:
………………①
Wherein, C irepresent the content of a certain property material in testing sample, unit is ug/g;
A ifor the peak area of property material a certain in testing sample, unit is U (integration unit);
A sfor the peak area of internal standard compound matter, unit is U (integration unit);
M sfor adding the amount of internal standard compound matter, unit is ug;
M is for taking tobacco quality, and unit is g;
W is moisture in cut tobacco content to be measured, and unit is %;
K ifor the standard working curve slope of each property material;
(6) calculating of cigarette pungent note index S:
7 kinds of property materials all have contribution to the pungent perfume (or spice) of cigarette smoke, evaluate the percentage contribution of a certain property material to the pungent perfume (or spice) of cigarette by smell activity value OAV, the pungent note index of cigarette be 7 kinds of property material smell activity values adding and:
The pungent note index of cigarette 2.
In formula: C ifor the content of i kind property material in testing sample; t ifor the fragrance threshold value of i kind property material; O ifor the OAV value of i kind property material, namely n is the number of property material; Because Low Flavour Threshold is very low, for ease of comparing with Analyses Methods for Sensory Evaluation Results, the OAV value of each property material is multiplied by a coefficient, f ifor the correction factor of each property material, specifically as shown in table 2;
Table 2
Property material Correction factor f i γ-hexalactone 1 Styracine 10 -1 Heliotropin 10 -3 4-vinyl guaiacol 10 -1 Eugenol 10 -3 3,4-dihydrocoumarin 10 -2 Isoeugenol 10 -2
(7) the pungent fragrant aromatic style feature evaluation of cigarette:
According to the standards of grading of table 3, the pungent fragrant aromatic style of cigarette is passed judgment on;
The pungent fragrant aromatic style judgment criteria of table 3 cigarette
Pungent fragrant feature in cigarette flavor and cigarette pungent note index S correlation, namely cigarette pungent note index S value is higher, then show that the pungent fragrant aromatic style of this cigarette is more remarkable.
CN201510404205.0A 2015-07-10 2015-07-10 Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance Pending CN105004827A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510404205.0A CN105004827A (en) 2015-07-10 2015-07-10 Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510404205.0A CN105004827A (en) 2015-07-10 2015-07-10 Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance

Publications (1)

Publication Number Publication Date
CN105004827A true CN105004827A (en) 2015-10-28

Family

ID=54377578

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510404205.0A Pending CN105004827A (en) 2015-07-10 2015-07-10 Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance

Country Status (1)

Country Link
CN (1) CN105004827A (en)

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106093246A (en) * 2016-08-11 2016-11-09 云南中烟工业有限责任公司 A kind of quantitative forecasting technique of Medicated cigarette spicy
CN106198793A (en) * 2016-07-06 2016-12-07 云南中烟工业有限责任公司 A kind of supercritical fluid chromatography gaschromatographic mass spectrometry measures the method for phenolic compound in cigarette mainstream flue gas
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

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JOHN C. LEFFINGWELL ET AL: "Identification of the Volatile Constituents of Cyprian Latakia Tobacco by Dynamic and Static Headspace Analyses", 《LEFFINGWELL REPORTS》 *
冒德寿 等: "基于味觉活力值的烟气苦味指数模型的建立", 《烟草科技》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106198793A (en) * 2016-07-06 2016-12-07 云南中烟工业有限责任公司 A kind of supercritical fluid chromatography gaschromatographic mass spectrometry measures the method for phenolic compound in cigarette mainstream flue gas
CN106093246A (en) * 2016-08-11 2016-11-09 云南中烟工业有限责任公司 A kind of quantitative forecasting technique of Medicated cigarette spicy
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

Similar Documents

Publication Publication Date Title
CN104991007A (en) Method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma
CN105092729A (en) Method for accurate characterization and evaluation of milky aroma characteristic in cigarette aroma
CN104991023A (en) Method for exactly characterizing and evaluating flower aroma characteristics in cigarette aroma
CN104991006A (en) Method for exactly characterizing and evaluating clean aroma characteristics in cigarette aroma
CN105004808A (en) Method for accurately characterizing and evaluating medicinal herb fragrance characteristics of cigarette fragrance
CN105044264A (en) Method for accurate characterization and evaluation of characteristics of baking aroma in cigarette aroma
CN104991005A (en) Method for exactly characterizing and evaluating bean aroma characteristics in cigarette aroma
CN105136947A (en) Method of accurately representing and evaluating fruit smell character in fragrance of tobacco
CN102901779B (en) Discrimination method for caramel sweet taste characteristics of tobacco leaf based on flavor components
CN105004827A (en) Method for accurately characterizing and evaluating spicy characteristics of cigarette fragrance
CN104569263B (en) A kind of method of quick and precisely evaluating cigarette constant product quality
CN104991024A (en) Method for exactly characterizing and evaluating wood aroma characteristics in cigarette aroma
CN105158385A (en) Method for accurately characterizing and evaluating flue-cured tobacco smoke aroma characteristic in cigarette aroma
CN102288718B (en) Method for identifying genuine and fake cigarettes by using headspace-gas chromatography-mass spectrum (HS-GC-MS) total ion current chromatogram map technique
CN103134850A (en) Tea quality rapid detection apparatus and detection method based on characteristic fragrance
CN109696501B (en) Method for identifying characteristic volatile flavor substances of meat or meat products
CN102033110A (en) Method for evaluating cigarette flavoring uniformity
CN106404884A (en) Method for quickly evaluating quality consistency of flavors and fragrances of volatile cigarettes by HS-IMR-MS
CN105004826A (en) Method for accurately characterizing and evaluating green fragrance characteristics of cigarette fragrance
Sun et al. Differentiation of flue-cured tobacco leaves in different positions based on neutral volatiles with principal component analysis (PCA)
CN109298082B (en) Method for identifying artificial essence added in tea
CN101382557B (en) Cigarette quality analytical method
CN109738567B (en) Method for evaluating uniformity of cut tobacco flavoring mode
CN105021727A (en) Accurate characterization and evaluation method of cocoa aroma characteristics of cigarette aroma
CN105092730A (en) Method for accurate characterization and evaluation of cream aroma characteristic in cigarette aroma

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20151028

RJ01 Rejection of invention patent application after publication