CN104991007A - Method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma - Google Patents

Abstract

The invention discloses a method for exactly characterizing and evaluating sweet aroma characteristics in cigarette aroma. Aroma substance quantitative data are acquired through an HS-GC-MS/MS detecting method, and a cigarette sweet aroma note index T is obtained by calculating and establishing a threshold value of a corresponding aroma substance. The method is easy and convenient to operate, not easily disturbed by impurities, and accurate in detecting results. The selectivity and the sensitivity of GC-MS/MS are higher than those of GC-MS; the problems that the sensitivity of the GC-MS is low, the resolution is insufficient, the selectivity is low, false positive results are easily generated, and enough qualitative/quantitative information cannot be given and the like are avoided. According to the method, the sweet aroma characteristics of a cigarette are described and expressed correspondingly from the perspective of material basis; the subjectivity of sensory evaluation is avoided; the sweet aroma style of a cigarette product is characterized and evaluated objectively and comprehensively.

Description

A kind of method of fragrant and sweet 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 fragrant and sweet 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 furanone equal size is low, but contributes the material of large (namely threshold value is low) to the remarkable effect of the fragrant and sweet 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 fragrant and sweet 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 fragrant and sweet note index T obtaining cigarette, the fragrant and sweet 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 fragrant and sweet feature in accurate characterization and evaluating cigarette fragrance, comprises the following steps:

(1) using benzaldehyde, β-cyclocitral, ethyl cinnamate, alpha-angelica lactone, gamma-undecalactone, dihydroactinidiolide, damascone, dorinone, geranyl acetone, α-ionone, phenylethyl alcohol, phenylacetaldehyde, 5 methyl furfural, ethyl maltol, furanone, acetophenone, the fragrant ether of imperial Ting and farnesyl acetone 18 kinds of property materials as the fragrant and sweet aromatic style of appreciable impact cigarette fall;

(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 18 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: 70min, 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 50 DEG C, keeps 2min, with the ramp to 200 DEG C of 5 DEG C/min, keeps 10min; Again with the ramp to 250 DEG C of 10 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:

$C_i=\frac{A_i{m}_s}{A_s{K}_i}\×\frac{1}{m\×(1-w)}$ ………………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 fragrant and sweet note index T:

18 kinds of property materials all have contribution to cigarette smoke is fragrant and sweet, evaluate a certain property material percentage contribution fragrant and sweet to cigarette by smell activity value OAV, the fragrant and sweet note index of cigarette be 18 kinds of property material smell activity values adding and:

The fragrant and sweet note index of cigarette $T=\underset{i=1}{\overset{n}{\Σ}}{f}_i\frac{c_i}{t_i}=\underset{i=1}{\overset{n}{\Σ}}{f}_i{O}_i$ ………………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
		Benzaldehyde	10 -1
β-cyclocitral	10 -1
		Ethyl cinnamate	10 -1
Alpha-angelica lactone	1
		Gamma-undecalactone	10 -1
Dihydroactinidiolide	10 -1
		Damascone	10 -5
Dorinone	10 -6
		Geranyl acetone	10 -2
α-ionone	10 -3
		Phenylethyl alcohol	10 -2
Phenylacetaldehyde	10 -3
		5 methyl furfural	10 -2
Ethyl maltol	10 -4
		Furanone	10 -5

Acetophenone	10 -2
		The fragrant ether of imperial Ting falls	10 -3
Farnesyl acetone	10 -1

(7) the fragrant and sweet aromatic style feature evaluation of cigarette:

According to the standards of grading of table 3, cigarette flavor is passed judgment on;

The fragrant and sweet aromatic style judgment criteria of table 3 cigarette

Fragrant and sweet feature in cigarette flavor and cigarette fragrant and sweet note index T correlation, namely cigarette fragrant and sweet note index T value is higher, then show that the fragrant and sweet 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 fragrant and sweet 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 fragrant and sweet note index, this expression formula comprehensively also builds the index (fragrant and sweet note index T) characterizing the fragrant and sweet aromatic style of cigarette with corresponding threshold calculations, carry out the fragrant and sweet aromatic style of comprehensive characterization and evaluating cigarette product.The proposition of fragrant and sweet note index T model has carried out corresponding description and expression from the angle of material base to the fragrant and sweet feature of cigarette, many sensory evaluating smoking's features are explained from material base, explain furanone equal size low, but contribute the material of large (namely threshold value is low) to the remarkable effect of the fragrant and sweet aromatic style of cigarette to sense organ fragrance.And avoid the subjectivity of sensory evaluating smoking, the fragrant and sweet 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); Benzaldehyde, β-cyclocitral, ethyl cinnamate, alpha-angelica lactone, gamma-undecalactone, dihydroactinidiolide, damascone, dorinone, geranyl acetone, α-ionone, phenylethyl alcohol, phenylacetaldehyde, 5 methyl furfural, ethyl maltol, furanone, acetophenone, imperial Ting fragrant ether, farnesyl acetone, naphthalene (purity is all greater than 98%, all purchased from lark prestige) fall.

(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 18 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: 70min, 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 50 DEG C, keeps 2min, with the ramp to 200 DEG C of 5 DEG C/min, keeps 10min; Again with the ramp to 250 DEG C of 10 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 18 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 18 kinds of property materials per sample, calculates the content of wherein a certain property material:

$C_i=\frac{A_i{m}_s}{A_s{K}_i}\×\frac{1}{m\×(1-w)}$ ………………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 18 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 18 kinds of property materials (ug/g) in A brand cigarette

Sequence number	Title	The content (ug/g) of object
			1	Benzaldehyde	0.127
2	β-cyclocitral	0.150
			3	Ethyl cinnamate	0.152
4	Alpha-angelica lactone	0.375
			5	Gamma-undecalactone	2.192
6	Dihydroactinidiolide	1.876
			7	Damascone	2.501
8	Dorinone	5.094
			9	Geranyl acetone	1.676

10	α-ionone	0.885
			11	Phenylethyl alcohol	0.774
12	Phenylacetaldehyde	0.508
			13	5 methyl furfural	0.115
14	Ethyl maltol	0.037
			15	Furanone	1.217
16	Acetophenone	2.051
			17	The fragrant ether of imperial Ting falls	0.062
18	Farnesyl acetone	0.900

(2) the fragrant and sweet note index of A brand cigarette (T _a) calculating:

Based on said determination result, bring formula below into:

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 18 kinds of property materials is as shown in table 5.

The smell activity value (O of 18 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	Benzaldehyde	0.35	0.363	10 -1
2	β-cyclocitral	0.19	0.789	10 -1
					3	Ethyl cinnamate	0.1	1.52	10 -1
4	Alpha-angelica lactone	10	0.038	1
					5	Gamma-undecalactone	0.95	2.307	10 -1
6	Dihydroactinidiolide	0.95	1.975	10 -1

7	Damascone	9×10 -5	27788.889	10 -5
					8	Dorinone	2×10 -6	2547000	10 -6
9	Geranyl acetone	5×10 -2	33.52	10 -2
					10	α-ionone	0.006	147.50	10 -3
11	Phenylethyl alcohol	0.024	32.25	10 -2
					12	Phenylacetaldehyde	0.004	127	10 -3
13	5 methyl furfural	0.02	5.75	10 -2
					14	Ethyl maltol	1×10 -4	370	10 -4
15	Furanone	4×10 -5	30425	10 -5
					16	Acetophenone	0.065	31.554	10 -2
17	The fragrant ether of imperial Ting falls	0.002	31	10 -3
					18	Farnesyl acetone	0.15	6	10 -1

The fragrant and sweet note index of A brand cigarette (T _a)=5.84, show that the fragrant and sweet aromatic style of this brand cigarette is stronger.

Embodiment 2:

Repeat the process of embodiment 1, select another brand cigarette B, measure its 18 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 18 kinds of property materials is as shown in table 7.

Table 6 HS-GC-MS/MS method measures the result of 18 kinds of property materials (ug/g) in B brand cigarette

Sequence number	Title	The content (ug/g) of object
			1	Benzaldehyde	0.157
2	β-cyclocitral	0.209
			3	Ethyl cinnamate	0.137
4	Alpha-angelica lactone	0.625
			5	Gamma-undecalactone	0.577
6	Dihydroactinidiolide	1.838

7	Damascone	2.872
			8	Dorinone	5.086
9	Geranyl acetone	1.694
			10	α-ionone	0.913
11	Phenylethyl alcohol	0.686
			12	Phenylacetaldehyde	0.271
13	5 methyl furfural	0.116
			14	Ethyl maltol	0.342
15	Furanone	1.173
			16	Acetophenone	2.176
17	The fragrant ether of imperial Ting falls	0.078
			18	Farnesyl acetone	0.848

The smell activity value (O of 18 kinds of property materials in table 7 B brand cigarette pipe tobacco _i)

Sequence number	Title	Fragrance threshold value (ug/g)	O i	f i
					1	Benzaldehyde	0.35	0.449	10 -1
2	β-cyclocitral	0.19	1.1	10 -1
					3	Ethyl cinnamate	0.1	1.37	10 -1
4	Alpha-angelica lactone	10	0.063	1
					5	Gamma-undecalactone	0.95	0.607	10 -1
6	Dihydroactinidiolide	0.95	1.935	10 -1
					7	Damascone	9×10 -5	31911.111	10 -5
8	Dorinone	2×10 -6	2543000	10 -6
					9	Geranyl acetone	5×10 -2	33.88	10 -2
10	α-ionone	0.006	152.167	10 -3
					11	Phenylethyl alcohol	0.024	28.583	10 -2
12	Phenylacetaldehyde	0.004	67.75	10 -3

13	5 methyl furfural	0.02	5.8	10 -2
					14	Ethyl maltol	1×10 -4	3420	10 -4
15	Furanone	4×10 -5	29325	10 -5
					16	Acetophenone	0.065	33.477	10 -2
17	The fragrant ether of imperial Ting falls	0.002	39	10 -3
					18	Farnesyl acetone	0.15	5.653	10 -1

The fragrant and sweet note index of B brand cigarette (T _b)=5.95.Show that the fragrant and sweet aromatic style of this brand cigarette is comparatively strong, but do not reach strong degree, the fragrant and sweet aromatic style of this brand cigarette comparatively A brand cigarette is slightly high.

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 fragrant and sweet index judge score value.Result is as shown in table 8.

The fragrant and sweet note exponential sum sensory evaluation contrast of table 8 A and B two brand cigarettes

Brand	Fragrant and sweet note index	Fragrant and sweet index sensory evaluation score value
			A	5.84	6
B	5.95	6

As known from Table 8, the fragrant and sweet note index that embodiment 1-2 draws and fragrant and sweet index sensory evaluation score value do not have significant difference, demonstrate the accurate feasibility of the method for fragrant and sweet 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 fragrant and sweet aromatic style of cigarette can be characterized and passed judgment on.

Claims (1)

1. the method for fragrant and sweet feature in accurate characterization and evaluating cigarette fragrance, comprises the following steps:

(1) using benzaldehyde, β-cyclocitral, ethyl cinnamate, alpha-angelica lactone, gamma-undecalactone, dihydroactinidiolide, damascone, dorinone, geranyl acetone, α-ionone, phenylethyl alcohol, phenylacetaldehyde, 5 methyl furfural, ethyl maltol, furanone, acetophenone, the fragrant ether of imperial Ting and farnesyl acetone 18 kinds of property materials as the fragrant and sweet aromatic style of appreciable impact cigarette fall;

(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 18 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: 70min, 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 50 DEG C, keeps 2min, with the ramp to 200 DEG C of 5 DEG C/min, keeps 10min; Again with the ramp to 250 DEG C of 10 DEG C/min, keep 20min;

1. 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:

$C_i=\frac{A_i{m}_s}{A_s{K}_i}\×\frac{1}{m\×(1-w)}$ ………………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 fragrant and sweet note index T:

18 kinds of property materials all have contribution to cigarette smoke is fragrant and sweet, evaluate a certain property material percentage contribution fragrant and sweet to cigarette by smell activity value OAV, the fragrant and sweet note index of cigarette be 18 kinds of property material smell activity values adding and:

The fragrant and sweet note index of cigarette $T=\underset{i=1}{\overset{n}{\Σ}}{f}_i\frac{c_i}{t_i}=\underset{i=1}{\overset{n}{\Σ}}{f}_i{O}_i$ ………………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 Benzaldehyde 10 ^-1 β-cyclocitral 10 ^-1 Ethyl cinnamate 10 ^-1 Alpha-angelica lactone 1 Gamma-undecalactone 10 ^-1 Dihydroactinidiolide 10 ^-1 Damascone 10 ^-5 Dorinone 10 ^-6 Geranyl acetone 10 ^-2 α-ionone 10 ^-3 Phenylethyl alcohol 10 ^-2 Phenylacetaldehyde 10 ^-3 5 methyl furfural 10 ^-2 Ethyl maltol 10 ^-4 Furanone 10 ^-5 Acetophenone 10 ^-2 The fragrant ether of imperial Ting falls 10 ^-3 Farnesyl acetone 10 ^-1

(7) the fragrant and sweet aromatic style feature evaluation of cigarette:

According to the standards of grading of table 3, the fragrant and sweet aromatic style of cigarette is passed judgment on;

The fragrant and sweet aromatic style judgment criteria of table 3 cigarette

Fragrant and sweet feature in cigarette flavor and cigarette fragrant and sweet note index T correlation, namely cigarette fragrant and sweet note index T value is higher, then show that the fragrant and sweet aromatic style of this cigarette is more remarkable.