CN103995087A - Method for testing cigarette fragrance sense sensorial threshold - Google Patents
Method for testing cigarette fragrance sense sensorial threshold Download PDFInfo
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- CN103995087A CN103995087A CN201410212857.XA CN201410212857A CN103995087A CN 103995087 A CN103995087 A CN 103995087A CN 201410212857 A CN201410212857 A CN 201410212857A CN 103995087 A CN103995087 A CN 103995087A
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Abstract
The invention relates to a method for testing a cigarette fragrance sense sensorial threshold. The method specifically comprises the following steps: 1) diluting cigarette fragrance to initial concentration by using ethanol, and subsequently diluting into four concentration gradients according to a ratio of 1/3, 1/9, 1/27 and 1/81 of the initial concentration; 2) quantitatively injecting into cigarette, at the same time, injecting ethanol of the same concentration to prepare a blank sample, and balancing according to demands; 3) performing smoke panel testing by using a method that blind testing and comparison in pair by at least 13 people are combined, so as to primarily confirm a concentration range of the threshold; 4) inserting a concentration value A in the middle of the threshold concentration range obtained in the step 3), performing smoke panel testing according to the method of the step 3), so as to further reduce the concentration range of the threshold; 5) inserting a concentration value B in the middle of the threshold concentration range obtained in the step 4), performing smoke panel testing by using a three-point verification method by 5-7 people, and repeating the steps till a threshold point is found. The method can confirm which substances can function on the sense of the cigarette and the function degree, and thus has great development prospect.
Description
Technical field
The invention belongs to tobacco aromatics using threshold value determination technical field, a kind of method that is specifically related to sensory evaluating smoking of employing is measured the sense organ threshold value of tobacco aromatics using.
Background technology
In recent years, the direction that State Tobacco Monopoly Bureau proposes China's tobacco science and technology future development is that the sound tobacco of carrying out " lowering harm and decreasing coking " technical research comprehensively, serving as theme, meet to develop Chinese-style cigarette and production tobacco industry needs to implement " lowering harm and decreasing coking " engineering is attached most importance to, General Promotion Chinese tobacco scientific and technological level.Yet, along with carrying out in a deep going way of " lowering harm and decreasing coking " engineering, the problem that cigarette flavor amount and flavouring essence quality reduce, dry sensation is obvious, physiology satisfaction deficiency etc. directly affects the inherent organoleptic quality of cigarette constantly manifests, especially the in the situation that of the existing very large decline of tar content at present, further significantly fall Jiao, the problems referred to above more and more highlight.Therefore, how to increase cigarette flavor amount, carry raise note, set off nature cigarette fragrant, reduce flue gas drying sense, strengthen flue gas promote the production of body fluid sense, raising cigarette comfort level and satisfaction, cigarette product after further " lowering harm and decreasing coking " still can be accepted by consumer, become the main attack problem of China's tobacco business and Chinese-style cigarette development.
Threshold value in fragrance refers to the least concentration value that fragrance matter is experienced by people's sense organ in certain medium, comprises in theory sense of smell and taste threshold.In food threshold value determination, generally include and only depend on fragrance (smell) threshold value of sense of smell evaluation or the taste threshold of measuring by trial test, can be referred to as identification threshold value.For cigarette, need the sense of taste, sense of smell and sense of touch acting in conjunction to experience the situation of flue gas.Modern study is found, the composition of having identified in flue gas has kind more than 5000, wherein to cigarette flavor is influential, there is a solanone, phenylethyl alcohol, Megastigmatrienone, geranyl acetone, furfural, maltol, damascone, irisone, benzaldehyde, acetyl pyrroles etc. are hundreds of, yet this class material not only has the effect of the draft perfume (or spice) of being fuming, can augment the characteristic perfume of all kinds of tobaccos, and can directly affect the mellow and full sense of cigarette cigarette, alkaline matter wherein has extremely strong supplementary function to the physiology satisfaction of cigarette, the aromatic style that has caused people to bring when the cigarette of suction different brands due to the difference of these micro constitutent content, difference in flue gas impression and sense organ comfortableness, this is also to highlight cigarette brand style and features simultaneously, allow consumer understand the style and features of cigarette and the key of cigarette brand expansion and development.In the production run of cigarette, need to add different tobacco aromatics using compositions, these tobacco aromatics using compositions have different action effects under different additions, when addition is high, may, when affecting cigarette flavor, bring the variation of smoke behavior and pleasant impression; When addition is low, may not affect cigarette flavor, but can bring the variation of smoke behavior and pleasant impression aspect, such as: make flue gas enrichment, flue gas is mellow and full or conglobation property improves, or make cigarette pleasant impression comfortable, increase sweetly promote the production of body fluid, pungency diminishes, etc.
Yet, in current China tobacco business, the evaluation of tobacco aromatics using monomer and when application are mainly investigated to the impact that it changes cigarette interior quality, in evaluation procedure, tobacco aromatics using consumption is selected all more arbitrarily, lacks relevant reference data.Therefore want correctly to evaluate the size of tobacco aromatics using to cigarette organoleptic effect, must know its threshold value to cigarette organoleptic effects.The sense organ threshold value of tobacco aromatics using is the least concentration value that this composition reflects when sense organ Comprehensive Assessment; It or affects the odor characteristic of cigarette under this concentration value, or affects the smoke behavior of cigarette, or the comfortableness of fragrance cigarette, etc.The method of the mensuration tobacco aromatics using sense organ threshold value the present invention relates to, be exactly after determining above-mentioned a certain tobacco aromatics using sense organ threshold value, by Modern Methods, obtain the concentration of this material in cigarette, by analyzing this material concentration obtaining, remove in its sense organ threshold value, can obtain the active threshold value of the sense organ of this material in certain cigarette.By comparing the size of the active threshold value of sense organ of different material in this complicated fragrance system of flue gas, can determine which material works to cigarette organoleptic feature, the degree of effect is how.The inventive method can connect cigarette flavor component and essence and flavoring agent constituent analysis result and cigarette sense organ, in formula and blending, brings into play application effect, and then raising cigarette technical merit.
Summary of the invention
For overcoming prior art defect, the object of the invention is to provide a kind of assay method of tobacco aromatics using sense organ threshold value, in order to greatly to improve cigarette technical merit.
For achieving the above object, the present invention adopts following technical scheme:
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) accurately take a certain amount of tobacco aromatics using, after diluting with ethanol, as initial concentration, then according to the dilution proportion of initial concentration 1/3,1/9,1/27,1/81, become four concentration gradients;
2) according to pipe tobacco weight 1% by the tobacco aromatics using calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, under the condition of 22 ± 2 ℃ of relative humidity 60 ± 5%, temperature, balance is 48 hours;
3) group of smokeing panel test that is comprised of minimum 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, and interpretation of result adopts the probability statistical analysis under 5% level of signifiance, according to statistics, carrys out the concentration of definite threshold point below and more than threshold point; If four concentration all more than threshold point, further dilution; If four concentration all, below threshold point, increases the concentration of tobacco aromatics using, until tentatively determine the concentration range of threshold value, be designated as concentration I (lower limit)-concentration II (upper limit);
4) in the middle of the threshold concentration scope obtaining in step 3), (be the mean value of concentration I and concentration II, lower same) a concentration value A of insertion, according to the test of smokeing panel test of the method for step 3), according to smoking result, determine that the concentration value A that inserts is whether more than threshold point; If more than threshold point, in the middle of concentration I and this concentration, (i.e. the mean value of two concentration) inserts a concentration value again; If below threshold point, in the middle of this concentration and concentration II, (i.e. the mean value of two concentration) inserts a concentration value again; So repeat 0-4 test and further dwindle the concentration range of threshold value, be designated as concentration III (lower limit)-concentration IV (upper limit);
5) in the middle of the threshold concentration scope obtaining in step 4), (be the mean value of concentration III and concentration IV, lower same) a concentration value B of insertion, organize again a 5-7 people's the group of smokeing panel test to adopt the test of smokeing panel test of three-point assay method, interpretation of result adopts the probability statistical analysis under 5% level of signifiance, and whether the concentration value determine inserting according to smoking result is more than threshold point; If more than threshold point, in the middle of concentration III and this concentration value B, (i.e. the mean value of two concentration) inserts a concentration value again; If below threshold point, in the middle of this concentration value B and concentration IV, (i.e. the mean value of two concentration) inserts a concentration value again; So revision test is further dwindled the concentration range of threshold value, until find threshold point.
Concrete; tobacco aromatics using described in step 1) can be phenylethyl alcohol, maltol, solanone, Megastigmatrienone, geranyl acetone, damascone, irisone, strawberry furanone, methyl cyclopentenyl ketone, 2,3-dimethyl pyrazine, furfural, geranyl acetone, 2-acetyl group pyrazine or acetyl pyrrole etc.
In described step 3), adopt the blind method of commenting and relatively combining in pairs, be specially: often take turns the test of smokeing panel test two samples are provided, one be blank sample A, and another is the sample B of interpolation tobacco aromatics using; By sample being numbered to the information whether cigarette is added to tobacco aromatics using, conceal, each sample encoded is chosen at random 3 figure places and is formed; The number of times that sample A, B and B, these two kinds of order of A occur equates, and each sample encoded of smokeing panel test between personnel does not repeat as far as possible; In the process of smokeing panel test, every smoke panel test personnel according to by low concentration to the order of high concentration to passing judgment in the difference aspect odor characteristic between the two, determine the cigarette that wherein adds tobacco aromatics using; For reduce the error that artificial conjecture factor causes, each concentration suction two-wheeled, just two-wheeled all correct judgment person calculate correctly, otherwise miscalculation.
Three-point assay method in described step 5) is specially: everyone provides three cigarette at every wheel, wherein two, or add tobacco aromatics using or for blank, on every cigarette all by one group of different coding being formed by 3 figure places, after being smoked panel test by the personnel that smoke panel test, determine that wherein different cigarette, the error causing in order to reduce artificial conjecture factor, each concentration suction two-wheeled, two-wheeled all correct judgment person is just calculated correctly, otherwise miscalculates.
In the present invention, in the personnel that smoke panel test requirement, smoke panel test environmental requirement and the process of smokeing panel test, the removing of the residual smoke in oral cavity is carried out with reference to YC/T 138-1998.The personnel that smoke panel test preferably possess the work experience of more rich cigarette product exploitation and maintenance or blending, have accumulated abundant sensory evaluation experience.
Compared to the prior art, beneficial effect of the present invention:
In recent years, Chinese tobacco keeps high speed development, and the development of industry has exceeded the transnational tobacco company average speed of development of these three world rankings front threes of Altria group, British American Tobacco and Japan Tobacco Inc (JTI), and the international competitiveness of industry is highly improved.Meanwhile, Chinese tobacco enterprise adheres to scientific-technical progress, carries forward vigorously technological innovation, and the whole industry has strengthened the input to scientific research, and sci-tech innovation ability is strengthened greatly." lowering harm and decreasing coking " of one of four major strategies problem obtains new progress, and aspect production of cigarettes, widespread use new technology, new technology, new material, improve cigarette composition structure, the security that improves cigarette product quality and suck.State Bureaus in 2003 have clearly proposed the strategic problem of development Chinese-style cigarette, formulate < < Chinese cigarette development in science and technology outline > >, emphasized to greatly develop the Chinese-style cigarette with independent intellectual property right and core technology.The present invention meets Chinese tobacco industrial expansion direction completely, meets " the emerging cigarette of science and education " strategy that State Bureau determines.The inventive method can determine which material works to the sense organ of cigarette, and the degree of effect how, has boundless development prospect.
Embodiment
The present invention is described further by the following examples, but protection scope of the present invention is not limited to this.
embodiment 1
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) maltol is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the maltol calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours.
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, it is 12 people that 1/3 initial concentration is smoked panel test correct, it is 8 people that 1/9 initial concentration is smoked panel test correct, and it is 6 people that 1/27 initial concentration is smoked panel test correct, and it is 3 people that 1/81 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the 1/3-1/9 that the concentration range of tentatively determining threshold value is initial concentration, the preliminary threshold range of maltol is that the content of every cigarette is 11ppm(concentration I)-33ppm(concentration II).
4) in the middle of the threshold concentration scope obtaining in step 3), inserting a concentration value A(is 22ppm), according to the test of smokeing panel test of the method for step 3), whether the concentration value 22ppm that determines insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 22ppm concentration is 9 people, illustrates that this concentration is below threshold value; In the middle of 22ppm-33ppm, insert again a concentration value; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 22ppm(concentration III of every cigarette)-27.5ppm(concentration IV).
5) in the middle of the threshold concentration scope obtaining in step 4), insert i.e. 24.8 ppm of a concentration value B(), then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 5 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value 24.8 ppm are more than threshold value, in the middle of 22ppm-24.8ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of maltol in cigarette is that 24ppm/ props up cigarette.
Table 1 Paired Comparisons probability statistical analysis table
3, the table 2 method probability statistical analysis table of smokeing panel test
embodiment 2
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) strawberry furanone is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the strawberry furanone calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours;
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, and it is 12 people that 1/3 initial concentration is smoked panel test correct, and it is 11 people that 1/9 initial concentration is smoked panel test correct, and it is 6 people that 1/27 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the 1/9-1/27 that the concentration range of tentatively determining threshold value is initial concentration, and the preliminary threshold range of strawberry furanone is that the content of every cigarette is 3.7ppm-11ppm;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value 7.4ppm, according to the test of smokeing panel test of the method for step 3), whether the concentration value 7.4ppm that determines insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 7.4ppm concentration is 11 people, illustrates that this concentration is more than threshold value; In the middle of 3.7ppm-7.4ppm, insert again a concentration value 5.5ppm; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 3.7ppm-5.5ppm of every cigarette;
5) in the middle of the threshold concentration scope obtaining in step 4), insert concentration value 4.6 ppm, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 5 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value is more than threshold value, in the middle of 3.7ppm-4.6ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of strawberry furanone in cigarette is that 4.15ppm/ props up cigarette.
embodiment 3
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) methyl cyclopentenyl ketone (MCP) is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the MCP calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours;
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, and it is 12 people that 1/3 initial concentration is smoked panel test correct, and it is 12 people that 1/9 initial concentration is smoked panel test correct, and it is 5 people that 1/27 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the 1/9-1/27 that the concentration range of tentatively determining threshold value is initial concentration, and the preliminary threshold range of MCP is that the content of every cigarette is 3.7ppm-11ppm;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value 7.4ppm, according to the test of smokeing panel test of the method for step 3), whether the concentration value 7.4ppm that determines insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 7.4ppm concentration is 11 people, illustrates that this concentration is more than threshold value; In the middle of 3.7ppm-7.4ppm, insert again a concentration value; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 6.5ppm-7.4ppm of every cigarette.
5) in the middle of the threshold concentration scope obtaining in step 4), insert concentration value 6.95 ppm, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 3 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value 6.95 ppm are below threshold value, in the middle of 6.95ppm-7.4ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of MCP in cigarette is that 7.2ppm/ props up cigarette.
embodiment 4
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) 2,3-dimethyl pyrazine is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by 2 after dilution, 3-dimethyl pyrazine calibrated shot, in cigarette, is injected the ethanol of same concentrations simultaneously and is made blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours;
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, it is 13 people that 1/3 initial concentration is smoked panel test correct, it is 12 people that 1/9 initial concentration is smoked panel test correct, it is 11 people that 1/27 initial concentration is smoked panel test correct, and it is 12 people that 1/81 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the smoking result of four concentration is all more than threshold point, therefore further test is proceeded in dilution, the 1/729-1/2187 that the concentration range of tentatively determining threshold value is initial concentration, 2, the preliminary threshold range of 3-dimethyl pyrazine is that the content of every cigarette is 0.045ppm-0.14ppm;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value 0.09ppm, according to the test of smokeing panel test of the method for step 3), whether the concentration value 0.09ppm that determines insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 0.09ppm concentration is 11 people, illustrates that this concentration is more than threshold value; In the middle of 0.045ppm-0.09ppm, insert again a concentration value; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 0.068ppm-0.09ppm of every cigarette;
5) in the middle of the threshold concentration scope obtaining in step 4), insert a concentration value 0.079ppm, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 3 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value is below threshold value, in the middle of 0.079ppm-0.09ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of 2,3-dimethyl pyrazine in cigarette is that 0.085ppm/ props up cigarette.
embodiment 5
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) furfural is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the furfural calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours.
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, it is 13 people that 1/3 initial concentration is smoked panel test correct, it is 12 people that 1/9 initial concentration is smoked panel test correct, it is 12 people that 1/27 initial concentration is smoked panel test correct, and it is 11 people that 1/81 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the smoking result of four concentration is all more than threshold point, therefore further test is proceeded in dilution, the 1/81-1/243 that the concentration range of tentatively determining threshold value is initial concentration, the preliminary threshold range of furfural is that the content of every cigarette is 0.4ppm-1.2ppm;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value 0.8ppm, according to the test of smokeing panel test of the method for step 3), whether the concentration value 0.8ppm that determines insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 0.8ppm concentration is 11 people, illustrates that this concentration is more than threshold value; In the middle of 0.4ppm-0.8ppm, insert again a concentration value; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 0.6ppm-0.8ppm of every cigarette;
5) in the middle of the threshold concentration scope obtaining in step 4), insert concentration value 0.7 ppm, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 3 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value is below threshold value, in the middle of 0.7ppm-0.8ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of furfural in cigarette is that 0.75ppm/ props up cigarette.
embodiment 6
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) geranyl acetone is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the geranyl acetone calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours.
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, it is 13 people that 1/3 initial concentration is smoked panel test correct, it is 12 people that 1/9 initial concentration is smoked panel test correct, it is 13 people that 1/27 initial concentration is smoked panel test correct, and it is 12 people that 1/81 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the smoking result of four concentration is all more than threshold point, therefore further test is proceeded in dilution, the 1/177147-1/531441 that the concentration range of tentatively determining threshold value is initial concentration, the preliminary threshold range of geranyl acetone is that the content of every cigarette is 0.19ppb-0.56ppb;
4) in the middle of the threshold concentration scope obtaining in step 3), inserting a concentration value A(is 0.38ppb), according to the test of smokeing panel test of the method for step 3), whether the concentration value of determining insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 0.38ppb concentration is 9 people, illustrates that this concentration is below threshold value; In the middle of 0.38ppb-0.56ppb, insert again a concentration value; Revision test is further dwindled the concentration range of threshold value; Determining the concentration range that approaches threshold point is most the 0.38ppb-0.47ppb of every cigarette;
5) in the middle of the threshold concentration scope obtaining in step 4), insert a concentration value 0.43ppb, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 5 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value is more than threshold value, in the middle of 0.38ppb-0.43ppb, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of geranyl acetone in cigarette is that 0.4ppm/ props up cigarette.
embodiment 7
An assay method for tobacco aromatics using sense organ threshold value, it comprises the steps:
1) 2-acetyl group pyrazine is diluted to 1% initial concentration with the ethanol of volumetric concentration 70%, then according to 1/3,1/9,1/27,1/81 dilution proportion, becomes four concentration gradients;
2) adopt essence injector according to pipe tobacco weight 1% by the 2-acetyl group pyrazine calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, in relative humidity 60 ± 5%, under the condition that temperature is 22 ± 2 ℃, balance is 48 hours.
3) group of smokeing panel test that is comprised of 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, it is 13 people that 1/3 initial concentration is smoked panel test correct, it is 13 people that 1/9 initial concentration is smoked panel test correct, it is 13 people that 1/27 initial concentration is smoked panel test correct, and it is 12 people that 1/81 initial concentration is smoked panel test correct.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 1), the smoking result of four concentration is all more than threshold point, therefore further test is proceeded in dilution, the 1/2187-1/6561 that the concentration range of tentatively determining threshold value is initial concentration, the preliminary threshold range of 2-acetyl group pyrazine is that the content of every cigarette is 0.015ppm-0.045ppm;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value 0.03ppm, according to the test of smokeing panel test of the method for step 3), whether the concentration value of determining insertion according to smoking result is below threshold point.The correct number of smokeing panel test under 0.03ppm concentration is 9 people, illustrates that this concentration is below threshold value; Determining the concentration range that approaches threshold point is most the 0.03ppm-0.045ppm of every cigarette;
5) in the middle of the threshold concentration scope obtaining in step 4), insert concentration value 0.038 ppm, then the test of smokeing panel test of the group of smokeing panel test being formed by 7 people employing three-point assay method, the correct number of smoking result is 5 people.Interpretation of result adopts probability statistical analysis under 5% level of signifiance (specifically can referring to table 2), show that this concentration value is more than threshold value, in the middle of 0.03ppm-0.038ppm, inserts a concentration value again; Repeat to smoke panel test and test the concentration range of further dwindling threshold value, finally determining the sense organ threshold value of 2-acetyl group pyrazine in cigarette is that 0.034ppm/ props up cigarette.
Claims (3)
1. an assay method for tobacco aromatics using sense organ threshold value, is characterized in that, comprises the steps:
1) accurately take a certain amount of tobacco aromatics using, after diluting with ethanol, as initial concentration, then according to the dilution proportion of initial concentration 1/3,1/9,1/27,1/81, become four concentration gradients;
2) according to pipe tobacco weight 1% by the tobacco aromatics using calibrated shot after dilution in cigarette, inject the ethanol of same concentrations simultaneously and make blank sample, under the condition of 22 ± 2 ℃ of relative humidity 60 ± 5%, temperature, balance is 48 hours;
3) group of smokeing panel test that is comprised of minimum 13 people adopts the test of smokeing panel test of the blind method of commenting and relatively combining in pairs, and interpretation of result adopts the probability statistical analysis under 5% level of signifiance, according to statistics, carrys out the concentration of definite threshold point below and more than threshold point; If four concentration all more than threshold point, further dilution; If four concentration all, below threshold point, increases the concentration of tobacco aromatics using, until tentatively determine the concentration range of threshold value, be designated as concentration I-concentration II;
4) in the middle of the threshold concentration scope obtaining in step 3), insert a concentration value A, according to the test of smokeing panel test of the method for step 3), whether the concentration value A that determines insertion according to smoking result is more than threshold point; If more than threshold point, in the middle of concentration I and this concentration, insert again a concentration value; If below threshold point, in the middle of this concentration and concentration II, insert again a concentration value; So repeat 0-4 test and further dwindle the concentration range of threshold value, be designated as concentration III-concentration IV;
5) in the middle of the threshold concentration scope obtaining in step 4), insert a concentration value B, organize again a 5-7 people's the group of smokeing panel test to adopt the test of smokeing panel test of three-point assay method, interpretation of result adopts the probability statistical analysis under 5% level of signifiance, and whether the concentration value determine inserting according to smoking result is more than threshold point; If more than threshold point, in the middle of concentration III and this concentration value B, insert again a concentration value; If below threshold point, in the middle of this concentration value B and concentration IV, insert again a concentration value; So revision test is further dwindled the concentration range of threshold value, until find threshold point.
2. the assay method of tobacco aromatics using sense organ threshold value as claimed in claim 1, it is characterized in that, in described step 3), adopt the blind method of commenting and relatively combining in pairs, be specially: often take turns the test of smokeing panel test two samples are provided, one is blank sample A, and another is for adding the sample B of tobacco aromatics using; By sample being numbered to the information whether cigarette is added to tobacco aromatics using, conceal, each sample encoded is chosen at random 3 figure places and is formed; The number of times that sample A, B and B, these two kinds of order of A occur equates, and each sample encoded of smokeing panel test between personnel does not repeat; In the process of smokeing panel test, every smoke panel test personnel according to by low concentration to the order of high concentration to passing judgment in the difference aspect odor characteristic between the two, determine the cigarette that wherein adds tobacco aromatics using; Each concentration suction two-wheeled, two-wheeled all correct judgment person is just calculated correctly, otherwise miscalculates.
3. the assay method of tobacco aromatics using sense organ threshold value as claimed in claim 1, it is characterized in that, three-point assay method in described step 5) is specially: everyone provides three cigarette at every wheel, wherein two the same, or add tobacco aromatics using or for blank, on every cigarette all by one group of different coding being formed by 3 figure places, after being smoked panel test by the personnel that smoke panel test, determine that wherein different cigarette, each concentration suction two-wheeled, two-wheeled all correct judgment person is just calculated correctly, otherwise miscalculates.
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Address after: 450000 Yulin South Road, Henan, Zheng Dong, No. 16 South Road, Zhengzhou Applicant after: China Tobacco Henan Industrial Co., Ltd. Applicant after: Zhengzhou University of Light Industry Address before: 450000 Zhengzhou agricultural road, Henan, No. 29 Applicant before: China Tobacco Henan Industrial Co., Ltd. Applicant before: Zhengzhou University of Light Industry |
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Application publication date: 20140820 |