CN108645746B - Electrical heating non-combustible cigarette sensory quality analysis method based on furnace volatile matter - Google Patents
Electrical heating non-combustible cigarette sensory quality analysis method based on furnace volatile matter Download PDFInfo
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Abstract
The invention relates to an electric heating non-combustible cigarette sensory quality analysis method based on oven volatile matters, which comprises the following steps: step (1), extracting a sample; step (2), measuring volatile matters of the sample furnace; step (3), measuring the moisture in the sample; step (4), sensory evaluation; and (5) predicting the sensory quality by adopting a partial least square method according to the oven volatile matter and moisture results of the sample. The invention provides a method for measuring furnace volatile matters and moisture of the cigarette core of an electric heating non-combustible cigarette for the first time, particularly the furnace volatile matters are used as measurement indexes for the first time, the method is simple, convenient and quick, and a foundation is laid for quantitative and qualitative analysis of the cigarette core of the electric heating non-combustible cigarette. The model can be used for objectively evaluating the quality of the cigarette sample, and errors caused by artificial smoking evaluation are avoided. The invention can quantify whether peculiar smell and mildew exist through the values of three indexes of smoke quantity, aroma, fragrance and strength.
Description
Technical Field
The invention relates to a sensory quality analysis method for an electric heating non-combustible cigarette, in particular to a sensory quality analysis method for an electric heating non-combustible cigarette based on furnace volatile matters, and belongs to the field of cigarettes.
Background
The electric heating non-combustion cigarette refers to that the tobacco sheet prepared by the paper making method is heated by means of physics, chemistry, electricity and the like, so that the tobacco sheet generates smoke and is sucked by people. The tobacco products are classified as 'heating non-burning tobacco products' by the national tobacco administration because the appearance and the manufacturing process of the tobacco products are similar to those of tobacco products. The core substrate is similar to cigarette tobacco, is a sheet manufactured by a dry papermaking process, is a main source of cigarette smoke which is not combusted by heating, and is a core carrier for consumer consumption experience.
The sensory quality of the electrically heated non-combustible cigarette is an important index for evaluating the electrically heated non-combustible cigarette, sensory evaluation is usually carried out according to the evaluation standard of the conventional cigarette at present, however, the existing evaluation standard is manually evaluated, the subjectivity is too strong, and the sensory quality of the cigarette, especially the sensory quality of the electrically heated non-combustible cigarette, cannot be objectively reflected.
Meanwhile, aiming at the electric heating non-combustible cigarette, the smoke amount, aroma and strength are required to be graded, whether peculiar smell and mildew exist is judged, subjective factors are eliminated, and aiming at smoke evaluators, special training is required, manpower and material resources are wasted, the quality of the cigarette is identified through manual smoking, and the cigarette is harmful to human bodies, especially when the cigarette with peculiar smell and mildew is smoked, so that a method for replacing manual smoke evaluative is required. The existing common cigarette researches the quality trend of cigarette formula by analyzing chemical components or quantitatively analyzing volatile components or non-volatile components by using a chemical method, however, the chemical method has the defects of low speed, more data and complex analysis method.
The oven volatile matter is the sample oven volatile matter which is the ratio of the reduced weight to the original weight of the sample when a new base material of the cigarette which is not burnt is heated to a constant weight under a specified drying temperature, and the oven volatile matter contains various substances, including volatile/semi-volatile organic compounds, moisture and the like, and is expressed by percentage.
At present, no method for measuring electric heating non-combustible cigarette furnace volatile matters exists, the furnace volatile matters have certain influence on the sensory quality of the electric heating non-combustible cigarettes, and research and analysis based on the furnace volatile matters are considered for objectively and conveniently evaluating the sensory quality of the electric heating non-combustible cigarettes.
Disclosure of Invention
In order to make up for the blank of the prior art, the invention provides an electric heating non-combustible cigarette sensory quality analysis method based on oven volatile matters, and the specific scheme of the invention is as follows:
the sensory quality analysis method of the electric heating non-combustible cigarette based on the oven volatile matter comprises the following steps:
step (1), sample extraction: extracting sufficient finished product electric heating non-combustible cigarette cigarettes of the same brand from the same batch of the rolling production line; dividing the smoke into two parts, wherein one part is used for measuring furnace volatile matters and water, and the other part is used for performing smoke panel test according to sensory technical requirements;
step (2), volatile matter determination of a sample furnace:
taking out two core base materials with the same mass from the cigarette, wherein one core base material is used for measuring oven volatile matters, putting the core base materials into a sample box with a known weight, and weighing in time to obtain m 1;
opening the cover of the sample box, placing the sample box in an oven, and drying by blowing, wherein the placing density of the sample box is not less than l/120 cm 2; starting timing when the temperature rises back and is kept at (120 +/-2) ° C; timing to about 40min, covering, taking out the sample box, placing into a dryer, cooling to room temperature, and weighing to obtain m 2;
the furnace volatiles are calculated according to equation (1)
In the formula:
WL- - -furnace volatiles,%;
m1- -core substrate mass before baking, in grams;
m2- -the amount of the core base material after baking, the unit is gram;
step (3), measurement of moisture in sample
Another portion of the core substrate was used for moisture determination;
step (4), sensory evaluation
The other part of the samples are evaluated according to the sensory technical requirements, the smoke quantity, the aroma, the fragrance and the strength of the samples are evaluated, and whether peculiar smell and mildew exist or not is judged;
and (5) predicting the sensory quality by adopting a partial least square method according to the oven volatile matter and moisture results of the sample.
Further, in the step (2), the sampling quantity is determined according to the weight of the core base material of a single cigarette, the total weight of the core base material in each sample box is ensured to reach 3.0 g-3.5 g, and timely capping and weighing are carried out.
Further, the moisture determination comprises the following steps:
step (3.1), preparation of Standard solution
Weighing a certain amount of distilled water or deionized water as an internal standard substance, dissolving the internal standard substance in an extracting agent, preparing at least 4 standard solutions, wherein the concentration range of the standard solutions covers the detected water concentration of the sample solution, and one standard solution is blank without adding water as a solvent;
step (3.2), preparation of sample extract
Dissolving the core substrate in a volume of extractant to ensure that the extractant submerges the filter disc or the volume of the extractant is adjusted to give a suitable standard curve moisture concentration range; vibrating and extracting for at least 20min to ensure that the core base material is not shaken to be broken, so that the water content of the core base material is completely extracted, and preparing a sample extract;
step (3.3), making a standard curve
Respectively injecting the standard solutions into a gas chromatographic column, recording peak areas or peak heights of the water and the internal standard substance, and performing at least two times of determination; calculating the peak area ratio or peak height ratio of the water content of each standard solution and the internal standard substance, making a relation curve of the water content and the peak area ratio or peak height ratio, or calculating a regression equation, wherein the correlation coefficient of the regression curve is more than 0.999;
step (3.4), measurement
Injecting the sample extraction liquid and the blank extraction liquid into a gas chromatograph respectively, calculating the peak area ratio or the peak height ratio of the target substance and the internal standard substance, repeatedly measuring for two times under the same condition, and calculating the average value of parallel measurement;
step (3.5), calculating
Calculating the water concentration of the sample extraction liquid and the blank extraction liquid by using a standard curve or a regression equation;
the moisture content of the total particulate matter of the cigarette smoke is obtained by the formula (2):
WS＝(c1-c2)×V…………………………(2)
in the formula:
WS-moisture content of total particulate matter of cigarette smoke, wherein the unit is milligram per cigarette;
c 1-moisture concentration of sample solution in milligrams per milliliter;
c 2-moisture concentration of blank solution in milligrams per milliliter;
v is the volume of the extractant, and the unit is milliliter;
further, the internal standard was dissolved in isopropanol so that the internal standard concentration was 5 mL/L.
Further, the column is a capillary tube, and the capillary tube operating conditions are as follows:
column temperature: an isotherm of 170 ℃; the temperature of a sample inlet is 250 ℃; the temperature of the detector is 250 ℃; carrier gas: helium with the flow rate of 8 mL/min; sample introduction volume: 1.0 μ L; the split ratio is as follows: 5:1.
Further, in the step (4), the number of the smokers is not less than seven at each time, and the smoke amount is scored according to sufficient smoke, slightly less smoke and less smoke; the fragrance and the aroma are given a score according to the full and exquisite fragrance, strong pleasant feeling, sufficient and slightly rough fragrance, better pleasant feeling, slightly rough fragrance and good pleasant feeling; the warhead gives a score as appropriate, slightly larger or smaller, larger or smaller.
Further, in the step (5), the oven volatile matter content obtained in the step (2) and the moisture content obtained in the step (3) are used as a first matrix X, the sensory evaluation result obtained in the step (4) is used as a second matrix Y, and a robust multivariate calibration model of the cigarette sensory quality, the oven volatile matter content and the moisture content is constructed by using the second matrix Y, wherein the relationship between the first matrix X and the second matrix Y is as follows: y ═ XB + E, where X is the set of self variables, i.e. the set of oven volatiles and moisture content; y is a variable set, namely three sensory indexes of smoke amount, aroma, fragrance and strength; b is the regression coefficient, E is the residual matrix.
Further, the method also comprises a step (6) of judging whether peculiar smell and mildew exist according to the predicted values of the three sensory indexes of the smoke quantity, the aroma and the flavor and the strength, and the method specifically comprises the following steps:
(1) calculating the predicted value of the peculiar smell by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the strength, and performing the following steps:
wherein M is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if M is more than or equal to 27.5, peculiar smell exists, and if M is less than 27.5, the peculiar smell is normal;
(2) and calculating the mildew predicted value by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the flavor and the strength according to the following formula:
wherein N is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if N is greater than 13.5, mildew exists, and if N is less than 13.5, the normal condition is obtained.
Compared with the prior art, the invention has the following beneficial effects:
(1) the method for measuring the furnace volatile matter and the moisture of the cigarette core of the electric heating non-combustible cigarette is put forward for the first time, particularly the furnace volatile matter is used as a measurement index for the first time, the method is simple, convenient and quick, and a foundation is laid for quantitative and qualitative analysis of the cigarette core of the electric heating non-combustible cigarette.
(2) According to the invention, the relation between the oven volatile matter and the moisture of the cigarette core and the sensory quality of the electrically heated non-combustible cigarette is researched by a partial least square method, and the smoke quantity, the aroma, the fragrance and the strength of the cigarette core are further predicted according to the content of the oven volatile matter and the moisture of the cigarette core, wherein the smoke quantity, the aroma, the fragrance and the strength average MAE are respectively 0.153, 0.162 and 0.099 which are less than 0.500, so that the established model has good prediction capability on three sensory quality indexes of the smoke quantity, the aroma, the fragrance and the strength, and can be used for objective quality evaluation of cigarette samples, and errors caused by artificial smoking evaluation are avoided.
(3) The predicted values of the three indexes of the smoke quantity, the aroma, the fragrance and the strength selected by the invention have a certain numerical relationship with whether peculiar smell and mildew exist, and the results of whether peculiar smell and mildew exist can be quantized through the values of the three indexes of the smoke quantity, the aroma, the fragrance and the strength.
Drawings
FIG. 1 is a hyperbolic graph of a smoke amount prediction value and a smoke amount evaluation value; wherein, the X axis is the sample number; the Y-axis is the smoke score;
FIG. 2 is a hyperbolic graph of the predicted value and the evaluation value of fragrance and aroma; wherein, the X axis is the sample number; y-axis is fragrance score;
FIG. 3 is a hyperbolic plot of predicted value versus puff comment value for a puff; wherein, the X axis is the sample number; the Y-axis is the stiffness score.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of examples of the present invention, and not all examples. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The sensory quality analysis method of the electrically heated non-combustible cigarette based on oven volatiles in this example.
1. Instrumentation and equipment
Balance: span >50g, precision 0.001 g.
Electric heating air blast drying oven: the temperature fluctuation degree is +/-1 ℃, and the temperature uniformity is +/-2 ℃.
A sample box: a diameter of about 64mm and a height of about 40mm, and good sealing properties are required.
Other tools: silica gel dryers, gloves, blades, scissors, and the like.
Analytical balance: the sensory dose is 0.1 mg.
Gas chromatograph: is provided with a thermal conductivity cell detector, a recorder and an integrator.
Capillary column: an inner diameter of 0.530mm, a film thickness of 40.0 μm, and a column length of 30 m. The stationary phase is bonded polystyrene-divinylbenzene.
2. Reagent: analytical grade reagents were used.
Carrier gas: high purity nitrogen or helium.
Isopropyl alcohol: the water content is not higher than 1.0 mg/mL.
Internal standard substance: the ethanol or the methanol is more than or equal to 99 percent.
Standard substance: distilled or deionized water.
Extracting agent: the internal standard was dissolved in isopropanol so that the internal standard concentration was typically 5 mL/L. If the temperature of the extractant is not controlled during storage, the temperature of the extractant should be balanced to (22 +/-2) DEG C before use.
Standard solution:
accurately weighing 10 microliters of standard substance in the extractant to an accuracy of 0.01mg to prepare at least 4 standard solutions whose concentrations should range over the expected detected water concentration in the sample solution, wherein one standard solution is free of water (solvent blank).
To prevent water absorption, the container holding the extractant should be equipped with a dewatering device, all solutions should be sealed, and the extractant should be continuously stirred before use to homogenize the water. The extractant used for the standard solution preparation should be the same batch as the extractant. It is recommended that the standard solution be prepared at least once a week.
3. Sample extraction
Extracting 60 finished products of the same brand, namely, electrically heated non-combustible cigarettes from the same batch of the cigarette production line; 30 of these measured oven volatiles and sample moisture; the remaining 30 were reviewed according to sensory technical requirements;
4. sample oven volatiles determination:
(1) switching on the power supply of the oven, turning on the heating switch and the blast switch, and keeping the ventilation opening at a half-open state, wherein the temperature in the oven is stabilized at (120 +/-2) DEG C.
(2) And opening the cover of the sample box, placing the sample box and the first sample box cover in a drying oven for drying for 30min in a blowing way, covering, taking out the sample box, placing the sample box in a dryer, cooling to room temperature, weighing to the weight of 0.001g, and immediately placing the sample box in the dryer.
(3) Cigarette sample preparation
And taking out the core substrate, putting the core substrate into a sample box with a known weight, weighing the core substrate in time until the weight is accurate to 0.00lg, repeating the steps, and preparing a sample.
The sampling quantity is determined according to the weight of the single cigarette core base material, the total weight of the core base material in each sample box is ensured to reach 3.0 g-3.5 g, and the sample box is covered and weighed timely.
(4) Opening the cover of the sample box, placing the sample box in an oven, and drying by blowing, wherein the placing density of the sample box is not less than l/120 cm 2; and starting timing when the temperature rises back and is kept at (120 +/-2) DEG C.
(5) The time is up to 40min, the sample box is taken out by covering and placed in a dryer, and the sample box is weighed to the accuracy of 0.001g after being cooled to the room temperature. The measuring person should wear the spun yarn gloves during the measuring process.
The furnace volatiles are calculated according to equation (1)
In the formula:
WL- - -furnace volatiles,%;
m1- -core substrate mass before baking in grams (g);
m2- -amount of core base material after baking in units of grams (g).
The oven volatiles measurements are expressed as the average of the parallel test results to the nearest 0.01%.
If the absolute value difference of the parallel test results is more than 0.30%, the test should be re-sampled. The oven volatile content of the samples of this example are shown in table 1.
5. Determination of moisture in a sample
Step (1) preparing a standard solution
Weighing 50mL of distilled water or deionized water as an internal standard substance, dissolving the internal standard substance in an extracting agent, preparing at least 4 standard solutions, wherein the concentration ranges of the standard solutions cover the detected water concentration of a sample solution, and one standard solution is blank without adding water as a solvent;
step (2) preparing a sample extract
Dissolving the core substrate in a volume of extractant to ensure that the extractant submerges the filter disc or the volume of the extractant is adjusted to give a suitable standard curve moisture concentration range; vibrating and extracting for at least 20min to ensure that the core base material is not shaken to be broken, so that the water content of the core base material is completely extracted, and preparing a sample extract;
step (3) making a standard curve
Injecting 1.0 μ L of standard solution into gas chromatographic column, recording water and internal standard peak area (or peak height), and performing at least two measurements.
Calculating the peak area ratio (or peak height ratio) of the water content of each standard solution (including solvent blank) and the internal standard substance, making a relation curve of the water content and the peak area ratio (or peak height ratio), or calculating a regression equation, wherein the correlation coefficient of the regression curve is more than 0.999.
The standard curve was generated once per test batch. In addition, after every 20 samples are measured, a medium concentration standard solution should be injected, and if the obtained result is different from the original value by more than 5%, the whole standard curve should be made again.
Step (4), measurement
Injecting the sample extraction liquid and the blank extraction liquid into a gas chromatograph respectively, calculating the peak area ratio or the peak height ratio of the target substance and the internal standard substance, repeatedly measuring for two times under the same condition, and calculating the average value of parallel measurement;
step (5), calculating
Calculating the water concentration of the sample extraction liquid and the blank extraction liquid by using a standard curve or a regression equation;
the moisture content of the total particulate matter of the cigarette smoke is obtained by the formula (2):
WS＝(c1-c2)×V…………………………(2)
in the formula:
WS is the moisture content of the total particulate matter of the cigarette smoke, and the unit is milligram per cigarette;
c 1-moisture concentration of sample solution in milligrams per milliliter;
c 2-moisture concentration of blank solution in milligrams per milliliter;
v is the volume of the extractant, and the unit is milliliter;
the results were accurate to 0.01mg per channel, with an average value of 0.01 mg.
In preparation for the gas chromatograph, the gas chromatograph is adjusted and operated according to the manufacturer lifetime to ensure complete separation of the moisture, internal standard and solvent peaks. The analysis time is about 4min, and 2. mu.L of extractant conditioning instrument should be injected before analysis. The oven volatile content of the samples of this example are shown in table 1.
TABLE 1 oven volatiles and moisture content of samples to be tested
6. Sensory evaluation
The other part of the sample is evaluated according to the sensory technical requirements, and the smoke quantity, the aroma, the fragrance and the strength are evaluated; judging whether peculiar smell and mildew exist;
the sensory quality judgment standard of the electric heating non-burning cigarette is shown in the table 2:
TABLE 2 sensory quality evaluation criteria for electrically heated non-combustible cigarettes
The sensory quality defect is class a, i.e. a severe quality defect. The method comprises the following steps: has obvious peculiar smell or mildew.
The sensory was measured by the dark scoring method, as given in Table 2. The number of persons participating in the evaluation is not less than seven persons each time.
The verification rule is as follows:
the sensory quality score is made by percentage, and the highest score is 100. Each item is divided into score units of 0.5.
When the smoke amount, the aroma and the fragrance and the strength are evaluated, the quality of each item meets the requirements of the corresponding item, and the corresponding evaluation is carried out.
And (4) counting results:
the single term average score was calculated to the nearest 0.01 according to the following formula.
In the formula:
∑Xi-some singleton score is summed;
n-the number of persons participating in the evaluation;
The sensory quality score is expressed as the sum of the individual mean scores to the nearest 0.1. The amount of smoke, aroma and flavor, and strength index scores of the samples of this example are shown in table 3.
Table 3 Smoke amount, aroma, flavor, strength, odor, and mildew evaluation results of the other part of the samples
7. According to the oven volatile matter and moisture results of the samples, the changes of the sensory quality trend of the samples are researched by adopting a partial least square method.
7.1 Partial Least Squares (PLS) model
Taking the oven volatile matter content obtained in the step (2) and the moisture content obtained in the step (3) as a first matrix X, taking the sensory evaluation result obtained in the step (4) as a second matrix Y, and constructing a robust multivariate calibration model of the cigarette sensory quality, the oven volatile matter content and the moisture content by using the second matrix Y, wherein the relationship between the first matrix X and the second matrix Y is as follows: y ═ XB + E, where X is the set of self variables, i.e. the set of oven volatiles and moisture content; y is a variable set, namely three sensory indexes of smoke amount, aroma, fragrance and strength; b is the regression coefficient, E is the residual matrix.
7.2 data analysis
A PLS processing module of SIMCA-P11.5 software (Umetrics AB Inc.) is adopted, oven volatile matters and water content are used as an X matrix, and 3 sensory characteristics (smoke amount, aroma, fragrance and strength) are used as a Y matrix to construct a robust multivariate calibration model between the cigarette sensory quality and the oven volatile matters and the water content.
3 main sensory characteristic aroma style characteristics of the electric heating non-burning cigarette are expressed by a yn (n is 1-3) variable to form a sensory characteristic Y matrix. Each sensory style characteristic score of different samples is different, and no zero score is existed. As can be seen from Table 4, there are significant differences in the sensory style characteristics of the different samples of cigarettes. Independent variables are two indicators of oven volatiles and moisture, represented by xn (n ═ 1-2) variables, making up the X matrix.
7.3 creation of PLS model of this example
Taking the contents of volatile matters and water of 30 to-be-measured heated non-burning cigarette sample furnaces as an independent variable matrix X, taking 3 sensory fragrance style characteristic indexes of the sample as a dependent variable matrix Y, carrying out NIPALS modeling analysis, wherein the number of latent variables T obtained by PLS model decomposition is 5, and the model has strong explanatory power on Y1 (smoke amount), Y2 (fragrance and fragrance) and Y3 (strength) sensory indexes.
The contribution degree of X (furnace volatile matter) is large, the regression coefficient B is 0.866, and the increase of the content of the furnace volatile matter can increase the smoke quantity, the aroma and the flavor and the strong evaluation score; the reverse contribution of X (moisture content) is large, the regression coefficient B is-0.259, and a decrease in moisture content may also increase the amount of smoke, aroma, flavor, and strong evaluation scores.
7.4 validation of the PLS model
The oven volatiles and water contents of the samples to be tested (30 samples) were substituted into the PLS model established in 6.3 to calculate and predict the smoke amount, aroma, fragrance and strength index scores, the results are shown in Table 4,
TABLE 4 prediction results of the smoke amount, aroma, flavor, strength, odor, and mildew indexes of the samples to be tested
The results of the sensory evaluation are plotted as a hyperbolic curve, as shown in fig. 1-3, it can be seen that the model has good prediction effect on the test set, and the error between the predicted value and the actual value is small on each sample. And calculating MAE values (absolute errors) of two sets of a predicted value and an actual smoking result, wherein the smoke quantity, the aroma and fragrance and the average MAE of the strength of the test set are 0.153, 0.162 and 0.099 which are less than 0.500 in sequence, so that the established model has good prediction capability on three sensory quality indexes of the smoke quantity, the aroma and fragrance and the strength, and can be used for objectively evaluating the quality of a cigarette sample.
Judging whether peculiar smell and mildew exist according to the predicted values of three sensory indexes of the smoke quantity, the aroma and the strength, which comprises the following steps:
(1) calculating the predicted value of the peculiar smell by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the strength, and performing the following steps:
wherein M is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if M is more than or equal to 27.5, peculiar smell exists, and if M is less than 27.5, the peculiar smell is normal. The results are shown in table 4, the odor values of nos. 6, 11, 12, and 13 are greater than 27.5, and the presence of odor was judged to be consistent with the actual smoking results in table 3.
(2) And calculating the mildew predicted value by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the flavor and the strength according to the following formula:
wherein N is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if N is greater than 13.5, mildew exists, and if N is less than 13.5, the normal condition is obtained. The results are shown in Table 4, the mildew values of No. 6 and No. 11 are greater than 13.5, and it is judged that there is mildew, and the results are consistent with the actual results of the smoking in Table 3.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (7)
1. The sensory quality analysis method of the electric heating non-combustible cigarette based on the oven volatile matter is characterized by comprising the following steps of: the method comprises the following steps:
step (1), sample extraction: extracting sufficient finished product electric heating non-combustible cigarette cigarettes of the same brand from the same batch of the cigarette production line; dividing the smoke into two parts, wherein one part is used for measuring furnace volatile matters and water, and the other part is used for performing smoke panel test according to sensory technical requirements;
step (2), volatile matter determination of a sample furnace:
taking out two parts of core base material with the same mass from the cigarette, wherein one part is used for measuring oven volatile matter, putting the core base material into a sample box with known weight, and weighing in time to obtain m1；
Opening the cover of the sample box, placing the sample box in an oven, and drying by blowing air at the middle layer, wherein the placing density of the sample box is not less than l/120 cm2(ii) a Starting timing when the temperature rises back and is kept at 120 +/-2 ℃; timing to 40min, covering, taking out the sample box, placing into a dryer, cooling to room temperature, and weighing to obtain m2；
The content of furnace volatiles is calculated according to the formula (1)
In the formula:
WL- - -furnace volatile content,%;
m1-core substrate mass before baking in grams;
m2-the amount of core base material after baking in grams;
step (3), measurement of moisture in sample
Another portion of the core substrate was used for moisture determination;
step (4), sensory evaluation
The other part of the samples are evaluated according to the sensory technical requirements, the smoke quantity, the aroma, the fragrance and the strength of the samples are evaluated, and whether peculiar smell and mildew exist or not is judged;
step (5), predicting the sensory quality by adopting a partial least square method according to the oven volatile matter and moisture results of the sample;
taking the oven volatile matter content obtained in the step (2) and the moisture content obtained in the step (3) as a first matrix X, taking the sensory evaluation result obtained in the step (4) as a second matrix Y, and constructing a robust multivariate calibration model of the cigarette sensory quality, the oven volatile matter content and the moisture content by using the second matrix Y, wherein the relationship between the first matrix X and the second matrix Y is as follows: y = XB + E, where X is a set of self-variables, i.e. a set of oven volatiles and moisture content; y is a variable set, namely three sensory indexes of smoke amount, aroma, fragrance and strength; b is a regression coefficient, E is a residual matrix, and then predicted values of three sensory indexes of the smoke quantity, the aroma and the strength are obtained according to the furnace volatile matter content and the water content.
2. A sensory quality analysis method according to claim 1, characterized in that: in step (2), the number of samples to be taken is determined in accordance with the weight of the core substrate for a single cigarette, ensuring that the total weight of core substrate in each sample box is between 3.0 g-3.5 g, and taking care to cover and weigh in time.
3. A sensory quality analysis method according to claim 1, characterized in that: the moisture determination comprises the following steps:
step (3.1), preparation of Standard solution
Weighing a certain amount of distilled water or deionized water as an internal standard substance, dissolving the internal standard substance in an extracting agent, preparing at least 4 standard solutions, wherein the concentration range of the standard solutions covers the moisture concentration expected to be detected in a sample solution, and one standard solution is blank without adding water as a solvent;
step (3.2), preparation of sample extract
Dissolving the core substrate in a volume of extractant to ensure that the extractant submerges the filter disc or the volume of the extractant is adjusted to give a suitable standard curve moisture concentration range; vibrating and extracting for at least 20min to ensure that the core base material is not shaken to be broken, so that the water content of the core base material is completely extracted, and preparing a sample extract;
step (3.3), making a standard curve
Respectively injecting the standard solutions into a gas chromatographic column, recording peak areas or peak heights of the water and the internal standard substance, and performing at least two times of determination; calculating the peak area ratio or peak height ratio of the water content of each standard solution and the internal standard substance, making a relation curve of the water content and the peak area ratio or peak height ratio, or calculating a regression equation, wherein the correlation coefficient of the regression curve is more than 0.999;
step (3.4), measurement
Injecting the sample extraction liquid and the blank extraction liquid into a gas chromatograph respectively, calculating the peak area ratio or the peak height ratio of the target substance and the internal standard substance, repeatedly measuring for two times under the same condition, and calculating the average value of parallel measurement;
step (3.5), calculating
Calculating the water concentration of the sample extraction liquid and the blank extraction liquid by using a standard curve or a regression equation;
the moisture content of the total particulate matter of the cigarette smoke is obtained by the formula (2):
WS=（c1-c2）×V…………………………（2）
in the formula:
WS-moisture content of total particulate matter of cigarette smoke, wherein the unit is milligram per cigarette;
c 1-moisture concentration of sample solution in milligrams per milliliter;
c 2-moisture concentration of blank solution in milligrams per milliliter;
v is volume of extractant, and the unit is milliliter.
4. A sensory quality analysis method according to claim 3, characterized in that: the internal standard was dissolved in isopropanol so that the internal standard concentration was 5 mL/L.
5. A sensory quality analysis method according to claim 3, characterized in that: the chromatographic column is a capillary tube, and the operation conditions of the capillary tube are as follows:
column temperature: an isotherm of 170 ℃; the temperature of a sample inlet is 250 ℃; the temperature of the detector is 250 ℃; carrier gas: helium with the flow rate of 8 mL/min; sample introduction volume: 1.0 μ L; the split ratio is as follows: 5:1.
6. A sensory quality analysis method according to claim 1, characterized in that: in the step (4), the number of the smokers is not less than seven at each time, and the smoke amount is scored according to sufficient smoke, slightly less smoke and less smoke;
the fragrance and the aroma are given a score according to the full and exquisite fragrance, strong pleasant feeling, sufficient and slightly rough fragrance, better pleasant feeling, slightly rough fragrance and good pleasant feeling; the tightening head is suitable, slightly larger or smaller, larger or smaller
A score is given.
7. A sensory quality analysis method according to claim 1, characterized in that: the method also comprises a step (6) of judging whether peculiar smell and mildew exist according to the predicted values of the three sensory indexes of the smoke quantity, the aroma and the strength, and the method specifically comprises the following steps:
(1) calculating the predicted value of the peculiar smell by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the strength, and performing the following steps:
wherein M is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if M is more than or equal to 27.5, peculiar smell exists, and if M is less than 27.5, the peculiar smell is normal;
(2) and calculating the mildew predicted value by using the predicted values of the three sensory indexes of the smoke amount, the aroma and the flavor and the strength according to the following formula:
wherein N is a predicted odor value, x is a predicted smoke amount value, y is a predicted fragrance and aroma value, and z is a predicted strength value; if N is greater than 13.5, mildew exists, and if N is less than 13.5, the normal condition is obtained.
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