CN114486616A - Method for evaluating heated cigarette formula based on substance heated quality change information - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 35
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- 239000000126 substance Substances 0.000 title claims abstract description 10
- 238000009472 formulation Methods 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 230000004580 weight loss Effects 0.000 claims abstract description 24
- 238000002411 thermogravimetry Methods 0.000 claims abstract description 13
- 238000011156 evaluation Methods 0.000 claims abstract description 11
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- 238000012360 testing method Methods 0.000 claims description 4
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- 235000002637 Nicotiana tabacum Nutrition 0.000 description 8
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
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- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 1
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- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 1
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- G06F18/21—Design or setup of recognition systems or techniques; Extraction of features in feature space; Blind source separation
- G06F18/213—Feature extraction, e.g. by transforming the feature space; Summarisation; Mappings, e.g. subspace methods
- G06F18/2135—Feature extraction, e.g. by transforming the feature space; Summarisation; Mappings, e.g. subspace methods based on approximation criteria, e.g. principal component analysis
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
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Abstract
The invention discloses a method for evaluating a heated cigarette formula based on substance heated quality change information, which comprises the following steps: (1) preparing a plurality of heated cigarette formula samples and standard formula samples; (2) thermogravimetric experiments; (3) processing the thermogravimetric curve to obtain a differential weight loss curve; (4) calculating the similarity of differential weight loss curves of a plurality of heated cigarette formulas and a standard formula; (5) evaluation of various heated cigarette formulations. The method avoids the influence and difference of subjective factors brought by the traditional artificial sensory evaluation. The method is more objective and efficient, and has the advantages of good repeatability, high sensitivity and simplicity in operation.
Description
Technical Field
The invention belongs to the technical field of tobacco, and particularly relates to a method for evaluating a heated cigarette formula by adopting a principal component-Mahalanobis distance analysis method based on material heated quality change information.
Background
The heating cigarette is also named as a non-burning tobacco product, and is a novel tobacco product. The heating cigarette is to heat the tobacco material by a special heating source, and the nicotine and the flavor substances in the tobacco material are volatilized to generate smoke gas to meet the requirements of smokers during heating. Different from the traditional cigarette, the cigarette is heated without burning, thereby completely changing the smoke generation and transmission mechanism, reducing the harmful components generated by high-temperature combustion and cracking of the tobacco, and effectively improving the safety.
In a mixed system containing two or more components, the process of transferring one or some of the components from a zone of high concentration to a zone of low concentration, due to the difference in concentration, is called a mass transfer process. The mass transfer process can be carried out in one phase or between two phases, and the mass transfer between the two phases is the basis of the separation process; mixing and transport involve changes in mass or concentration within a single phase or between phases. The heat transfer process is physically "similar" to the mass transfer process, involving changes in heat or temperature within or between phases. Whether a conventional tobacco product or a heated cigarette, its use can be described as the tobacco substrate being heated to release smoke material, form an aerosol and be drawn into the oral cavity by suction. Thus, the transport-transport process of smoke substances is the core and the heating of the tobacco substrate is the basis. The thermogravimetric analysis (TG/DTA) can provide stable reaction conditions under the condition of temperature programming, and is the most ideal experimental tool in the research of tobacco pyrolysis. Derivative thermogravimetry, also called derivative thermogravimetry, is derived from the thermogravimetry, and is a technology for recording the first derivative of a TG curve to temperature or time, and the result obtained by experiments is a derivative thermogravimetry curve, namely a DTG curve. The DTG curve is characterized by: the initial reaction temperature, the maximum reaction rate temperature and the reaction termination temperature of each weight loss stage can be accurately reflected; the area of each peak on the DTG curve is in direct proportion to the weight loss of the corresponding sample on the TG curve; when the TG curve is not obvious to the steps of some heating processes, the DTG curve can be obviously distinguished. The thermogravimetry method is mainly characterized by strong quantification and can accurately measure the mass change and the change rate of the substance. According to this feature, whenever a mass change occurs when a substance is heated, it can be studied by thermogravimetry.
At present, the formula development of the heated cigarette mainly adopts a manual smoking evaluation method, a large number of people are used for smoking evaluation and scoring aiming at different raw materials, and finally, a heated cigarette formula sample which is closest to a reference standard formula sample is obtained. The formula development and maintenance mainly depend on experience accumulation and evaluation judgment of formula personnel, and the working intensity is high and the subjectivity is strong. In order to improve the universality of heated cigarette formula development and reduce the workload of formula designers, a standard heated cigarette formula database and a mathematical model which are established by thermogravimetric experiments are utilized, objective data are utilized to assist the development of the heated cigarette formula, and the method has important significance for reducing the influence of subjective factors and the characterization of differences and improving the quality stability of the heated cigarette.
The invention is therefore proposed.
Disclosure of Invention
The invention provides a method for evaluating a formula of a heated cigarette based on material heated quality change information, and particularly relates to a method for evaluating and developing a formula of the heated cigarette by adopting a Mahalanobis distance analysis method of main components according to the material heated quality change information. The method can well avoid the influence of subjective factors and the characterization of differences brought by artificial sensory evaluation in the prior art, improves the universality of the formula development of the heated cigarettes and reduces the workload of formula designers.
The technical scheme of the invention is as follows:
a method for evaluating a heated cigarette formula based on substance heated quality change information comprises the following steps:
(1) preparing a plurality of heated cigarette formula samples and standard formula samples;
(2) thermogravimetric experiments;
(3) processing the thermogravimetric curve to obtain a differential weight loss curve;
(4) calculating the similarity of differential weight loss curves of a plurality of heated cigarette formulas and a standard formula;
(5) evaluation of multiple heated cigarette formulations.
Preferably, the mass of each formula sample in the step (1) is not less than 5g, and the formula sample is balanced in a constant temperature and humidity environment with the temperature of (22 +/-1) DEG C and the relative humidity of (60 +/-2)% for 48 hours before thermogravimetric experiments.
Preferably, the step (2) of the thermogravimetric experiment is: weighing a certain mass (5.00 +/-0.05) mg of the formula sample, placing the formula sample in a crucible, and heating the formula sample by the following temperature rise program: the initial temperature is 30 ℃, the heating rate is 10 ℃/min, the termination temperature is 350 ℃, and the test is carried out under the air flow of 50 mL/min; the sensitivity of the balance is not lower than 0.1 mu g, and the resolution of the curve is not lower than 5000 ten thousand resolution points; before the thermogravimetric experiment, the thermogravimetric analyzer is kept for 10min at 900 ℃ so as to completely discharge impurities in the furnace body.
Preferably, the step (3) of processing the thermogravimetric curve to obtain a differential weight loss curve comprises the following steps: and monitoring the mass change of the formula sample in the pyrolysis process in real time by using a thermogravimetric analyzer, and deriving the weight data with respect to time according to a time-weight relationship diagram to obtain a differential weight loss curve.
Preferably, the step (4) of calculating the similarity of the differential weight loss curve of the heated cigarette formula and the standard formula comprises the following steps: and reducing the dimension of the differential weight loss curve, selecting several main components with the highest contribution rate and the accumulated contribution rate not less than 90 percent according to the contribution rate of each component after dimension reduction, and calculating the Mahalanobis distance between the heated cigarette formula and the standard formula.
Preferably, the step of performing dimension reduction on the differential weight loss curve comprises: decomposing the total number m of the heated cigarette formula samples and the standard formula samples and a weight loss data matrix X (m multiplied by n) of a differential weight loss curve data dimension n into the following forms: x is TPT(ii) a Wherein T (m × n) is a score matrix, and P (m × n) is called a load matrix; and (3) selecting a matrix T (m multiplied by k) consisting of k principal component score vectors with the highest contribution rate and the accumulated contribution rate not less than 90% to replace a differential weightlessness data matrix X, namely the matrix after dimensionality reduction.
Preferably, the cigarette formulation and label are heatedThe Mahalanobis distance calculation of the quasi-formula comprises the following steps: calculating the covariance S of the multi-vector of the matrix T (m × k) after dimension reduction according to a formula
Calculating the mahalanobis distance between the formula of the heated cigarette and the standard formula; wherein t isi,tjRespectively are main component data after the dimensionality reduction of a standard formula and the heated cigarette formula.
Preferably, the evaluation step of the heated cigarette formula in the step (5) is as follows: the smaller the mahalanobis distance, the less the difference between the selected heated cigarette formulation and the standard formulation sample, and the more useful.
The invention has the following beneficial effects:
1. the method avoids subjective factor influence and difference characterization brought by the traditional method of smoking by means of artificial sensory evaluation, improves the universality of heated cigarette formula development, reduces the workload of formula designers, and improves the quality stability of the heated cigarettes.
2. The method is simple to operate, the sample usage amount is extremely small and is within 10 mg; the method does not use any wet chemical means such as solvent and the like, is nontoxic and harmless, has no harm to operators, and does not cause environmental pollution.
3. The method is more objective and efficient, has good repeatability and high sensitivity, and has unique advantages in the development of heating cigarette products in the tobacco industry.
Drawings
FIG. 1 is a TG \ DTG plot of the heated cigarette formulation samples (samples) and the standard formulation samples (standards) of example 1.
Figure 2 is a principal component projection of the heated cigarette formula (specimen) and standard formula (standard) samples of example 1.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited to these examples. The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
1. Selecting 1 standard formula sample and 7 heated cigarette formula samples, respectively weighing 5g, respectively sieving with 100 mesh sieve, and balancing in constant temperature and humidity environment with (22 + -1) deg.C and relative humidity of (60 + -2)% for 48 hr.
2. Before sample analysis, a thermogravimetric analyzer is arranged to be kept for 10min at 900 ℃ so as to completely discharge impurities in the furnace body, and an empty crucible is taken as a reference. Weigh (5.00 ± 0.05) mg of sample into a hot-weight platinum crucible, with the temperature program: the initial temperature was 30 deg.C, the ramp rate was 10 deg.C/min, the end temperature was 350 deg.C, and the test was conducted at a flow rate of 50mL/min air. The sensitivity of the balance is not lower than 0.1 mu g, and the resolution of the curve is not lower than 5000 ten thousand resolution points.
3. And (3) acquiring thermogravimetric curves at 350 ℃ of the heated cigarette formula sample (sample) and the standard formula sample (standard product), and deriving the weight data with respect to time according to the thermogravimetric curves of the relationship between the obtained time and the obtained weight to obtain differential weightlessness curve data. The Thermogravimetric (TG) and thermogravimetric differential curves (DTG) of the heated cigarette formulation (sample) and the standard formulation (standard) are shown in fig. 1.
4. The differential weight loss curve data matrix X (m × n) for the 1 standard formulation sample and the 7 heated cigarette formulation samples described above was decomposed into the following form: x is TPTWhere m is the total number of the standard formula samples and the heated cigarette formula samples, and m is 8; n is the dimension of the data of the differential weight loss curve, and n is 1921; and T (m multiplied by n) is a scoring matrix, each scoring vector is orthogonal, and according to the contribution rate of each scoring vector, k principal component scoring vectors with the highest contribution rate and the accumulated contribution rate not lower than 90% are selected to form a matrix T (m multiplied by n) after dimensionality reduction to replace the original data matrix X (m multiplied by n). The contribution rate of each principal component after dimensionality reduction is shown in table 1; in this example, the first 3 principal components with an accumulated contribution rate of 99%, i.e., k is 3, and the principal component projection result is shown in fig. 2.
TABLE 1 principal Components contribution ratio
| Principal component | PC1 | PC2 | PC3 | PC4 | PC6 | PC7 |
| Rate of contribution | 84.75991 | 11.86536 | 3.120169 | 0.139657 | 0.010374 | 0.0033739 |
5. Calculating the covariance S of the multi-vector of the score matrix T (m × k) of the first 3 selected principal components according to the formula
Calculating the Mahalanobis distance between 7 heated cigarette formula samples and 1 standard formula sample; wherein t isi,tjRespectively are main component data of the standard formula sample and 7 heated cigarette formula samples after dimensionality reduction. The results are shown in Table 2.
TABLE 2 Mahalanobis distance for heated cigarette formula samples and standard formula samples
| | Sample | 1 | |
|
Sample No. 4 | Sample No. 5 | Sample No. 6 | Sample 7 | |
| Mahalanobis distance | 0 | 2.518278 | 2.201948 | 3.166245 | 2.079259 | 2.151341 | 0.857089 | 1.765304 |
As can be seen from table 2, the mahalanobis distance between the heated cigarette formula sample 6 and the standard formula sample was the smallest, and the cigarette formula sample was heated 7 times; the mahalanobis distance between the heated cigarette formula sample 3 and the standard sample is the largest; indicating that the heated cigarette formulation 6 had minimal variability from the standard formulation samples.
In order to further verify the results, the seven heated cigarette formula samples and the standard formula sample tissue expert were subjected to sensory smoking, and the smoking results are shown in table 3.
TABLE 3 sensory test results of the expert
| | Sample | 1 | |
|
Sample No. 4 | Sample No. 5 | Sample No. 6 | Sample 7 | |
| |
100 | 90 | 90 | 85 | 92 | 91 | 97 | 93 | |
| Evaluation of quality Difference | - | Difference | Difference | Greater difference | Difference | Difference | Slight difference | Minor differences |
As can be seen from the results in table 3, the sensory difference between the heated cigarette formulation sample 6 and the standard formulation sample was minimal, the difference between the hot cigarette formulation sample 7 and the standard formulation sample was small, and the difference between the hot cigarette formulation sample 3 and the standard formulation sample was large. Consistent with the calculated mahalanobis distance results of the method of the present invention. The heated cigarette formula sample can be used directly by replacing the standard formula sample with sample 6.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A method for evaluating a heated cigarette formula based on substance heated quality change information is characterized by comprising the following steps:
(1) preparing a plurality of heated cigarette formula samples and standard formula samples;
(2) thermogravimetric experiments;
(3) processing the thermogravimetric curve to obtain a differential weight loss curve;
(4) calculating the similarity of differential weight loss curves of a plurality of heated cigarette formulas and a standard formula;
(5) evaluation of multiple heated cigarette formulations.
2. The method of claim 1, wherein step (1) each formulation sample has a mass of not less than 5 g; before thermogravimetric experiment, the sample was equilibrated in an environment with a temperature of (22 + -1) ° C and a relative humidity of (60 + -2)% for 48 hours.
3. The method of claim 1, wherein the thermogravimetric experiment of step (2) comprises the steps of: weighing a certain mass of the formula sample, placing the formula sample in a crucible, and performing a temperature rise procedure: the initial temperature is 30 ℃, the heating rate is 10 ℃/min, the termination temperature is 350 ℃, and the test is carried out under the air flow of 50 mL/min; the sensitivity of the balance is not lower than 0.1 mu g, and the resolution of the curve is not lower than 5000 ten thousand resolution points.
4. The method according to claim 1, wherein the step (3) of processing the thermogravimetric curve to obtain a differential weight loss curve comprises the steps of: and monitoring the mass change of the formula sample in the pyrolysis process in real time by using a thermogravimetric analyzer, and deriving the weight data with respect to time according to a time-weight relationship diagram to obtain a differential weight loss curve.
5. The method according to claim 1, wherein the step (4) of calculating the degree of similarity of the differential weight loss curve of the heated cigarette formulation to the standard formulation comprises the steps of: and reducing the dimension of the differential weight loss curve, selecting several main components with the highest contribution rate and the accumulated contribution rate not less than 90 percent according to the contribution rate of each component after dimension reduction, and calculating the Mahalanobis distance between the heated cigarette formula and the standard formula.
6. The method according to claim 5, wherein the step of performing a dimension reduction on the differential weight loss curve comprises: will heat the rollThe total number m of the smoke formula samples and the standard formula samples, and a weight loss data matrix X (m X n) of a differential weight loss curve data dimension n are decomposed into the following forms: x is TPT(ii) a Wherein T (m × n) is a score matrix, and P (m × n) is called a load matrix; and (3) selecting a matrix T (m multiplied by k) consisting of k principal component score vectors with the highest contribution rate and the accumulated contribution rate not less than 90% to replace a differential weightlessness data matrix X, namely the matrix after dimensionality reduction.
7. The method of claim 6, wherein the step of calculating the mahalanobis distance of the heated cigarette formulation from the standard formulation comprises: calculating the covariance S of the multi-vector of the matrix T (m × k) after dimension reduction according to a formula
Calculating the mahalanobis distance between the formula of the heated cigarette and the standard formula; wherein t isi,tjRespectively are main component data after the dimensionality reduction of a standard formula and the heated cigarette formula.
8. The method of claim 7, wherein the step (5) of evaluating the heated cigarette formulation comprises the steps of: the smaller the mahalanobis distance, the less difference between the selected heated cigarette formulation and the standard formulation sample.
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| CN114778374A (en) * | 2022-05-05 | 2022-07-22 | 江苏中烟工业有限责任公司 | Tobacco leaf classification method and device, electronic equipment and storage medium |
| CN116148004A (en) * | 2022-11-29 | 2023-05-23 | 江苏中烟工业有限责任公司 | Method for evaluating consistency of axial distribution of formula tobacco shreds in cigarette and application |
| CN116148004B (en) * | 2022-11-29 | 2024-03-26 | 江苏中烟工业有限责任公司 | Method for evaluating consistency of axial distribution of formula tobacco shreds in cigarette and application |
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