CN113049436A - Method for rapidly analyzing consistency of tobacco flavor and fragrance and application thereof - Google Patents
Method for rapidly analyzing consistency of tobacco flavor and fragrance and application thereof Download PDFInfo
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Abstract
本发明提供了一种烟用香精香料品质控制方法。所述方法包括以下步骤：将烟用香精香料采用热重分析法进行检测，比较受热过程中待测样品重量变化曲线与标准样品重量变化曲线的一致性，判别品质是否一致。该方法操作便捷，样品需求量少，且无需对样品进行任何前处理，通过失重曲线能够灵敏捕捉到样品的差异性信息，为烟用香精香料的一致性判定提供了一种快速准确的分析方法。该方法可以与常规的嗅香、气相色谱对比的补充，形成一种新的品质控制方法，克服现有的方法无法检测样品中微量的水或高沸点成分的偏差，使烟用香精香料品质控制更准确。同时为卷烟生产质量控制提供了良好的技术保障和数据支持。
The invention provides a quality control method of flavor and fragrance for tobacco. The method includes the following steps: detecting tobacco flavors and fragrances by thermogravimetric analysis, comparing the consistency between the weight change curve of the sample to be tested and the standard sample weight change curve during the heating process, and judging whether the quality is consistent. The method is convenient to operate, requires less sample, and does not require any pretreatment of the sample. The difference information of the sample can be sensitively captured through the weight loss curve, which provides a fast and accurate analysis method for the consistency judgment of tobacco flavors and fragrances. . The method can be supplemented with conventional olfactory aroma and gas chromatography to form a new quality control method, overcome the deviation of the existing methods that cannot detect trace amounts of water or high-boiling point components in the sample, and enable the quality control of tobacco flavors and fragrances. more acurrate. At the same time, it provides a good technical guarantee and data support for the quality control of cigarette production.
Description
Technical Field
The invention belongs to the field of analysis of tobacco raw materials, and particularly relates to a method for rapidly analyzing consistency of tobacco flavors and fragrances and application thereof.
Background
Quality evaluation needs to be carried out on different batches of essences and flavors in the cigarette production process, and the existing evaluation method mainly adopts the modes of refraction density, chromatic aberration, gas chromatography-mass spectrometry spectrogram comparison, artificial smell and the like for judgment. Although these methods reflect the quality of the sample in most cases, when the water content of the sample is high or some high boiling point components (such as sugars) are incorporated, these methods are difficult to identify, so that some unqualified samples are judged to be qualified, thereby greatly affecting the quality stability of the final product.
Therefore, the method for rapidly analyzing the consistency of the tobacco flavor and fragrance is provided on the basis of the prior art, can be used as a supplement for evaluating the quality of the tobacco flavor and fragrance, and has important significance for the production of cigarettes.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for rapidly analyzing the consistency of tobacco flavors and fragrances. The method can be used for rapidly detecting whether the problem that the moisture content is higher or high-boiling-point components are doped in the tobacco flavor and fragrance.
The invention also aims to provide a quality control method of the tobacco flavor and fragrance.
The above purpose of the invention is realized by the following technical scheme:
a method for rapidly analyzing consistency of tobacco flavors and fragrances comprises the following steps:
carrying out thermal weight loss analysis on the tobacco essence and spice samples, and comparing the consistency of the weight change curve of the sample to be detected and the weight change curve of the standard sample in the heating process; when the weight change curve of the sample to be detected is consistent with the weight change curve of the standard sample, judging that the quality is the same; and when the weight change curve of the sample to be detected is inconsistent with the weight change curve of the standard sample, judging that the quality is different.
In the invention, when the weight change curve of the sample to be detected and the weight change curve of the standard sample can be basically overlapped in the whole detection range to be judged to be consistent, and when the weight change curve of the sample to be detected and the weight change curve of the standard sample are only partially overlapped in the whole detection range and the rest part is deviated, or the weight change curves are deviated in the whole stage, the weight change curves are judged to be inconsistent.
Preferably, the thermogravimetric analysis conditions are: sample amount: 10-80 mg; purging gas: n is a radical of2Or compressed air; temperature rising procedure: heating to 150-600 ℃ at a rate of 1-50 ℃/min.
Preferably, the temperature-raising program raises the temperature to 400 ℃ at a rate of 10 ℃/min.
Preferably, the conditions of thermogravimetric analysis further comprise, purge gas flow rate: 90mL/min, equilibrium air flow: 10 mL/min.
Preferably, for each sample to be tested, two parallel samples are selected to be tested respectively.
A quality control method for tobacco essence and flavor comprises performing smell comparison, gas chromatography spectrogram comparison and thermal weight loss analysis comparison on a sample to be detected and a standard sample in sequence; when all the contrasts are consistent, judging that the sample to be detected is consistent with the standard sample; and when any comparison is inconsistent, terminating the comparison and judging that the sample to be detected is inconsistent with the standard sample.
For the smell comparison, whether the smell is consistent or not is judged by judging whether the result scores of the experts are the same or not.
And for the gas chromatographic spectrogram, when corresponding time corresponds to peak substances, the peak substances are judged to be consistent when the peak intensities are the same, and the peak substances are judged to be inconsistent in other conditions.
For the thermogravimetric analysis, when the weight change curve of the sample to be detected and the weight change curve of the standard sample can be basically overlapped in the whole detection range to be judged to be consistent, and when the weight change curve of the sample to be detected and the weight change curve of the standard sample are only partially overlapped in the whole detection range and the rest part is deviated, or the weight change curves are deviated in the whole stage, the weight change curves are judged to be inconsistent.
Preferably, the conditions for the thermogravimetric analysis comparison are sample amount: 10-80 mg; purging gas: n is a radical of2Or compressed air; temperature rising procedure: heating to 150-600 ℃ at a rate of 1-50 ℃/min.
Preferably, the temperature-raising program raises the temperature to 400 ℃ at a rate of 10 ℃/min.
Preferably, the conditions of thermogravimetric analysis further comprise, purge gas flow rate: 90mL/min, equilibrium air flow: 10 mL/min.
Preferably, for each sample to be tested, two parallel samples are selected to be tested respectively.
The method is suitable for common tobacco flavors and fragrances, which are either plant-derived or synthetic. The plant source includes plant extract, tincture, extract, etc. More preferably a plant extract flavour, for example apple flavour.
Compared with the prior art, the invention has the following beneficial technical effects:
the invention provides a method for rapidly analyzing consistency of tobacco essence and flavor, and particularly relates to a method for analyzing whether component differences exist in tobacco essence and flavor of different batches by using a thermogravimetric analysis method. The method can be supplemented with conventional smelling and gas chromatography, forms a new quality control method, overcomes the defect that the existing method can not detect the deviation of trace water or high boiling point components in a sample, and ensures that the quality control of the tobacco essence perfume is more accurate. Meanwhile, good technical guarantee and data support are provided for the cigarette production quality control.
Drawings
FIG. 1 is a gas mass spectrum of a sample of example 1;
FIG. 2 is a thermogravimetric plot of the sample of example 1;
FIG. 3 is a gas mass spectrum of the sample of example 2;
FIG. 4 is a thermogravimetric plot of the sample of example 2.
Detailed Description
Unless otherwise specified, the raw materials, reagents and solvents used in the present invention were all purchased commercially without any treatment. The present invention is described in further detail with reference to the following examples, but the embodiments of the present invention are not limited to the examples, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention. In the present specification, "part" and "%" represent "part by mass" and "% by mass", respectively, unless otherwise specified.
In the embodiment, the tobacco essence is apple essence.
Example 1
Taking a tobacco essence sample, uniformly dividing the tobacco essence sample into a part a and a part b, adding 5% of water into the part a, and uniformly mixing; and then sampling the samples a and b respectively for odor comparison, wherein the fragrance concentration and the style are basically consistent, and the samples a and b are judged to be consistent.
Respectively sampling samples a and b for gas chromatographic analysis:
gas chromatography conditions: sample inlet temperature: 250 ℃, carrier gas: high purity He (99.999%); sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 100: 1; he flow rate: 1.00 mL/min; a chromatographic column: DB-5MS60m 0.25mm 0.25 μm; temperature rising procedure: keeping at 50 deg.C for 1 min; then heating to 200 ℃ at a speed of 3 ℃/min, and keeping for 0 min; then heating to 280 ℃ at a speed of 10 ℃/min and keeping for 15 min; solvent retardation: 2.6 min. Transmission line temperature: 230 ℃; an ionization mode: EI; ionization energy: 70 ev; scanning range: 35.0 to 450.0 amu.
The results are shown in FIG. 1. From the gas chromatogram, it was found that the two were not different and were judged to be identical.
Samples a and b were taken for thermogravimetric analysis:
and taking 80mg of the sample a and the sample b, placing the samples in a thermogravimetric analyzer, and performing thermogravimetric analysis under the following conditions: purging gas: n is a radical of2Or compressed air; the flow rate of the purge gas: 90mL/min, equilibrium air flow: 10 mL/min; temperature rising procedure: the temperature is raised to 400 ℃ at a speed of 10 ℃/min.
After the test, repeated sampling was performed for thermogravimetric analysis test, and the test results are shown in fig. 2.
As can be seen from fig. 2, the thermogravimetric curve of the a-sample to which moisture was added was inconsistent with the b-sample, and thus it was recognized that the a-sample was inconsistent with the b-sample.
Example 2
Taking an essence sample for cigarettes, uniformly dividing the essence sample into two parts, namely c and d, adding 5% invert sugar into the sample c, and uniformly mixing; and then sampling the c sample and the d sample respectively, and comparing smells and smells to judge that the samples are consistent.
And respectively sampling samples c and d for gas chromatographic analysis:
gas chromatography conditions: sample inlet temperature: 250 ℃, carrier gas: high purity He (99.999%); sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 200: 1; he flow rate: 1.00 mL/min; a chromatographic column: DB-5MS60m 0.25mm 0.25 μm; temperature rising procedure: keeping at 50 deg.C for 1 min; then heating to 200 ℃ at a speed of 3 ℃/min, and keeping for 1 min; then heating to 280 ℃ at a speed of 10 ℃/min and keeping for 10 min; solvent retardation: 2.6 min. Transmission line temperature: 230 ℃; an ionization mode: EI; ionization energy: 70 ev; scanning range: 35.0 to 450.0 amu.
The results are shown in FIG. 3. From the gas chromatogram, it was found that the two were not different and were judged to be identical.
And taking 80mg of the sample c and the sample d, placing the samples in a thermogravimetric analyzer, and performing thermogravimetric analysis under the following conditions: purging gas: n is a radical of2Or compressed air; the flow rate of the purge gas: the concentration of the water is 90mL/min,balance gas flow rate: 10 mL/min; temperature rising procedure: the temperature is raised to 400 ℃ at a speed of 10 ℃/min.
After the test, the sample was sampled repeatedly for testing, and the test result is shown in fig. 4.
As can be seen from fig. 4, the thermogravimetric curve of the c-sample to which sugar was added does not agree with the d-sample, and thus it can be recognized that the c-sample does not agree with the d-sample.
Example 3
Taking apple essence, taking 4 different batches from the same manufacturer, and taking the earliest batch as a standard batch (standard batch: 1 month and 1 day in 2019, 3 months and 1 day in 2019, 2 month and 1 day in 2019, 5 months and 1 day in 2019, and 3 month and 1 day in 2019, 7 months and 1 day in 2019). After each batch is purchased, performing smell test, gas chromatography spectrogram test and thermogravimetric analysis test respectively to form records, and comparing each batch with a standard batch. The results are shown in Table 1.
Gas chromatography conditions: sample inlet temperature: 250 ℃, carrier gas: high purity He (99.999%); sample introduction amount: 1 mu L of the solution; the split ratio is as follows: 100: 1; he flow rate: 1.00 mL/min; a chromatographic column: DB-5MS
60m 0.25mm 0.25 μm; temperature rising procedure: keeping at 50 deg.C for 1 min; then heating to 200 ℃ at a speed of 3 ℃/min, and keeping for 0 min; then heating to 280 ℃ at a speed of 10 ℃/min and keeping for 15 min; solvent retardation: 2.6 min. Transmission line temperature: 230 ℃; an ionization mode: EI; ionization energy: 70 ev; scanning range: 35.0 to 450.0 amu.
Thermogravimetric analysis conditions: purging gas: n is a radical of2Or compressed air; the flow rate of the purge gas: 90mL/min, equilibrium air flow: 10 mL/min; temperature rising procedure: the temperature is raised to 400 ℃ at a speed of 10 ℃/min.
TABLE 1
| Batch 1 | Batch 2 | Batch 3 | |
| Smelling incense | Uniformity | Uniformity | Uniformity |
| Gas chromatography | Uniformity | Uniformity | Uniformity |
| Thermogravimetric analysis | Uniformity | Uniformity | Inconsistency |
The quality control method for the essence and the spice increases the comparison of thermogravimetric analysis, and can find the quality difference which is difficult to find in the prior art, so that the quality control is more accurate.
Claims (10)
1. A method for rapidly analyzing the consistency of tobacco flavors and fragrances is characterized by comprising the following steps:
carrying out thermal weight loss analysis on the tobacco essence and spice samples, and comparing the consistency of the weight change curve of the sample to be detected and the weight change curve of the standard sample in the heating process; when the weight change curve of the sample to be detected is consistent with the weight change curve of the standard sample, judging that the quality is the same; and when the weight change curve of the sample to be detected is inconsistent with the weight change curve of the standard sample, judging that the quality is different.
2. The essence spice for tobacco according to claim 1The method for rapidly analyzing consistency is characterized in that the thermogravimetric analysis conditions are as follows: sample amount: 10-80 mg; purging gas: n is a radical of2Or compressed air; temperature rising procedure: heating to 150-600 ℃ at a rate of 1-50 ℃/min.
3. The method for rapidly analyzing the consistency of the tobacco flavors and fragrances according to claim 2, wherein the temperature rise program is used for raising the temperature to 400 ℃ at a speed of 10 ℃/min.
4. The method for rapidly analyzing the consistency of the tobacco flavors and fragrances according to claim 2, wherein the thermogravimetric analysis conditions further comprise the following purge gas flow: 90mL/min, equilibrium air flow: 10 mL/min.
5. The method for rapidly analyzing the consistency of the tobacco flavors and fragrances according to claim 1, wherein two parallel samples are selected for each sample to be tested and are respectively tested.
6. A quality control method for tobacco essence and flavor is characterized by comprising the steps of sequentially carrying out smell comparison, gas chromatography spectrogram comparison and thermal weight loss analysis comparison on a sample to be detected and a standard sample; when all the contrasts are consistent, judging that the sample to be detected is consistent with the standard sample; and when any comparison is inconsistent, terminating the comparison and judging that the sample to be detected is inconsistent with the standard sample.
7. The quality control method of tobacco flavor and fragrance as claimed in claim 6, wherein the conditions of thermogravimetric analysis and comparison are sample amount: 10-80 mg; purging gas: n is a radical of2Or compressed air; temperature rising procedure: heating to 150-600 ℃ at a rate of 1-50 ℃/min.
8. The quality control method of tobacco flavor and fragrance as claimed in claim 7, characterized in that the temperature rise program is to raise the temperature to 400 ℃ at a speed of 10 ℃/min.
9. The quality control method of tobacco flavor and fragrance according to claim 7, characterized in that the thermogravimetric analysis further comprises the following conditions of purge gas flow: 90mL/min, equilibrium air flow: 10 mL/min.
10. The method for controlling the quality of the tobacco flavor and fragrance as claimed in claim 6, wherein for each sample to be tested, two parallel samples are selected for testing respectively.
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| 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 |
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