CN101393182B - Method for measuring flavor quality of tobacco and tobacco products - Google Patents

Abstract

The invention discloses a method for measuring the aroma quality of tobacco and its products. The method selects all or part of the basic aroma substances as representative characteristic substances through the production route of the aroma substances and the degradation rule of the precursor substances; Then, use simultaneous distillation extraction-gas chromatography/mass spectrometry to measure and analyze the aroma components of tobacco leaves; then set the response factor of the detected substances to the instrument as 1, and directly use the data obtained by the instrument to calculate the sample The KR value of the calculation factor can intuitively characterize the quality of the sample fragrance. This method provides a convenient and effective determination method for tobacco quality control.

Description

A method for measuring the aroma quality of tobacco and its products

technical field

The invention relates to a method for measuring tobacco quality. In particular, it relates to a method for characterizing and assisting in identifying the aroma quality of tobacco leaves and smoke starting from the key aroma components of tobacco leaves.

Background technique

Since the 1930s, tobacco workers at home and abroad have devoted themselves to the analysis and research of tobacco chemical components, trying to infer the quality of tobacco from several chemical components of tobacco. In 1936, the German tobacco chemist Bruckner classified the components of tobacco leaves according to the taste, and proposed the Bruckner quality index, which is quite consistent with the evaluation of the smoke of many tobacco leaf products. In 1948, C.Pyriki simplified Brückner's calculation formula and proposed the Pyriki quality index. Soviet tobacco chemist Shi Muke proposed in 1953 that the ratio of soluble sugar to protein content was used as the quality index of oriental tobacco and flue-cured tobacco taste. In 1951, J.M. Moseley used the ratio of nicotine to the ammonia equivalent of total volatile bases as an index to measure the quality of Burley tobacco. The larger the ratio, the better the quality of the tobacco. This ratio has a lower sugar content. The assessment of the quality of air-cured tobacco has certain reference significance. In addition, indicators that characterize the quality of tobacco leaves include "sugar-nitrogen ratio", "sugar-nicotine ratio", "ratio", "total particle-phase nicotine ratio" or "tar-nicotine ratio" in smoke, etc. Dr. Zuo Tianjue, a Chinese-American, and Academician Zhu Zunquan of the Chinese Academy of Engineering also proposed indicators for evaluating high-quality flue-cured tobacco and burley tobacco from the taste quality. The above values play a certain role in the evaluation of tobacco quality. However, practice shows that due to the limitations of analytical techniques, these indicators are generally relatively broad and vague, and these values are still difficult to accurately and objectively describe the flavor quality of tobacco and its products.

With the continuous development of analytical technology and the continuous deepening of tobacco research, it has been proven that tobacco contains thousands of aroma components. These substances undergo a series of intricate reactions in the process of tobacco smoking, such as cracking, synthesis , dry distillation, etc., have an extremely important impact on the aroma quality of cigarette smoke. At the same time, the entire process of tobacco growth, modulation and processing is also the process of production, accumulation, and demise of tobacco aroma substances. The key aroma substances of tobacco The increase or decrease is closely related to the change of its fragrance quality. Therefore, how to characterize and evaluate the aroma quality of tobacco and its products through the change of aroma components has become a hot and difficult research topic for domestic and foreign tobacco scientists. In the prior art, there is no comparatively perfect measuring method.

Contents of the invention

The object of the present invention is to aim at the deficiencies of the prior art, and provide a method for measuring the flavor quality of tobacco and its products with intuitive data display, convenient operation and good reliability.

The purpose of the present invention is achieved through the following technical solutions.

The invention provides a method for measuring the aroma quality of tobacco and its products. The method adopts the following steps:

1. Select all or part of the basic aroma substances as representative characteristic substances through the production pathway of aroma substances and the degradation law of precursor substances;

2. Determination and analysis of aroma components in tobacco leaves by simultaneous distillation extraction-gas chromatography/mass spectrometry;

3. Set the response factor of the detected substances to the instrument as 1, and directly use the data obtained by the instrument to calculate the calculation factor KR value of the sample, which can intuitively characterize the quality of the sample fragrance.

Wherein, the representative characteristic substances are dihydroactinolactone, total macrostigmatrienone, phenylacetaldehyde, solanone or/and 2,3'-bipyridine.

Compared with the prior art, the present invention has the following beneficial effects:

1. Through in-depth and systematic research, important progress has been made in identifying the flavor quality of tobacco and its products, revealing that there is a positive correlation between the KR value of tobacco and its products and its sensory quality, and cigarettes with high sensory quality scores have a higher KR value. is also correspondingly higher;

2. Through the established mathematical processing of the analysis and testing results, the data are comparable;

3. Set the response factor of the detected substances to the instrument as 1, and directly apply the data obtained by the instrument, which effectively simplifies the calculation process;

4. Obtain the index value through mathematical calculation, and use the magnitude of the value to characterize the aroma quality of tobacco and its products, which provides a convenient and effective measurement method for the production, processing and quality maintenance and quality control of tobacco products.

Description of drawings

Figure 1 is a total ion chromatogram of the aroma components of brand A cigarette shredded tobacco;

Figure 2 is the total ion chromatogram of the aroma components of brand B cigarette shredded tobacco;

Fig. 3 is the total ion chromatogram of aroma components in shredded tobacco of brand C cigarette;

Fig. 4 is a total ion chromatogram of aroma components in brand D cigarette shredded tobacco;

Figure 5 is the total ion chromatogram of aroma components in B2F tobacco leaves;

Figure 6 is a total ion chromatogram of aroma components in C3F tobacco leaves;

Fig. 7 is a total ion chromatogram of aroma components in X3F tobacco leaves.

Detailed ways

Through the specific examples and typical application examples given below, the present invention can be further clearly understood. But they are not limitations to the protection scope of the present invention.

Example 1

——Sample processing process

After roasting the shredded tobacco at (40±1)°C for 4 hours, crush it with a pulverizer, pass through a 40-mesh sieve, and balance the obtained tobacco powder in a balance box at a temperature of 22°C and a humidity of 60% for 24 hours. 25.0 g of tobacco powder samples were put into a simultaneous distillation and extraction device, and dichloromethane was used as a solvent to continuously and dynamically extract tobacco shreds for 2 hours. After the obtained extract was dried over anhydrous sodium sulfate, it was concentrated to 1.0 mL in a rotary evaporator. Add 50 μl, 0.1mol/L benzyl acetate in absolute ethanol, shake well, and analyze it with Agilent6890N/5973N GC/MS analyzer.

Instruments and experimental conditions used:

Reagents: dichloromethane (AR, Xilong Chemical), anhydrous sodium sulfate (AR, Tianjin Kemiou Company), absolute ethanol (chromatographically pure, Dima Company), benzyl acetate (chromatographically pure, Bailingwei Company) ; Instruments: 6890N/5973N GC/MS coupled instrument (Agilent, USA); rotary evaporator (Büchi, Switzerland); PB602-S electronic balance (sensitivity 0.01g, METTLER TOLEDO, Switzerland); simultaneous distillation extraction device (self-made );

8℃/min260℃(15min)；GC/MS analysis conditions: chromatographic column: HP-5MS (30m×0.25mm×0.25μm) capillary column; inlet temperature: 240°C; carrier gas: He, 1mL/min; temperature program: 50°C ( 1min) 8℃/min160℃(2min)

8℃/min260℃(15min);

Injection volume: 2μL, split ratio: 25:1; transfer line temperature: 280°C; ionization mode: EI, ionization energy: 70eV; ion source temperature: 230°C; quadrupole temperature: 160°C; mass range 35-455aum. , using NIST98, Wiley275 spectral library search qualitative.

Example 2

- Calculation of compound content

Calculate the relative content of each substance by formula 1:

$\mathrm{<span\; class="notranslate">\; Ce</span>}<span\; class="notranslate">\; =</span>\mathrm{<span\; class="notranslate">\; \&beta;</span>}<span\; class="notranslate">\; \&times;</span>\frac{\mathrm{<span\; class="notranslate">\; Cr</span>}<span\; class="notranslate">\; \&times;</span>\mathrm{<span\; class="notranslate">\; At</span>}}{\mathrm{<span\; class="notranslate">\; Ar</span>}}<span\; class="notranslate">\; -</span><span\; class="notranslate">\; -</span><span\; class="notranslate">\; -</span><span\; class="notranslate">\; (</span>\mathrm{<span\; class="notranslate">\; 1</span>}<span\; class="notranslate">\; )</span>$

In the formula, Ce—the relative correction content of the target component; β—the correction coefficient, the value is 7.2; Cr—the content of the internal standard; At—the peak area of the target component; Ar—the peak area of the internal standard.

Example 3

——Compilation of KR index

Bring the value calculated by formula 1 into formula 2, and the obtained value is the KR value

KR value = product of positive correlation factors / product of negative correlation factors (2)

Positively correlated factors include: 3-hydroxy-2-butanone, hexanal, bread ketone, furfural, furfuryl alcohol, 2-cyclopentene-1,4-dione, 1-(2-furyl)-ethanone, butane Lactone, Benzaldehyde, 5-Methylfurfural, 6-Methyl-5-Hepten-2-one, Benzyl Alcohol, Linalool, Phenylethyl Ethanol, 2,6-Nadienal, Zanal, 2 -Methoxy-4-vinylphenol, BETA-Damascone, BETA-Dihydrodamascone, Geranylacetone, BETA-Ionone, Dihydroactinolactone, Macrostigmatrienone A, Macrobean 29 substances including trienone B, macrostigmatrienone C, macrostigmatrienone D, 3-oxo-ALPHA-ionol, methyl myristate, and naringone.

Negative correlators include: pyridine, 3-methyl-2-butenal, phenol, phenylacetaldehyde, 2-methylphenol, 2-methoxy-phenol, indole, solanone, dehydronornicotine Alkali, 2,3'-bipyridine, cembratrienediol and other 11 substances.

Example 4

—— Calculation process of KR value

According to the origin of aroma components and their impact on cigarette quality, the aroma substances are distinguished. The 40 substances selected from the analysis results are used as the basic substances of the factor set. By selecting the appropriate factors from the basic substances and using the formula (2) Carry out corresponding mathematical calculations to obtain corresponding KR values, so the calculation expressions of KR values for different types of samples may be different, but if the types of samples are the same, then the calculation expressions of their KR values must be the same of. Under normal circumstances, the positive correlation factors dihydroactinolactone, the total amount of macrostigmatrienone and the negative correlation factors phenylacetaldehyde, solanone, 2,3'-bipyridine are brought into formula 2 for calculation to obtain the KR value.

Application Example 1

Choose four brand cigarettes (* sample codes are respectively A, B, C, D) that price category, sensory quality difference is relatively big, measure according to the method of the present invention, the results are shown in Table 1 and Fig. 1～4, are judged and smoked According to the regulations of "GB5606.4-2005 Cigarette Sensory Technical Requirements", the expert panel evaluates the sensory quality of cigarettes, and the evaluation results are shown in Table 2.

Table 1. Aroma components and KR values of shredded tobacco of different brands of cigarettes

Table 2 Smoking results of sensory quality evaluation of cigarettes

The experimental data in Table 2 clearly shows that there is a positive correlation between the KR value of cigarettes and their sensory quality, and cigarettes with high sensory quality scores have correspondingly higher KR values.

Application Example 2

——Determination of tobacco leaves of different grades (*sample codes are C3F, X3F, B2F)

Tobacco leaves of different grades were selected and cut into shreds, and processed according to the content of the invention. The analysis and processing results are shown in Table 3 and Figures 5-7. The smoke evaluation expert group evaluated the richness of smoke, pleasantness, transparency, aroma quality, aroma quality, Evaluate the clumping properties, lingering properties, miscellaneous gas, stimulation, aftertaste and other aspects, and the evaluation results are shown in Table 4.

Table 3. Analysis results and KR values of aroma components in different grades of tobacco leaves

Table 4. Tobacco leaf sensory quality evaluation results and KR value

It can also be seen from Table 4 that the KR value of tobacco leaves is positively correlated with sensory quality, and the KR value of better quality C3F tobacco leaves is relatively higher than that of other grades of tobacco leaves.

Claims (2)

1. one grow tobacco and the assay method of goods fragrance quality, it is characterized in that: this method adopts following steps:

(1) by the generation approach of fragrance matter and the degradation rule of precursor substance, from basic fragrance matter, select all or part of material as representative property material, described basic fragrance matter is 3-hydroxyl-2-butanone, pyridine, 3-methyl-2-butene aldehyde, hexanal, bread ketone, furfural, furfuryl alcohol, 2-cyclopentene-1, the 4-diketone, 1-(2-furyl)-ethyl ketone, butyrolactone, benzaldehyde, 5 methyl furfural, phenol, 6-methyl-5-hepten-2-one, phenmethylol, phenylacetaldehyde, the 2-methylphenol, 2-methoxyl-phenol, linalool, phenylethyl alcohol, 2,6-nonadienal KURA flower aldehyde, indoles, 2-methoxyl-4-vinylphenol, solanone, the BETA-damascenone, the BETA-damascone, the dehydrogenation nornicotine, geranyl acetone, the BETA-irisone, 2,3 '-dipyridine, dihydroactinidiolide, Megastigmatrienone A, Megastigmatrienone B, Megastigmatrienone C, Megastigmatrienone D, 3-oxo-ALPHA-ionol, methyl myristate, grapefruit ketone and Xi Bai three enediols; Wherein, 3-hydroxyl-2-butanone, hexanal, bread ketone, furfural, furfuryl alcohol, 2-cyclopentene-1, the 4-diketone, 1-(2-furyl)-ethyl ketone, butyrolactone, benzaldehyde, 5 methyl furfural, 6-methyl-5-hepten-2-one, phenmethylol, linalool, phenylethyl alcohol, 2,6-nonadienal KURA flower aldehyde, 2-methoxyl-4-vinylphenol, the BETA-damascenone, the BETA-damascone, geranyl acetone, the BETA-irisone, dihydroactinidiolide, Megastigmatrienone A, Megastigmatrienone B, Megastigmatrienone C, Megastigmatrienone D, 3-oxo-ALPHA-ionol, methyl myristate and grapefruit ketone are the positive correlation factor; Pyridine, 3-methyl-2-butene aldehyde, phenol, phenylacetaldehyde, 2-methylphenol, 2-methoxyl-phenol, indoles, solanone, dehydrogenation nornicotine, 2,3 '-dipyridine and Xi Bai three enediols are the negative correlation factor;

(2) adopt while distillation extraction-gas chromatography/mass spectrometry method that property material is carried out determination and analysis: as solvent pipe tobacco to be carried out dynamic extraction 2h continuously with methylene chloride, extract obtained behind anhydrous sodium sulfate drying, in Rotary Evaporators, be concentrated into 1.0mL, add the ethanol solution of the phenylmethyl acetate of 50 μ l, 0.1mol/L, shake up; Adopt the coupling analyser to analyze, its analysis condition is: chromatographic column HP-5MS, capillary column are 30m * 0.25mm * 0.25m; Injector temperature is: 240 ℃; Carrier gas: He, 1mL/min; Temperature programme: 50 ℃ kept 1 minute, improved 8 ℃ by per minute and were warming up to 160 ℃ of maintenances 2 minutes, improved 8 ℃ by per minute again and were warming up to 260 ℃ of maintenances 15 minutes;

(3) material that analyzing and testing is obtained all is set at 1 to the response factor of instrument, and the data computation of directly using instrument and being obtained draws the calculated factor KR value of sample, wherein, and the product of the product of KR value=positive correlation factor/negative correlation factor.

2. assay method according to claim 1, it is characterized in that: described representative property material is dihydroactinidiolide, Megastigmatrienone total amount, phenylacetaldehyde, solanone and 2,3 '-dipyridine, wherein, the positive correlation factor is dihydroactinidiolide and Megastigmatrienone total amount, the negative correlation factor be phenylacetaldehyde, solanone and 2,3 '-dipyridine.

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