CN113567608A - Method for measuring characteristic components of strokes in flavored cut tobacco and absorption rate and equipment evaluation method thereof - Google Patents
Method for measuring characteristic components of strokes in flavored cut tobacco and absorption rate and equipment evaluation method thereof Download PDFInfo
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- CN113567608A CN113567608A CN202110843188.6A CN202110843188A CN113567608A CN 113567608 A CN113567608 A CN 113567608A CN 202110843188 A CN202110843188 A CN 202110843188A CN 113567608 A CN113567608 A CN 113567608A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention belongs to the field of detection and analysis, and particularly relates to a method for determining the content of style characteristic components in flavored cut tobacco, wherein the flavored cut tobacco has a moss flavor and/or a cream flavor, and correspondingly, the style characteristic components are selected from beta-methyl bryosoate and/or benzyl benzoate; the method comprises the following steps: extracting the flavored cut tobacco by using ethyl acetate, and collecting extract liquor; filtering the extract, and collecting filtrate; detecting the filtrate by using a gas chromatography-mass spectrometer to obtain a detection spectrogram; and calculating the style characteristic component content in the flavored cut tobacco according to the detection spectrogram. The invention also relates to a method for measuring the absorptivity of the tobacco shreds to the characteristic components of the flavor in the tobacco shreds and a method for evaluating the performance of tobacco shred flavoring equipment. The method for measuring the content of the characteristic components in the flavored cut tobacco has the advantages of good repeatability, high accuracy and high precision.
Description
Technical Field
The invention belongs to the field of detection and analysis, and particularly relates to a method for determining the content of style characteristic components in flavored cut tobacco, a method for determining the absorptivity of the cut tobacco to style characteristic components in a spice and a method for evaluating the performance of cut tobacco flavoring equipment.
Background
In the actual production of the cigarette industry, the perfuming process comprises two working procedures of tobacco shred perfuming and tobacco shred feeding. At present, an effective detection means is not available for evaluating the style characteristic components in the flavored cut tobacco, for example, an effective monitoring means is not available for the style characteristic components in the flavored cut tobacco with moss flavor style and/or cream flavor style.
Therefore, a method for detecting the content of style characteristic components in flavored cut tobacco is needed.
Disclosure of Invention
One of the purposes of the invention is to provide a method for measuring the content of style characteristic components in flavored cut tobacco, which has good repeatability, high accuracy and high precision; it is a further object of the present invention to provide a method for determining the absorption rate of a characteristic constituent of a tobacco shred in a flavorant; the invention further aims to provide a method for accurately and reliably evaluating the performance of cut tobacco flavoring equipment.
To achieve the above object, a first aspect of the present invention relates to a method for determining the content of a style characteristic ingredient in a flavored cut tobacco, which is a flavored cut tobacco having a moss-like and/or cream-like flavor, correspondingly, the style characteristic ingredient is selected from methyl β -orcinol and/or benzyl benzoate;
the method comprises the following steps:
extracting the flavored cut tobacco by using ethyl acetate, and collecting extract liquor;
filtering the extract, and collecting filtrate;
detecting the filtrate by using a gas chromatography-mass spectrometer to obtain a detection spectrogram;
calculating the content of style characteristic components in the flavored cut tobacco according to the detection spectrogram;
wherein the content of the first and second substances,
the operating conditions of the gas chromatograph include: the chromatographic column is a DB-5MS capillary column; the temperature of the sample inlet is 240-260 ℃ (such as 245 ℃, 250 ℃ and 255 ℃); the temperature rising procedure is as follows: first, the mixture is kept at 50 to 70 ℃ (e.g., 55 ℃, 60 ℃, 65 ℃) for 1 to 5 minutes (e.g., 2 minutes, 3 minutes), heated at a rate of 1 to 3 ℃/minute (e.g., 2 ℃/minute) to 230 to 250 ℃ (e.g., 235 ℃, 240 ℃, 245 ℃), kept at 230 to 250 ℃ (e.g., 235 ℃, 240 ℃, 245 ℃) for 1 to 5 minutes (e.g., 2 minutes, 3 minutes), heated at a rate of 8 to 12 ℃/minute (e.g., 9 ℃/minute, 10 ℃/minute, 11 minutes) to 270 to 290 ℃ (e.g., 275 ℃, 280 ℃, 285 ℃), and kept at 270 to 290 ℃ (e.g., 275 ℃, 280 ℃, 285 ℃) for 3 to 8 minutes (e.g., 4 minutes, 5 minutes, 7 minutes);
the operating conditions of the mass spectrometer include: the ionization source is EI; the ion source temperature is 220 ℃ to 240 ℃ (for example, 225 ℃, 230 ℃, 235 ℃); the quadrupole rods are at a temperature of 140 ℃ to 160 ℃ (e.g., 145 ℃, 150 ℃, 155 ℃).
In some embodiments of the first aspect of the present invention, the ratio of the volume of ethyl acetate to the mass of the flavored cut tobacco is (10-30) mL:1g, e.g., 15mL:1g, 20mL:1g, 25mL:1 g.
In some embodiments of the first aspect of the present invention, a saturated saline solution, preferably a saturated saline solution at normal temperature, is added to the flavored cut tobacco before and/or during the extraction.
In some embodiments of the first aspect of the present invention, the ratio of the volume of the saturated saline solution to the volume of the ethyl acetate is 1 (1 to 4), for example, 1:2, 1: 3.
In some embodiments of the first aspect of the present invention, the extract is subjected to water removal prior to filtration.
In some embodiments of the first aspect of the present invention, the extract is passed through a column of anhydrous sodium sulfate to remove water;
in some embodiments of the first aspect of the present invention, the ratio of the height of the anhydrous sodium sulfate column to the volume of the extract is 1cm (10-30) ml, such as 1cm:15ml, 1cm:20ml, 1cm:25 ml.
In some embodiments of the first aspect of the present invention, the ratio of the diameter to the height of the anhydrous sodium sulfate column is (1-3: 1), such as 1:1, 1.3:1, 1.5:1, 1.8:1, 2:1, 2.2:1, 2.5:1, 2.7:1, 2.9: 1.
In some embodiments of the first aspect of the present invention, the operating conditions of the gas chromatograph further comprise one or more of:
A. the carrier gas is helium;
B. the flow rate of the column is 1-3 mL/min, such as 1.5mL/min, 2mL/min, 2.5 mL/min;
C. adopting a non-shunting mode;
D. the amount of sample is 0.5-3. mu.L, such as 1. mu.L, 1.5. mu.L, 2. mu.L, 2.5. mu.L.
In certain embodiments of the first aspect of the present invention, the GC-MS is Agilent model 7890A/5977C.
In some embodiments of the first aspect of the present invention, the operating conditions of the mass spectrometer further comprise one or more of:
(A) the temperature of the transmission line is 270 ℃ to 290 ℃, such as 275 ℃, 280 ℃ and 285 ℃;
(B) the electron energy is 60-80 eV, such as 65eV, 70eV and 75 eV;
(C) the scan mode is a selective ion scan, with time segments divided according to retention time.
In some embodiments of the first aspect of the present invention, the content of the style characteristic component in the flavored cut tobacco is calculated by an internal standard method according to the detection spectrogram.
In some embodiments of the first aspect of the present invention, the internal standard used in the internal standard method is phenylethyl acetate.
In some embodiments of the first aspect of the present invention, the flavored cut tobacco is flavored cut tobacco having a moss-like and/or mastic-like flavor.
In some embodiments of the first aspect of the present invention, filtration is performed using an organic filtration membrane.
In certain embodiments of the first aspect of the present invention, methyl β -orcinol is a characteristic constituent of the moss-like aroma and benzyl benzoate is a characteristic constituent of the musty-like aroma.
In certain embodiments of the first aspect of the present invention, the mass-to-charge ratio of the counterion of methyl β -orcinol is 136.
In certain embodiments of the first aspect of the present invention, the mass-to-charge ratio of the qualifying ion of methyl β -orcinol is 164 and/or 196.
In certain embodiments of the first aspect of the present invention, the retention time of methyl β -orcinol is from 61 to 62 min.
In certain embodiments of the first aspect of the present invention, the charge to mass ratio of the quantifying ion of benzyl benzoate is 105.
In certain embodiments of the first aspect of the present invention, the charge to mass ratio of the benzylic benzoate counterion is 91 and/or 212.
In some embodiments of the first aspect of the present invention, the retention time of benzyl benzoate is 65 to 66 min.
In some embodiments of the first aspect of the present invention, the internal standard substance is phenethylacetate.
In some embodiments of the first aspect of the present invention, the internal standard substance phenethylacetate has a mass-to-charge ratio of 91 for the qualitative ion.
In some embodiments of the first aspect of the present invention, the internal standard substance phenethylacetate has a retention time of 34-35 min.
The second aspect of the invention relates to a method for determining the absorptivity of a characteristic ingredient of a cut tobacco on a flavor, wherein the flavor has a moss flavor style and/or a cream flavor style, and correspondingly, the characteristic ingredient is selected from methyl beta-orcinol and/or benzyl benzoate;
the method comprises the following steps:
measuring the total amount of style characteristic components in tobacco shreds before flavoring and the total amount of style characteristic components in spices;
measuring the content of the style characteristic components in the flavored cut tobacco according to the method of the first aspect of the invention, and calculating the total amount of the style characteristic components in the flavored cut tobacco;
calculating the absorptivity of the tobacco shreds to the characteristic components of the flavor stroke by adopting the following formula;
the absorptivity of the tobacco shreds to the style characteristic components in the spice is 100% × (the total amount of the style characteristic components in the flavored tobacco shreds-the total amount of the style characteristic components in the flavored tobacco shreds)/the total amount of the style characteristic components in the spice.
In some embodiments of the second aspect of the present invention, the total amount of the style characteristic components in the flavored cut tobacco is calculated by multiplying the style characteristic component content in the flavored cut tobacco by the mass of the flavored cut tobacco.
In some embodiments of the second aspect of the present invention, the total amount of style-specific ingredients in the cut filler before perfuming is determined by:
the content of the style characteristic components in the cut tobacco before flavoring is measured according to the steps in the first aspect of the invention, and the total amount of the style characteristic components in the cut tobacco before flavoring is calculated.
In some embodiments of the second aspect of the present invention, the total amount of the style characteristic components in the cut tobacco before perfuming is calculated by multiplying the content of the style characteristic components in the cut tobacco before perfuming by the mass of the cut tobacco before perfuming.
In some embodiments of the second aspect of the present invention, the step of determining the level of style-specific ingredients in the cut filler prior to perfuming comprises:
extracting cut tobacco before perfuming by adopting ethyl acetate, and collecting extract liquor;
filtering the extract, and collecting filtrate;
detecting the filtrate by using a gas chromatography-mass spectrometer to obtain a detection spectrogram; wherein the operating conditions for gas chromatography and mass spectrometry are as described in the first aspect of the invention;
and calculating the style characteristic component content in the cut tobacco before perfuming according to the detection spectrogram.
In some embodiments of the second aspect of the present invention, the total amount of the style specific ingredients in the fragrance is determined by:
detecting the spice by using a gas chromatography-mass spectrometer to obtain a spectrogram; wherein the operating conditions for gas chromatography and mass spectrometry are as described in the first aspect of the invention;
and calculating the content of the style characteristic components in the spice according to the detection spectrogram, and further calculating the total amount of the style characteristic components in the spice.
In some embodiments of the second aspect of the present invention, the total amount of the flavor characteristic component in the flavor is calculated by multiplying the flavor characteristic component content in the flavor by the flavor quality.
The third aspect of the invention relates to a method for evaluating the performance of cut tobacco flavoring equipment, which comprises the following steps:
perfuming the cut tobacco by adopting cut tobacco perfuming equipment to obtain the perfumed cut tobacco with moss fragrance style and/or cream fragrance style;
determining the level of a style characteristic in a flavoured cut tobacco according to the method of the preceding aspect of the invention, and/or determining the rate of absorption of a style characteristic in a flavoured cut tobacco according to the method of the second aspect of the invention; wherein the style characteristic component is selected from beta-methyl orcinol and/or benzyl benzoate.
In some embodiments of the third aspect of the present invention, the shredded tobacco flavoring apparatus is conventional in the art.
In some embodiments of the third aspect of the present invention, the operating steps of the shredded tobacco flavoring apparatus are well known to those skilled in the art.
In some embodiments of the third aspect of the present invention, the composition and amount of flavor required to obtain a flavored cut tobacco having a moss and/or mastic flavor is known to those skilled in the art.
In some embodiments of the third aspect of the present invention, the performance of the cut tobacco perfuming device includes the quality of the perfuming effect, specifically, the content of style characteristic components in the perfumed cut tobacco and/or the absorption rate of style characteristic components in the cut tobacco to the perfume.
In some embodiments of the present invention, the performance of the cut tobacco perfuming equipment further includes the stability of the perfuming effect, specifically, the content of style characteristics in the perfumed cut tobacco is repeatedly measured, and the relative standard deviation of the repeated measurement is obtained.
In the present invention, unless otherwise specified, among others,
the term "moss flavor" refers to the green and sweet flavor characteristic of tree moss, a cigarette flavor that blends dry fruit and resin flavors, and is well known to those skilled in the art.
The term "stick-flavor" refers to a cigarette style having a sweet-fat characteristic aroma of a balsam, a balsam resin, and is well known to those skilled in the art.
The term "feeding" refers to a process of applying "liquor" to tobacco leaves during the production of cigarettes, which contributes to improving the sensory quality and the chemical composition of the smoke of the tobacco shreds. The "feed liquid" generally comprises seasonings, flavoring agents, humectants, combustion improvers and preservatives.
The invention obtains at least one of the following beneficial effects:
1. the method for measuring the content of the characteristic components in the flavored cut tobacco has the advantages of good repeatability, high accuracy and high precision.
2. The method can accurately measure the absorption rate of the tobacco shreds to the characteristic components of the flavor stroke.
3. The method can accurately and reliably evaluate the performance of the cut tobacco flavoring equipment.
Drawings
In order that the present disclosure may be more readily and clearly understood, reference is now made to the following detailed description of the embodiments of the present disclosure taken in conjunction with the accompanying drawings, in which
FIG. 1 is a selective ion chromatogram of a sample to be tested in example 1 of the present invention;
FIG. 2 is a standard operating curve for methyl beta-orcinol in example 1 of the present invention;
FIG. 3 is a standard working curve for benzyl benzoate according to example 1 of the present invention.
Detailed Description
Embodiments of the present invention will now be described more fully hereinafter with reference to the accompanying examples, in which some, but not all embodiments of the invention are shown. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1Determining the content of characteristic components in flavored tobacco shreds
1. Preparation of a series of standard working solutions:
weighing 20.0g of unflavored casing tobacco shred sample, adding 400ml of ethyl acetate extract, performing ultrasonic extraction for 20min, taking supernatant, passing through an anhydrous sodium sulfate column (filling a 1 cm-high anhydrous sodium sulfate column in a 5ml specification needle cylinder), then filtering with an organic filter membrane, and collecting filtrate as matrix filtrate for later use. Wherein, the feed liquid adopted by the tobacco shred feeding is the common feed liquid in the field, and the feeding operation is carried out according to the conventional operation in the field.
Accurately weighing 10mg of beta-methyl orcinol acid standard substance and 10mg of benzyl benzoate standard substance, accurately measuring the weight of the beta-methyl orcinol acid standard substance and the weight of the benzyl benzoate standard substance to 0.1mg, putting the beta-methyl orcinol acid standard substance and the benzyl benzoate standard substance into a 100mL volumetric flask, carrying out constant volume and dissolving by adopting the matrix filtrate to obtain a mixed standard stock solution containing 100 mu g/mL of beta-methyl orcinol acid and 100 mu g/mL of benzyl benzoate, and storing the mixed standard stock solution in a refrigerator at 4 +/-1 ℃; 6 series of standard working solutions (containing 2. mu.g/ml of phenethylacetate as an internal standard) were prepared from the mixed standard stock solutions, and the concentration of methyl β -orcinol was the same as that of benzyl benzoate in each standard working solution, as shown in Table 1; the concentration range covers the content of the sample which is expected to be detected, and the sample is stored in a refrigerator at 0-4 ℃.
TABLE 1
| Rank of | S1 | S2 | S3 | S4 | S5 | S6 |
| Concentration (μ g/mL) | 0.20 | 0.40 | 1.0 | 2.0 | 4.0 | 10.0 |
2. Pretreatment of flavored cut tobacco:
weighing 1.0g of flavored and casing tobacco shreds with moss flavor style and/or cream flavor style (the tobacco shreds are identical in type and casing treatment in steps 1 and 2), adding 20mL of ethyl acetate extract, adding 10mL of saturated saline solution, performing ultrasonic extraction for 20 minutes, taking supernatant, passing through an anhydrous sodium sulfate column (filling a 1 cm-high anhydrous sodium sulfate column in a 5 mL-specification needle cylinder), filtering with an organic filter membrane, collecting filtrate, adding an internal standard substance phenethyl acetate, and enabling the filtrate to contain 2 mug/mL of an internal standard substance to serve as a sample to be detected.
3. And (3) detection:
the matrix filtrate (added with phenethyl acetate as an internal standard substance with the concentration of 2 mu g/ml before detection), a series of standard working solutions and a sample to be detected are detected by a 7890A/5977C gas chromatography/mass spectrometer (Agilent company in the United states). Wherein, the selective ion chromatogram of the sample to be detected is shown in figure 1.
Operating conditions of gas chromatography: the chromatographic column is a DB-5MS capillary column with the specification of 60m 0.25mm 0.25 mu m; the carrier gas is helium; the column flow rate is 1.5 mL/min; the temperature of a sample inlet is 250 ℃; temperature rising procedure:
a non-shunting mode; the sample injection amount is 1 mu L;
operating conditions of mass spectrum: the temperature of the transmission line is 280 ℃; the ionization source is EI; the ion source temperature is 230 ℃; the temperature of the quadrupole rods is 150 ℃; the electron energy is 70 eV; the scan mode is a selective ion scan, with time segments divided according to retention time.
Beta-orcinol methyl ester is taken as a characteristic component of the moss flavor, benzyl benzoate is taken as a characteristic component of the cream flavor, and retention time, qualitative ions and quantitative ions of the characteristic component are shown in table 2.
TABLE 2
Linear regression analysis was performed using the ratio of the concentrations of methyl β -orcinol (or benzyl benzoate) and the internal standard in the series of standard working solutions as independent variables and the ratio of the peak areas of methyl β -orcinol (or benzyl benzoate) and the internal standard as dependent variables to obtain the standard working curve of methyl β -orcinol (or benzyl benzoate), as shown in fig. 2-3. The mass concentration corresponding to 3-fold signal-to-noise ratio (S/N: 3) was used as the detection limit, and the mass concentration corresponding to 10-fold signal-to-noise ratio (S/N: 10) was used as the quantification limit. The results are shown in Table 3.
TABLE 3
Substituting the peak area ratio of the beta-orcinol methyl ester to the internal standard substance in the sample to be detected and the content of the internal standard substance into a standard working curve of the beta-orcinol methyl ester, and calculating the content of the beta-orcinol methyl ester in the sample to be detected; and substituting the peak area ratio of the benzyl benzoate to the internal standard substance in the sample to be detected and the content of the internal standard substance into a standard working curve of the benzyl benzoate, and calculating the content of the benzyl benzoate in the sample to be detected.
And similarly, calculating the content of the beta-orcinol methyl ester and the content of benzyl benzoate in the matrix filtrate.
And then, respectively calculating the content of the beta-orcinol methyl ester and the content of the benzyl benzoate in the flavored cut tobacco by adopting the following formula. The average value of the two parallel measurement results is taken as the measurement result, the result is accurate to 0.01 mu g/g, and the relative average deviation of the two parallel measurement results is less than 10 percent.
Wherein:
x represents the content of beta-methyl orcinol acid ester (or benzyl benzoate) in the flavored cut tobacco, and the content is microgram/gram;
m represents the mass of the flavored cut tobacco, g;
v represents the total volume of the sample to be detected, ml;
c represents the content of beta-orcinol methyl ester (or benzyl benzoate) in the sample to be detected, and the content is microgram/mL;
C0represents the amount of methyl betaorcinol (or benzyl benzoate) in the matrix filtrate, μ g/mL.
The content of the style characteristic components in the flavored and casing tobacco shred samples with moss flavor style and/or cream flavor style is measured by the method and is measured for 6 times in parallel, and the result is shown in table 4.
TABLE 4
As can be seen from Table 4, the method of the present invention has good repeatability for determining the style characteristic components in tobacco shred samples.
Example 2
To the flavored and flavored shredded tobacco samples having a moss and/or mastic flavor of example 1, three concentration levels of methyl β -orcinol standard of 0.5 μ g/g, 1.0 μ g/g, and 2 μ g/g and three concentration levels of benzyl benzoate standard of 2.0 μ g/g, 4.0 μ g/g, and 8.0 μ g/g, respectively, were added to obtain a plurality of spiked samples.
Adding 20mL of ethyl acetate extract into each sample, adding 10mL of saturated saline solution, performing ultrasonic extraction for 20 minutes, taking supernatant, passing through an anhydrous sodium sulfate column (a 5mL needle cylinder is filled with a 1 cm-high anhydrous sodium sulfate column), filtering with an organic filter membrane, collecting filtrate, adding an internal standard substance phenethyl acetate to enable the filtrate to contain 2 mu g/mL of the internal standard substance, measuring the content of the characteristic component in the sample according to the step 3 in the example 1, and repeating the measurement for three times. The standard recovery rates and relative standard deviations were calculated from the average values of the characteristic component contents of the cut tobacco in table 4 of example 1 and the measured characteristic component contents of the standard samples, and the results are shown in table 5.
TABLE 5
As can be seen from Table 5, the standard recovery rate of the style characteristic components in the cut tobacco sample measured by the method is between 89% and 99.3%, which shows that the accuracy of the measurement by the method is high; and the repeatability of the method is good.
Example 3
Before transformation: the perfuming operation was carried out with a tobacco perfuming machine of the related art shown in figures 1 to 3 of the document CN 112335926A;
after transformation: the perfuming operation was carried out with a tobacco perfuming machine as shown in figures 4 to 7 of document CN 112335926A;
the tobacco flavoring machine before and after modification is adopted to flavor the same batch of the charging cut tobacco, and the adding amount and the composition of the spice are the same:
firstly, collecting the flavored and casing cut tobacco at the discharge end every 5 minutes from starting the machine, taking 200g of each sample, and sealing and storing;
secondly, starting a machine, collecting the flavoring and casing cut tobacco at the discharge end at a time point which is half of the total time consumed by the flavoring process, repeatedly sampling for multiple times, wherein each sample is 200g, and sealing and storing;
the amounts of flavor-characterizing ingredients in each of the flavored cut filler were measured according to the method of example 1 and the relative standard deviation RSD was calculated, and the results are shown in tables 6 to 7.
The absorbance of the flavored tobacco for the flavor profile was calculated according to the following formula.
Wherein the content of the first and second substances,
y represents the absorption (%) of the flavor profile ingredient by the added tobacco;
M1represents the total weight (g) of flavored cut filler;
W1shows the content (mu g/g) of style characteristic components in the flavored and casing cut tobacco;
M0shows the total weight (g) of cut filler before flavoring;
W0shows the content (mu g/g) of style characteristic components in the cut filler before flavoring;
s represents the total weight (g) of added perfume;
WSthe content of the flavor characterizing component (. mu.g/g) in the added perfume was shown.
Wherein the content of the style characteristic component in the cut filler before flavoring is determined by the method of example 1; the content of the style specific ingredients in the added perfume was measured using the instrument and conditions in step 3 of example 1 and calculated using an external standard method.
The absorption rates of the charged cut tobacco to the style characteristic components measured at each time point in the first item are averaged, and the absorption rates of the charged cut tobacco to the style characteristic components measured for a plurality of times in the second item are averaged, and the results are shown in table 8.
TABLE 6 Style characteristic ingredient content in flavored cut filler collected every 5 minutes
TABLE 7 Style characteristic component content in flavored casing tobacco collected at a time point half the total time taken for the flavoring process
As can be seen from tables 6 to 7, compared with the tobacco flavoring machine before modification, the tobacco flavoring machine after modification has higher content of style characteristic components and lower RSD, which indicates that the tobacco flavoring machine after modification has better effect, more uniform flavoring, higher stability and more reliable process, which is consistent with the technical effect claimed in the document CN112335926A, therefore, the method of the invention can accurately and reliably measure the content of the style characteristic components in the flavored tobacco.
TABLE 8 average value of absorption rate of charged tobacco shreds to style characteristics
As can be seen from table 8, compared with the tobacco flavoring machine before modification, the modified tobacco flavoring machine has the advantages that the absorption rate of the flavor characteristic components by the cut tobacco filler is obviously improved, and the technical effect is consistent with that claimed in the document CN112335926A, which shows that the method of the present invention can accurately and reliably determine the content of the flavor characteristic components in the cut tobacco filler.
Tables 6-8 also illustrate that the method of the present invention is well suited to evaluate the performance of tobacco flavoring equipment.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A method for determining the content of style characteristic components in flavored cut tobacco, wherein the flavored cut tobacco has a moss flavor and/or a cream flavor, and correspondingly, the style characteristic components are selected from methyl beta-orcinol and/or benzyl benzoate;
the method comprises the following steps:
extracting the flavored cut tobacco by using ethyl acetate, and collecting extract liquor;
filtering the extract, and collecting filtrate;
detecting the filtrate by using a gas chromatography-mass spectrometer to obtain a detection spectrogram;
calculating the content of style characteristic components in the flavored cut tobacco according to the detection spectrogram;
wherein the content of the first and second substances,
the operating conditions of the gas chromatograph include: the chromatographic column is a DB-5MS capillary column; the temperature of a sample inlet is 240-260 ℃; the temperature rising procedure is as follows: keeping the temperature at 50-70 ℃ for 1-5 minutes, heating to 230-250 ℃ at the speed of 1-3 ℃/minute, keeping the temperature at 230-250 ℃ for 1-5 minutes, heating to 270-290 ℃ at the speed of 8-12 ℃/minute, and keeping the temperature at 270-290 ℃ for 3-8 minutes;
the operating conditions of the mass spectrometer include: the ionization source is EI; the temperature of the ion source is 220-240 ℃; the temperature of the quadrupole rod is 140-160 ℃.
2. The method according to claim 1, wherein the volume of ethyl acetate to mass of flavored cut tobacco is (10-30) mL:1 g.
3. A method according to claim 1 or 2, wherein saturated salt water is added to the flavored cut tobacco before and/or during extraction;
preferably, the ratio of the volume of the saturated saline solution to the volume of the ethyl acetate is 1 (1-4).
4. The process according to any one of claims 1 to 3, wherein, prior to filtration, the extract is freed from water;
preferably, the extract is passed through a column of anhydrous sodium sulfate to remove water;
more preferably, the ratio of the height of the anhydrous sodium sulfate column to the volume of the extraction liquid is 1cm (10-30) ml.
5. The method of any one of claims 1 to 4, wherein the operating conditions of the gas chromatograph further comprise one or more of:
A. the carrier gas is helium;
B. the flow rate of the column is 1-3 mL/min;
C. adopting a non-shunting mode;
D. the sample injection amount is 0.5-3 μ L.
6. The method of any one of claims 1 to 5, wherein the operating conditions of mass spectrometry further comprise one or more of:
(A) the temperature of the transmission line is 270-290 ℃;
(B) the electron energy is 60-80 ev;
(C) the scan mode is a selective ion scan, with time segments divided according to retention time.
7. The method according to any one of claims 1 to 6, wherein the style characteristic component content in the flavored cut tobacco is calculated by an internal standard method according to a detection spectrogram;
preferably, the internal standard method adopts an internal standard substance of phenethyl acetate.
8. The method according to any one of claims 1 to 7, wherein the cut filler is a cut filler having a moss-like and/or cream-like flavor;
preferably, filtration is carried out using an organic filter membrane.
9. A method of determining the absorption rate of a cut tobacco for a flavor having a moss and/or mastic note, the flavor notes being selected from methyl β -orcinol and/or benzyl benzoate;
the method comprises the following steps:
measuring the total amount of style characteristic components in tobacco shreds before flavoring and the total amount of style characteristic components in spices;
measuring the content of the style characteristic components in the flavored cut tobacco according to the method of any one of claims 1 to 8, and calculating the total amount of the style characteristic components in the flavored cut tobacco;
calculating the absorptivity of the tobacco shreds to the characteristic components of the flavor stroke by adopting the following formula;
the absorptivity of the tobacco shreds to the style characteristic components in the spice is 100% × (the total amount of the style characteristic components in the flavored tobacco shreds-the total amount of the style characteristic components in the flavored tobacco shreds)/the total amount of the style characteristic components in the spice;
preferably, the total amount of style specific ingredients in the cut tobacco before perfuming is determined by the following steps:
measuring the content of the style characteristic components in the cut tobacco before perfuming according to the steps of any one of claims 1 to 8, and calculating the total amount of the style characteristic components in the cut tobacco before perfuming;
preferably, the total amount of style specific ingredients in the fragrance is determined by:
detecting the spice by using a gas chromatography-mass spectrometer to obtain a spectrogram; wherein the operating conditions for gas chromatography and mass spectrometry are as described in claims 1 to 8;
and calculating the content of the style characteristic components in the spice according to the detection spectrogram, and further calculating the total amount of the style characteristic components in the spice.
10. A method for evaluating the performance of cut tobacco perfuming equipment comprises the following steps:
perfuming the cut tobacco by adopting cut tobacco perfuming equipment to obtain the perfumed cut tobacco with moss fragrance style and/or cream fragrance style;
determining the level of a style characteristic in a flavoured cut tobacco according to the method of any of claims 1 to 8, and/or determining the rate of absorption of a style characteristic in a flavoured cut tobacco according to the method of claim 9; wherein the style characteristic component is selected from beta-methyl orcinol and/or benzyl benzoate.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106706794A (en) * | 2017-01-04 | 2017-05-24 | 江苏中烟工业有限责任公司 | Quantitative analysis method of main moss fragrance characteristics flavor component in fine cigarette mainstream smoke |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106706794A (en) * | 2017-01-04 | 2017-05-24 | 江苏中烟工业有限责任公司 | Quantitative analysis method of main moss fragrance characteristics flavor component in fine cigarette mainstream smoke |
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| VALLARINO, JOSE G. 等: "Acquisition of volatile compounds by gas chromatography-mass spectrometry (GC-MS)" * |
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