CN115524418A - Method for quantitatively evaluating replaceability of essence functional action - Google Patents
Method for quantitatively evaluating replaceability of essence functional action Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 27
- 230000009471 action Effects 0.000 title abstract description 4
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 33
- 239000000796 flavoring agent Substances 0.000 claims description 12
- 235000019634 flavors Nutrition 0.000 claims description 12
- 238000011156 evaluation Methods 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 9
- 230000001953 sensory effect Effects 0.000 claims description 9
- 230000037152 sensory function Effects 0.000 claims description 7
- 238000012360 testing method Methods 0.000 claims description 7
- 238000004458 analytical method Methods 0.000 claims description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 5
- 238000009499 grossing Methods 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 4
- 230000000694 effects Effects 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 230000000391 smoking effect Effects 0.000 claims description 3
- 239000007790 solid phase Substances 0.000 claims description 3
- 238000007781 pre-processing Methods 0.000 claims description 2
- 241000208125 Nicotiana Species 0.000 description 4
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 4
- 238000002470 solid-phase micro-extraction Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 238000011208 chromatographic data Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- SJWFXCIHNDVPSH-UHFFFAOYSA-N octan-2-ol Chemical compound CCCCCCC(C)O SJWFXCIHNDVPSH-UHFFFAOYSA-N 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 244000062730 Melissa officinalis Species 0.000 description 1
- 235000010654 Melissa officinalis Nutrition 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- -1 extractum Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000000865 liniment Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
- G01N2030/045—Standards internal
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2203/00—Investigating strength properties of solid materials by application of mechanical stress
- G01N2203/0014—Type of force applied
- G01N2203/0023—Bending
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Abstract
The invention relates to a method for quantitatively evaluating the substitutability of functional action of essence, which can objectively evaluate the consistency degree of the functional action of simulated essence and provide data and method support for the simulated essence to enter a cigarette essence full formula.
Description
Technical Field
The invention belongs to the field of cigarette flavoring, and particularly relates to a method for quantitatively evaluating replaceability of essence functional action.
Background
The essence is an important additive in cigarette production and manufacturing, and is prepared by blending synthetic monomers, essential oil, extractum, balm, extract and other different spices according to a certain proportion. In recent years, the tobacco industry puts forward the known, controllable and replaceable working requirements of tobacco essence, and the imitation preparation of the essence is a research hotspot in the tobacco industry at present.
The problems of complex flavor types, unclear sources, difficult control of the proportion and the like in the essence cause great difficulty in the essence imitation work, and the essence cannot be completely consistent with the imitated target essence. For this reason, the tobacco industry proposes: the imitated essence has the advantages of basically consistent main components and basically consistent sensory effect with the imitated target essence, and can be replaced. The two basically consistent requirements are relatively general, and how to quantitatively evaluate the substitution of the function of the essence becomes the difficulty in evaluating the imitation mixed essence.
Disclosure of Invention
The invention provides a method for quantitatively evaluating the substitutability of essence function, which comprises the following steps:
mixing the imitated blended essence into the imitated essence to obtain mixed essence samples with different mixing ratios;
adding the imitated essence, the blended essence sample and the imitated essence into a blank cigarette respectively, carrying out triangular smoking sensory evaluation, determining the blended essence sample with a significant difference with the imitated essence through three-point inspection, wherein the blending ratio corresponding to the blended essence sample with the smallest blending ratio in the blended essence samples with significant differences is a critical value of the consistency of the sensory functions of the imitated essence and the imitated essence, and determining that the consistency degree of the sensory functions of the imitated essence and the imitated essence is within the blending ratio.
In some embodiments, the number of the blended essence samples with different blending ratios is at least 9, and the blending ratios are distributed in a gradient manner between 0% and 100%.
In certain embodiments, a sample of blended flavor that differs significantly from the emulated flavor is determined according to the three-point test method specified in the national standard "GB/T12311 sensory analysis methods three-point test".
In some embodiments, the number of the blended flavor samples having different blending ratios is 9, and the gradient of the blending ratio is 10%. For example, the blending ratio of the imitation essence in the blended essence sample is 10%, 20%, 30%, 50%, 60%, 80% and 90% (mass percentage), respectively.
In certain embodiments, the method of quantitatively evaluating the substitutability of a flavor function further comprises:
collecting chromatographic fingerprint spectrums of the simulated essence and the simulated blending essence;
and (4) calculating the similarity of the chromatographic fingerprint spectrums of the simulated essence and the simulated essence, and determining the consistency degree of the main components of the simulated essence and the simulated essence.
In some embodiments, the similarity of the chromatographic fingerprint spectrums of the simulated essence and the simulated essence is calculated by using an included angle cosine method.
In certain embodiments, the method for quantitatively evaluating the substitutability of a flavor function further comprises: before the similarity of the chromatographic fingerprint of the simulated essence and the simulated essence is calculated, the chromatographic fingerprint is preprocessed, an electric signal of the chromatographic fingerprint changing along with time is extracted, and the electric signal is stored in a digital format.
In certain embodiments, pre-processing the chromatographic fingerprint comprises one or more of the following processes:
deducting baseline noise;
Savitzky-Golay smoothing filtering processing;
and calibrating the internal standard peak height.
In some embodiments, the Savitzky-Golay smoothing process selects a point number of 11 points and a polynomial degree of 3.
In certain embodiments, the chromatographic fingerprints of the simulated and simulated fragrances are collected using solid phase microextraction-gas chromatography mass spectrometry.
The invention has the beneficial technical effects
The method for quantitatively evaluating the substitutability of the function of the essence can objectively evaluate the consistency degree of the function of the imitated essence and the imitated essence, and provides data and method support for the imitated essence to enter the full formula of the cigarette essence.
In practical application, after the critical value of the consistency of the sensory functions of the imitated essence and the imitated essence is determined, the consistency degree of the sensory functions of the imitated essence and the imitated essence can be determined to be within the mixing proportion, namely within the mixing proportion, the imitated essence can be replaced by the imitated essence.
Drawings
Fig. 1 is a chromatographic fingerprint of an imitated essence A and an imitated compound essence FA, wherein the upper graph is the chromatographic fingerprint of the imitated essence A, and the lower graph is the chromatographic fingerprint of the imitated compound essence FA.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The raw materials, equipment or apparatus used are conventional products which are commercially available, and manufacturers are not indicated.
Examples
1. Sample preparation
Preparing simulated essence A and simulated compound essence FA.
Mixing the imitated blending essence FA with the imitated blending essence A according to the mass ratio of 10, 20, 30, 50, 60, 80 and 90 percent to obtain the blended essence, wherein the numbers of the blended essence are respectively C-10, C-20, C-30, C-50, C-60, C-80 and C-90.
2. Chromatographic fingerprint analysis
Performing chromatographic fingerprint analysis on the imitated essence FA, the imitated essence A and the blended essence by using solid phase microextraction-gas chromatography mass spectrometry (GC-MS) to obtain fingerprints, wherein the chromatographic fingerprint of the imitated essence A and the imitated essence FA is shown in figure 1.
The specific analysis method is as follows:
(1) Preparing a sample: accurately weighing a certain amount of sample to be detected in a headspace bottle, adding 10 mu L of ethanol solution (10 mg/L) of internal standard 2-octanol and 2.0g of sodium chloride, and sealing for detection.
(2) Solid phase micro-extraction: aging the SPME solid phase micro-extraction head at 250 deg.C for 30min, and simultaneously shaking and balancing the headspace bottle containing the sample to be tested at 60 deg.C for 15min. And inserting the aged extraction head into a headspace bottle containing a sample to be detected, adsorbing the headspace at 60 ℃ for 45min, inserting the headspace bottle into a gas chromatograph, analyzing the headspace bottle at 250 ℃ for 3min, and performing GC-MS analysis.
(3) GC-MS analysis: chromatography column, agilent HP-INNOWAX (30 m.times.0.25 mm.times.0.25 μm) elastic quartz capillary column; the temperature of a sample inlet is 250 ℃; temperature rising procedure: the initial column temperature is 40 ℃, the temperature is kept for 5min, the temperature is increased to 240 ℃ at the speed of 5 ℃/min, the temperature is kept for 5min, and the running time is 5min later; carrier gas, he (purity is more than 99.999%), and column flow is 1.0mL/min; no split-flow sample introduction.
MS conditions: an ionization source: EI; ionization energy: 70eV; ion source temperature: 230 ℃; mass spectrometry quadrupole temperature: 150 ℃; mass scan range (m/z): 35-450.
3. Fingerprint similarity evaluation
(1) Data processing: and (3) processing the obtained chromatogram by deducting baseline noise and Savitzky-Golay smoothing filtering (counting 11 points and carrying out polynomial times for 3 times), extracting an electric signal of the change of the chromatographic fingerprint along with time after calibrating the internal standard peak height, and storing the electric signal into a digital format.
(2) And (3) similarity calculation: similarity calculation is carried out on the chromatographic data of the imitated compound essence FA and the blended essence and the chromatographic data of the imitated essence A by adopting an included angle cosine method to obtain similarity, the consistency degree of the main components of the imitated compound essence A and the imitated essence A is determined, and the result is shown in table 1.
TABLE 1 evaluation results of replaceability
| Sample numbering | Degree of similarity (%) | Triangle sniff | Triangle evaluation |
| C-10 | 92.84 | No difference (9-2) | No difference (9-3) |
| C-20 | 85.38 | No difference (9-1) | No difference (9-3) |
| C-30 | 80.22 | No difference (9-3) | Obvious difference (9-6) |
| C-50 | 65.24 | No difference (9-5) | Obvious difference (9-8) |
| C-60 | 63.47 | Obvious difference (9-9) | Obvious difference (9-9) |
| C-80 | 60.89 | Obvious difference (9-9) | Obvious difference (9-9) |
| C-90 | 58.36 | Obvious difference (9-9) | Obvious difference (9-9) |
| FA | 90.56 | Obvious difference (9-9) | Obvious difference (9-9) |
Note: the number in the brackets in front is the number of the person who is evaluated, and the number in the brackets in the rear is the number of the accurately identified person.
From the evaluation results, it can be seen that: the similarity between the imitated compound essence FA and the imitated essence A is 90.56 percent, and the consistency degree of the components is 90.56 percent; along with the increase of the mixing proportion of the imitated essence FA, the similarity of the mixed essence and the imitated essence A is gradually reduced.
4. Sensory evaluation
Adding the imitated blended essence FA, the blended essence and the imitated essence A into a blank cigarette according to the mass ratio of 0.02%, selecting 9 persons according to GB/T12311 sensory analysis method triple inspection to perform triangle sniff and triangle smoking sensory evaluation, and obtaining the evaluation result shown in the table 1.
Sensory evaluation results show that: (1) The imitated blending essence FA and the imitated essence A have obvious difference through triangle sniffing and triangle evaluation; (2) With the increase of the mixing proportion of the imitated essence FA, the difference between the mixed essence sample and the imitated essence A sample can be gradually identified by triangle sniffing and triangle panel test, when the mixing proportion is 30%, the difference between the mixed essence sample and the imitated essence A sample can be obviously identified by triangle panel test, and the difference cannot be identified by triangle sniffing, which indicates that the sensitivity of triangle panel test is higher than that of triangle sniffing.
Therefore, the consistency degree of the sensory function effects of the imitated compound essence FA and the imitated essence A is determined to be within 30 percent, when the formula is replaced, the maximum replacement proportion of the imitated compound essence FA is 30 percent, and a replacement proportion test is recommended to be carried out within 30 percent.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (10)
1. A method for quantitatively evaluating the replaceability of a functional effect of essence, comprising the following steps:
mixing the imitated blended essence into the imitated essence to obtain mixed essence samples with different mixing ratios;
adding the imitated essence, the blended essence sample and the imitated essence into a blank cigarette respectively, carrying out triangular smoking sensory evaluation, determining the blended essence sample with a significant difference with the imitated essence through three-point inspection, wherein the blending ratio corresponding to the blended essence sample with the smallest blending ratio in the blended essence samples with significant differences is a critical value of the consistency of the sensory functions of the imitated essence and the imitated essence, and determining that the consistency degree of the sensory functions of the imitated essence and the imitated essence is within the blending ratio.
2. The method as claimed in claim 1, wherein the number of the blended flavor samples having different blending ratios is at least 9, and the blending ratios are distributed in a gradient manner between 0% and 100%.
3. A method as claimed in claim 1, wherein the sample of blended flavour which differs significantly from the flavour being emulated is determined by a triple point test as defined in the national standard "GB/T12311 sensory analysis method triple point test".
4. The method as set forth in claim 2, wherein the number of the blended flavor samples having different blending ratios is 9, and the gradient of the blending ratio is 10%.
5. The method of any of claims 1-4, further comprising:
collecting chromatographic fingerprint spectrums of the simulated essence and the simulated blending essence;
and calculating the similarity of the chromatographic fingerprint spectrums of the imitated blending essence and the imitated essence, and determining the consistency degree of the main components of the imitated blending essence and the imitated essence.
6. The method of claim 5, wherein the similarity of the chromatographic fingerprints of the simulated compound and simulated essence is calculated by an included angle cosine method.
7. The method of claim 5, further comprising: before the similarity of the chromatographic fingerprint of the simulated essence and the simulated essence is calculated, the chromatographic fingerprint is preprocessed, an electric signal of the chromatographic fingerprint changing along with time is extracted, and the electric signal is stored in a digital format.
8. The method of claim 7, wherein preprocessing the chromatographic fingerprint comprises one or more of:
deducting the baseline noise;
Savitzky-Golay smoothing filtering processing;
and calibrating the internal standard peak height.
9. The method of claim 8, wherein the Savitzky-Golay smoothing process selects a point number of 11 points and a polynomial degree of 3.
10. The method of claim 5, wherein the simulated flavor and the simulated flavor are collected by solid phase microextraction-gas chromatography mass spectrometry.
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