CN111610276A - Cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components - Google Patents
Cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components Download PDFInfo
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- CN111610276A CN111610276A CN202010519519.6A CN202010519519A CN111610276A CN 111610276 A CN111610276 A CN 111610276A CN 202010519519 A CN202010519519 A CN 202010519519A CN 111610276 A CN111610276 A CN 111610276A
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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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
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention relates to the technical field of cigarettes, in particular to a cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components; based on the characteristic that the characteristic component nicotine of the tobacco raw material of the cigarette is obviously different, cut tobacco of a formula corresponding to the tobacco grade and the blended raw material are respectively taken, crushed into powder and prepared into different blended raw material mass proportions, and a mathematical model is established by taking the mass proportion of the blended raw material as an independent variable and the nicotine value as a dependent variable; substituting the measured results of nicotine in different cigarette sections into the model, and calculating to obtain the actual mixing proportion of the raw materials in each section of the cigarette; the method can realize accurate measurement of the actual raw material blending proportion in different intervals of the same cigarette, has better matching property with the perception of consumers, has less sample consumption and simple and accurate detection method compared with the prior method, better avoids the phenomenon that the blending proportion is distorted possibly caused by large sample amount, and can provide technical support for accurate regulation and control of cigarette formula and cigarette rolling uniformity technology development.
Description
Technical Field
The invention relates to the technical field of cigarettes, in particular to a cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components.
Background
In the cigarette processing process, the blending phenomenon of various raw materials such as cut tobacco, reconstituted tobacco cut tobacco, cut stems, expanded cut tobacco and the like usually exists, and whether the blending of different raw materials is uniform or not has great influence on the quality of cigarette products. In recent years, with the digital proposal of cigarette design, the characterization means and the technical development of leaf group blending uniformity become one of the key research directions in the tobacco industry.
The cigarette production process in the tobacco industry mainly controls the blending proportion by adjusting the conveying flow of each raw material, but in the actual cigarette processing process, the tobacco shred blending instantaneous precision design tolerance value is far higher than the accumulated precision design tolerance value. The characterization means generally converts the blending uniformity index into mixing uniformity or density uniformity, and YC/T426 takes the product of sugar-base ratio and potassium as a characteristic value of a chemical index, so as to establish a method for detecting mixing uniformity. Chinese patents CN201410386289.5, CN201811203433.1, etc. provide a method for detecting mixing uniformity. Chinese patent CN 201710350791.4 provides a quantitative evaluation method for cigarette density distribution uniformity. The standards and patents have positive significance for judging the mixing uniformity or the density uniformity of the raw materials, but certain differences exist between evaluation indexes such as the mixing proportion uniformity, the mixing uniformity and the like, the existing standards and patents cannot realize accurate measurement of the actual mixing proportion of the raw materials in different intervals of a single cigarette, and simultaneously, the required sample amount is large and has a large difference with the actual sample amount perceived by consumers.
Disclosure of Invention
The invention provides a cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components, aiming at solving the technical problems that the existing standard and method can not realize accurate measurement of the actual mixing proportion of raw materials in different sections of a single cigarette, simultaneously the required sample amount is large, and the difference between the required sample amount and the actual sample amount sensed by a consumer is large; establishing a model by using the cut stem blending proportion and the nicotine value, verifying the accuracy of the model, and substituting the actual measurement of each section of nicotine into the model to obtain the actual blending proportion, thereby realizing the measurement of the blending proportion distribution of the raw material of a single cigarette.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components is characterized by comprising the following steps:
(1) taking tobacco and tobacco leaf shreds and tobacco stem shreds corresponding to the tobacco in the formula; drying the cut leaves and cut stems of the formula, crushing and sieving by a 40-mesh sieve; the cigarette is balanced for 48 hours at the temperature of 22 +/-1 ℃ and the relative humidity of 60% +/-3%; respectively measuring the moisture of the tobacco shreds, the formula leaf powder and the stem powder by using an oven method;
(2) mixing the cut tobacco powder and the cut stem powder in the formula in the step (1) according to a designed mass ratio by dry basis mass, so that the mass ratio of the cut stem powder is 0-100%, and respectively preparing a modeling sample and a verification sample;
(3) removing filter rod sections from the cigarettes in the step (1), segmenting the cigarettes in equal proportion, taking tobacco shreds of all sections of the cigarettes and the mixed tobacco powder in the step (2), and respectively measuring the nicotine content of each sample by using an internal standard curve method;
(4) analyzing the detection result, selecting 5-6 stem mixing proportion samples as modeling samples, taking the stem mixing proportion as an independent variable, taking the measured value of nicotine as a dependent variable, and establishing an actual measurement mathematical model;
and selecting the other 4-5 mixing proportions as verification samples, measuring the nicotine content of the verification samples, substituting the nicotine measurement result into the model to calculate the actually measured mixing proportion, wherein the range difference between the actually measured mixing proportion and the designed mixing proportion is less than 2 percent, and the model is accurate and effective.
(5) And (4) substituting the measured nicotine value of each section of the cigarette in the step (3) into the mathematical model in the step (4), and calculating to obtain the actual mixing proportion of each section of the raw materials of the cigarette.
Further, the mass of the cut stem powder in the step (2) accounts for 0%, 10%, 20%, 25%, 30%, 50%, 60%, 75%, 80% and 100% of the total mass of the mixed powder respectively; wherein the mass percentage of the cut stem powder in the modeling sample is 0%, 10%, 25%, 50%, 75% and 100%, and the mass percentage of the cut stem powder in the modeling sample is 20%, 30%, 60% and 80%.
Further, the step of determining the nicotine amount of each sample by the internal standard curve method in the step (3) comprises the following steps:
a, preparing a nicotine standard solution;
b, respectively weighing samples, accurately weighing the samples to 0.0001g, placing the samples in a 15mL centrifugal test tube, adding a NaOH solution, an extraction solvent and an internal standard working solution, shaking the samples, carrying out ultrasonic extraction, centrifuging the samples, filtering extract liquor by using a 0.45 mu m organic phase filter membrane to prepare a sample to be detected, and carrying out GC analysis on the sample to be detected and a standard solution according to the same parameters; the GC analysis conditions were: a chromatographic column: DB-WAX capillary column (30m × 0.25mmi.d, × 0.25.25 μm d.f), an injection port temperature of 250 ℃, a programmed temperature rise:
sample introduction amount: 1.0 μ L; the split ratio is as follows: 10: 1; carrier gas: helium (99.999%); flow rate of carrier gas: 1.0 mL/min; a detector: FID or MS;
and c, carrying out regression analysis on the corresponding concentration of the standard solution according to the ratio of the chromatographic peak area of the standard solution to the internal standard peak area to obtain a nicotine internal standard curve equation, and calculating the nicotine content of the sample according to the nicotine internal standard working curve.
Further, in the step (3), the cigarettes without the filter stick sections are equally divided into 4-8 sections by using scissors or other appliances according to equal proportion.
Further, the drying method in the step (1) is natural airing or drying in a forced air drying oven at 40 ℃ for 2 hours.
Further, the nicotine standard working solution concentration in the step (3) a is 10 μ g/mL, 50 μ g/mL, 100 μ g/mL, 200 μ g/mL, 500 μ g/mL respectively.
Further, the extraction solvent in the step (3) b is one of ethyl acetate and methyl tert-butyl ether, the ultrasonic working frequency is 40kHz, and the time is 40 min.
Further, the internal standard in the step (3) b is octadecane.
Compared with the prior art, the invention has the following beneficial effects:
the invention establishes the measuring method of the mixing proportion distribution of each section of raw material of the cigarette by taking the nicotine which is the characteristic component of the tobacco as a marker, and the measuring result has better matching property with the perception of consumers. Compared with the prior art, the method has the advantages of less sample consumption, high sensitivity and good repeatability, and can effectively guide cigarette enterprises to develop the development work of raw material mixing related technologies, thereby improving the stability of the quality of cigarette products.
Drawings
FIG. 1 is a superimposed chromatogram of a dust and stem of example 1 of the present invention, in which 1 is an internal standard and 2 is nicotine.
FIG. 2 is a standard curve diagram of an internal standard of example 1 of the present invention.
FIG. 3 is a diagram of an actual measurement model and a theoretical model in example 1 of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
(1) Instruments and reagents: model 6890/5975 gas chromatography-mass spectrometer (GC/MS, Agilent, USA); KQ-500DE model digital control ultrasonic cleaner (Kunshan ultrasonic instruments Co., Ltd.); l550 low speed centrifuges (xiang instrument centrifuges, ltd); CP2245 type electronic balance (sensory 0.0001g, Sartorius, Germany). Nicotine and n-octadecane as standard substances; ethyl acetate is chromatographic grade.
(2) Collecting samples: the method comprises the steps of blending cut stems and cigarettes of a certain specification (the design value of cut stem blending is 20%), and respectively taking tobacco branches and corresponding formula cut leaves and cut stems.
(3) Sample pretreatment and equilibrium water content determination: the cut leaves and cut stems of the formula are dried, crushed and sieved by a 40-mesh sieve. The cigarette is balanced for 48 hours in an environment with the temperature of 22 +/-1 ℃ and the relative humidity of 60% +/-3%. The water content of each sample was measured by the oven method.
(3) Sample preparation: mixing the cut tobacco powder and the cut stem powder according to a certain mass ratio on a dry basis, preparing a modeling sample by taking 0%, 10%, 25%, 50%, 75% and 100% of the cut stem powder, and preparing a verification sample by taking 20%, 30%, 60% and 80% of the cut stem powder. The cigarette sample is divided into 6 sections in equal proportion after the filter rod end is removed, and each section of tobacco shred is taken as a sample to be measured.
(4) Preparing a nicotine standard solution: standard working solutions with nicotine concentrations of 9.9. mu.g/mL, 49.3. mu.g/mL, 98.6. mu.g/mL, 197.2. mu.g/mL and 493.0. mu.g/mL were prepared using octadecane as an internal standard.
(5) And (3) sample determination: weighing 0.1g of sample (accurate to 0.0001g, adding and weighing all cigarette segmented samples) into a 15mL centrifuge tube, adding 2.5mL of 5% NaOH solution, 10mL of extraction solvent and 100 μ L of internal standard working solution (20.6mg/mL), manually shaking, performing 40kHz ultrasonic extraction for 40min, centrifuging at 4000rpm for 5min, taking 1mL of extract, passing through a 0.45 μm organic phase filter membrane to prepare a sample to be measured, and performing GC analysis on the sample to be measured and the standard solution according to the same parameters.
The GC analysis conditions were a DB-WAX capillary column (30m × 0.25.25 mm i.d., × 0.25.25 μm d.f), an inlet temperature of 250 ℃, temperature programming:sample introduction amount: 1.0 μ L; the split ratio is as follows: 10: 1; carrier gas: helium (99.999%); flow rate of carrier gas: 1.0 mL/min; a detector: FID.
(6) Drawing an internal standard curve equation: performing regression analysis on the corresponding concentration by using the ratio of the chromatographic peak area of the standard substance solution to the internal standard peak area to obtain a nicotine internal standard curve equation with y being 0.0036x-0.0075 and a linear correlation coefficient (r)2) Is 0.9999.
(7) Establishing and verifying a cut stem blended nicotine model: and calculating, modeling and verifying the nicotine amount of the sample through a nicotine internal standard working curve. The mass ratio of the cut stems in the modeling sample is used as an independent variable, the nicotine content is used as a dependent variable, an actual measurement model of the cut stems doped with nicotine is established, the actual measurement model is y-0.1682 x +22.054, and the linear correlation coefficient (r) is2) Is 0.9986. And calculating to obtain a theoretical model y which is-0.1697 x +21.907 by taking the mass ratio of the cut stems powder of 0 percent and 100 percent as independent variables and the amount of the nicotine as dependent variables. The actual measurement model is closer to the theoretical model.
The nicotine amount of the verified sample is measured and respectively substituted into an actual measurement model and a theoretical model to calculate the stem powder mixing proportion, the extreme difference value between the calculated mixing proportion and the designed mixing proportion is less than 2 percent, the RSD is less than 5 percent, and the result shows that the model is accurate and effective as shown in Table 1. The number of samples measured by the theoretical model is less, and the detection efficiency can be improved.
Table 1 verification sample measured values are compared to model calculated values (%, n ═ 6)
(8) And (3) sample determination results: selecting cigarettes with a certain specification and a designed value of the stem blending proportion of 20%, randomly selecting 10 cigarettes, dividing each cigarette into 6 sections, measuring the dry-base nicotine content of each sample, substituting the dry-base nicotine content into an actual measurement model to calculate the actual stem blending proportion of each sample, and as shown in table 2, the minimum stem blending proportion is 11.2%, the maximum stem blending proportion is 37.2%, and the actual stem blending proportion is respectively 8.8% and 17.2% deviated from the designed stem blending proportion.
Table 2 sample measured cut stem blending ratio (%)
Example 2
(1) Collecting samples: taking cut tobacco leaves and cut stems of the formula in the example 1, and preparing cigarette samples according to the cut stem mixing design value of 30%.
(2) The procedure of (7) is the same as in example 1.
(8) The mixing proportion of each section of the tobacco stems is distributed as follows: the method comprises the steps of determining a nicotine theoretical design value according to a blending design standard, randomly selecting 10 cigarettes, dividing each cigarette into 6 sections, measuring 60 samples, measuring the dry-base nicotine content of each sample, substituting the dry-base nicotine content into an actual measurement model to calculate the actual stem blending proportion of each sample, wherein the minimum stem blending proportion is 12.5%, the maximum blending proportion is 51.2%, and the deviation is 17.5% and 21.2% respectively compared with the design blending proportion.
Claims (8)
1. A cigarette raw material mixing proportion distribution measuring method based on tobacco characteristic components is characterized by comprising the following steps:
(1) taking tobacco and tobacco leaf shreds and tobacco stem shreds corresponding to the tobacco in the formula; drying the cut leaves and cut stems of the formula, crushing and sieving by a 40-mesh sieve; the cigarette is balanced for 48 hours at the temperature of 22 +/-1 ℃ and the relative humidity of 60% +/-3%; respectively measuring the moisture of the tobacco shreds, the formula leaf powder and the stem powder by using an oven method;
(2) mixing the cut tobacco powder and the cut stem powder in the formula in the step (1) according to a designed mass ratio by dry basis mass, so that the mass ratio of the cut stem powder is 0-100%, and respectively preparing a modeling sample and a verification sample;
(3) removing filter rod sections from the cigarettes in the step (1), segmenting the cigarettes in equal proportion, taking tobacco shreds of all sections of the cigarettes and the mixed tobacco powder in the step (2), and respectively measuring the nicotine content of each sample by using an internal standard curve method;
(4) analyzing the detection result, selecting 5-6 stem mixing proportion samples as modeling samples, taking the stem mixing proportion as an independent variable, taking the measured value of nicotine as a dependent variable, and establishing an actual measurement mathematical model;
selecting the other 4-5 mixing proportions as verification samples, measuring the nicotine content of the verification samples, substituting the nicotine measurement result into the model to calculate the actually measured mixing proportion, wherein the range difference between the actually measured mixing proportion and the designed mixing proportion is less than 2 percent, which indicates that the model is accurate and effective;
(5) and (4) substituting the measured nicotine value of each section of the cigarette in the step (3) into the mathematical model in the step (4), and calculating to obtain the actual mixing proportion of each section of the raw materials of the cigarette.
2. The method for measuring the blending proportion distribution of the cigarette raw materials based on the characteristic components of the tobacco, according to the claim 1, characterized in that the weight of the cut stem powder in the step (2) is respectively 0%, 10%, 20%, 25%, 30%, 50%, 60%, 75%, 80% and 100% of the total weight of the mixed powder; wherein the mass percentage of the cut stem powder in the modeling sample is 0%, 10%, 25%, 50%, 75% and 100%, and the mass percentage of the cut stem powder in the modeling sample is 20%, 30%, 60% and 80%.
3. The method for measuring the cigarette raw material mixing proportion distribution based on the tobacco characteristic components according to claim 1, wherein the step of measuring the nicotine amount of each sample by an internal standard curve method in the step (3) comprises the following steps:
a, preparing a nicotine standard solution;
b, respectively weighing the samples, accurately weighing the samples to 0.0001g, placing the samples in a 15mL centrifugal test tube, adding NaOH solution, an extraction solvent and an internal standard working solution, shaking the samples, carrying out ultrasonic extraction, centrifuging the samples, taking extract, and filtering the extract through a 0.45 mu m organic phase filter membrane to prepare a sample to be measured, wherein the sample to be measured and the standard solution are subjected to the same referenceGC analysis is carried out under the conditions of a chromatographic column of DB-WAX capillary column (30m × 0.25mm i.d., × 0.25.25 μm d.f), an injection port temperature of 250 ℃, a programmed temperature:
(ii) a Sample introduction amount: 1.0 μ L; the split ratio is as follows: 10: 1; carrier gas: helium (99.999%); flow rate of carrier gas: 1.0 mL/min; a detector: FID or MS;
and c, carrying out regression analysis on the corresponding concentration of the standard solution according to the ratio of the chromatographic peak area of the standard solution to the internal standard peak area to obtain a nicotine internal standard curve equation, and calculating the nicotine content of the sample according to the nicotine internal standard working curve.
4. The method for measuring the blending proportion distribution of the cigarette raw materials based on the characteristic components of the tobacco as claimed in claim 1, wherein the cigarettes without the filter rod segments are equally divided into 4 to 8 segments in step (3) by scissors or other devices according to equal proportion.
5. The method for measuring the blending proportion distribution of the cigarette raw materials based on the tobacco characteristic components is characterized in that the drying method in the step (1) is natural drying or drying in a blast drying oven at 40 ℃ for 2 hours.
6. The method for measuring the blending ratio distribution of tobacco raw materials based on characteristic components of tobacco as claimed in claim 3, wherein the concentration of the nicotine standard working solution in step (3) a is 10 μ g/mL, 50 μ g/mL, 100 μ g/mL, 200 μ g/mL, or 500 μ g/mL, respectively.
7. The method for measuring the blending ratio distribution of the cigarette raw material based on the characteristic components of the tobacco as claimed in claim 3, wherein the extraction solvent in the step (3) b is one of ethyl acetate and methyl tert-butyl ether, the ultrasonic working frequency is 40kHz, and the time is 40 min.
8. The method for measuring the blending proportion distribution of the cigarette raw material based on the characteristic components of the tobacco as claimed in claim 3, wherein the internal standard in the step (3) b is octadecane.
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