CN111458462A - Rapid detection method for ethanol content of reconstituted tobacco raw material ethanol extract - Google Patents
Rapid detection method for ethanol content of reconstituted tobacco raw material ethanol extract Download PDFInfo
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Abstract
The invention provides a method for rapidly detecting the ethanol content of reconstituted tobacco raw material ethanol extract, belonging to the technical field of reconstituted tobacco production and comprising the following steps of: (1) weighing a first concentrated solution of reconstituted tobacco raw materials to obtain a volume V0While simultaneously calculating the density rho0(ii) a (2) Adding ethanol into the first concentrated solution, and calculating to obtain ethanol concentration C of mixed solution after adding ethanol for the nth timenSolid content DnAnd density ρn(ii) a (3) Concentrating the solution, repeating the steps (1) and (2), and concentrating the ethanol to obtain ethanol solution Cn', solid content Dn' and density ρn'; (4) combining the two groups of experimental data, taking the solid content and the density as independent variables and the ethanol concentration as dependent variables, and performing multiple regression analysis to obtain a regression equation. The method is convenient to operate, has high result accuracy, is suitable for online detection of a production line and research in a laboratory, and can objectively represent the ethanol content of the reconstituted tobacco raw material ethanol extract.
Description
Technical Field
The invention belongs to the technical field of reconstituted tobacco production, and particularly relates to a method for quickly detecting the ethanol content of an alcohol extract of a reconstituted tobacco raw material.
Background
The reconstituted tobacco is also called paper-making reconstituted tobacco, which is widely applied to the tobacco industry because the paper-making reconstituted tobacco has the characteristics of good processing resistance, obvious tar reducing effect, strong product quality plasticity and the like.
The extraction is also called extraction, leaching and leaching, is a key link in the reconstituted tobacco production process, and the extraction process can separate flavor substances in the tobacco raw materials from solid matters insoluble in a solvent. The extraction process of the reconstituted tobacco usually adopts water or ethanol solution as a solvent. Researches show that water has a good extraction effect on water-soluble aroma substances such as saccharides, amino acids, phenols and the like in tobacco leaves, and in contrast, ethanol has a good dissolution effect on polar and low-polar key aroma components in tobacco raw materials, so that extraction of the tobacco raw materials by using an ethanol solution as a solvent is beneficial to improvement of the quality of reconstituted tobacco products.
The published Chinese patent with the application number of CN201911118313.6 discloses a method for detecting the purity of reconstituted tobacco coating liquid based on a composite washing technology, and the invention provides a method for detecting the purity of reconstituted tobacco coating liquid based on a composite washing technology, wherein the coating liquid is diluted firstly to reduce the viscosity of the liquid and improve the solid-liquid separation effect in the centrifugal process; in the process of multiple centrifugal washing, the sediment is washed by clear water, so that the influence of water-soluble components carried in wet sediment on the result accuracy can be reduced as much as possible; then ethanol is adopted to wash the precipitate, so that the influence of alcohol-soluble components carried in wet precipitate on the result accuracy can be reduced as much as possible; and finally, washing the precipitate by using ether, so that the influence of oil-soluble components carried in wet precipitate on the accuracy of the result can be reduced as much as possible. The detection method of the invention is simple, easy to implement, less in sampling amount and accurate in result. The detection method in this application, however, is not applicable to detection of the ethanol content in the concentrated solution.
The published Chinese patent with the publication number of CN106036985A discloses a method for manufacturing reconstituted tobacco by a high-aroma-retention paper-making method, wherein tobacco fragments used for producing the reconstituted tobacco by the paper-making method are extracted by ethanol, and an extracting solution is concentrated to obtain an alcohol extract for later use; and (3) preparing the reconstituted tobacco substrate from the tobacco fragments extracted by the ethanol by adopting a paper-making reconstituted tobacco production process, and spraying the ethanol extract on the surface of the reconstituted tobacco substrate by adopting a fragrance spraying mode to prepare the high-fragrance-retention paper-making reconstituted tobacco. The method can effectively avoid the loss of the aroma components of the reconstituted tobacco, and the prepared high-aroma-retention paper-making reconstituted tobacco has high aroma component content, high smoking aroma concentration and small wood miscellaneous gas, the smoking quality is close to that of natural tobacco, and the appearance color is more oily than that of the common paper-making reconstituted tobacco and is close to that of the natural tobacco. In this application, ethanol is used to extract and concentrate tobacco fragments. After extraction, the coating liquid needs to be prepared by reprocessing, and the content of ethanol needs to be monitored in the process.
In the prior art, an alcohol extract obtained by extracting a tobacco raw material with an ethanol solution needs to be concentrated in vacuum to meet the requirement for preparing a coating liquid, in order to research the evaporation condition of ethanol, the ethanol content of the alcohol extract in the concentration process needs to be detected, and the detection can be carried out by adopting a method of YC/T242-2008 'gas chromatography for detecting the content of ethanol, 1, 2-propylene glycol and glycerol', but the method needs to be provided with professional chemical analysis equipment, and meanwhile, the operation process is complex, the consumed time is long, and the requirement on an operator is high, so that the field timely feedback of a detection result cannot be realized.
Disclosure of Invention
In view of the above, the invention provides a method for rapidly detecting the ethanol content of reconstituted tobacco raw material ethanol extract, which is convenient to operate and high in result accuracy, is suitable for online detection of a production line and research of a laboratory, and can objectively represent the ethanol content of reconstituted tobacco raw material ethanol extract.
The application relates to a method for rapidly detecting ethanol content in reconstituted tobacco raw material ethanol extract, which comprises the following steps:
(1) accurately weighing a first concentrated solution of a reconstituted tobacco raw material with the mass of A and the solid content of D to obtain a volume of V0And simultaneously calculating the density rho of the first concentrated solution0The solid content is measured according to the tobacco industry standard YC/T31-1996 oven method for preparing tobacco and tobacco product samples and measuring moisture;
(2) adding ethanol into the first concentrated solution for n times, wherein the addition amount is S1、S2、S3……Sng, volume V of solution measured after each addition of ethanol1、V2、V3、……VnN is more than or equal to 5, (the volume of the solution after the ethanol is added for 1 st time, 2 nd time and 3 rd time till n times is V respectively1、V2、V3……VnAnd) calculating the ethanol concentration C of the mixed solution after the nth ethanol additionnSolid content DnAnd density ρn；
(3) And (3) taking a second concentrated solution of the reconstituted tobacco raw material with solid content of D 'and quality of A' extracted from the same reconstituted tobacco raw material, and repeating the step (1) and the step (2) to obtain: ethanol concentration Cn', solid content Dn' and density ρn’；
(4) Combining the two groups of experimental data, taking solid content and density as independent variables and ethanol concentration as dependent variables, performing multiple regression analysis to obtain a regression equation, and rapidly detecting the ethanol concentration of the reconstituted tobacco ethanol extract sample by using the regression equation to perform multiple regression analysis, wherein SPASS, EXCE L or other multivariate analysis can be usedPerforming regression analysis function on the ethanol concentration of the ethanol extract sample by using data processing software, determining the solid content C of the sample according to tobacco industry standard YC/T31-1996 oven method for preparing tobacco and tobacco product samples and determining moisture, and calculating the density rho (rho =) of the sample by detecting the mass and volume of the sample
Rho is sample density g/m L, A is sample mass g, V is sample volume m L), and the concentration of the sample ethanol can be calculated by substituting the solid content C and the density rho of the sample into a regression equation.
When the concentration of ethanol in the alcohol extract is measured, the solid content and the density of the concentrated solution are substituted into an equation to calculate the concentration of the ethanol, wherein the solid content of the concentrated solution can be measured by taking out part of the solution and then placing the solution in a drying box, and the density of the solution to be measured can be obtained by weighing and calculating the volume.
Wherein the reconstituted tobacco raw material is one or more than two of tobacco fragments, tobacco powder, tobacco stems, waste tobacco leaves, waste tobacco shreds and tobacco powder rods.
The preparation of the first concentrated solution comprises the following steps: the reconstituted tobacco raw material is taken as a raw material, ethanol is taken as an extracting agent, and a hyperconcentrated solution with the solid content of more than 40 percent and the ethanol content of less than or equal to 0.1 percent is obtained through vacuum concentration; adding distilled water into the super-concentrated solution, and uniformly mixing to obtain a first concentrated solution with lower solid content. Preparation of the second concentrated solution refers to the preparation method of the first concentrated solution. The formulas of the reconstituted tobacco raw materials used in the first concentrated solution and the second concentrated solution are the same, and the formulas of the reconstituted tobacco raw materials used in the first concentrated solution and the second concentrated solution are the same as the formula of the reconstituted tobacco raw material used in the alcohol extract to be detected.
Preferably, the ethanol is added in the same amount in the step (2), and S is1=S2=S3……SnThe ethanol concentration C in the step (2)nSolid content DnAnd density ρnThe calculation methods are respectively as follows:
wherein: cnThe concentration (mass concentration) of ethanol in the solution after the ethanol is added for the nth time is percent; dnAdding ethanol for the nth time, and then, adding the solid content of the solution in percent; rhonThe density of the solution after the addition of ethanol for the nth time is g/m L, n is the cumulative times of the addition of ethanol, S is the addition amount of ethanol for each time, g is the mass of the concentrated solution without the addition of ethanol, D is the solid content of the concentrated solution without the addition of ethanol, V is the solid content of the concentrated solution without the addition of ethanol0Volume of concentrate, m L.
Preferably, the ethanol in the step (2) is added in different amounts, S1≠S2≠S3……SnThen, the calculation methods of the ethanol concentration Cn, the solid content Dn and the density ρ n in the step (2) are respectively as follows:
and (3) adding ethanol for n times in the step (2), wherein the total amount of the finally added ethanol is 3-4 times of the mass A of the concentrated solution.
The volume of the solution was measured by stirring it well, standing and maintaining the temperature at 20 ℃.
The invention achieves the following beneficial effects: the invention provides a method for rapidly detecting the ethanol content of an alcohol extract of a reconstituted tobacco raw material, which solves the problem that the ethanol content of the alcohol extract cannot be timely fed back on site in the concentration process. The method does not need to use professional chemical analysis equipment, is convenient and fast to operate, has high result accuracy, is suitable for online detection of a production line and research in a laboratory, and can objectively represent the ethanol content of the reconstituted tobacco raw material ethanol extract.
Detailed Description
The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
Example 1
Detecting the content of ethanol in the ethanol extract obtained during the concentration of the reconstituted tobacco raw material ethanol extract in a certain formula.
A method for rapidly detecting the ethanol content of reconstituted tobacco raw material ethanol extract comprises the following steps:
(1) accurately weighing a first concentrated solution of a reconstituted tobacco raw material with the mass of A and the solid content of D to obtain
To a volume of V0And simultaneously calculating the density rho of the first concentrated solution0The solid content is measured according to the tobacco industry standard YC/T31-1996 oven method for preparing tobacco and tobacco product samples and measuring moisture;
(2) adding ethanol into the first concentrated solution for 5 times, wherein the addition amount is S1、S2、S3……Sng, measuring the volumes of the solution V1, V2, V3, V4 and V5 after adding ethanol each time, and calculating the ethanol concentration C5, the solid content D5 and the density rho 5 of the mixed solution after adding ethanol for the 5 th time;
(3) and (3) taking a second concentrated solution of the reconstituted tobacco raw material with solid content of D 'and quality of A' extracted from the same reconstituted tobacco raw material, and repeating the step (1) and the step (2) to obtain: ethanol concentration C5', solid content D5' and density ρ5’；
(4) Combining two groups of experimental data, taking solid content and density as independent variables and ethanol concentration as dependent variables, performing multiple regression analysis to obtain a regression equation, and using the regression equation to realize rapid detection of the ethanol concentration of the reconstituted tobacco ethanol extract sample
Rho is sample density, g/m L, A is sample mass, g, V is sample volume, m L), and the sample is put into a vacuum furnaceAnd substituting the solid content C and the density rho of the product into a regression equation, and calculating the concentration of the ethanol in the sample.
When the concentration of ethanol in the alcohol extract is measured, the solid content and the density of the concentrated solution are substituted into an equation to calculate the concentration of the ethanol, wherein the solid content of the concentrated solution can be measured by taking out part of the solution and then placing the solution in a drying box, and the density of the solution to be measured can be obtained by weighing and calculating the volume.
The reconstituted tobacco raw materials are a mixture of tobacco fragments, tobacco powder, tobacco stems and waste tobacco leaves.
The preparation of the first concentrated solution comprises the following steps: the reconstituted tobacco raw material is taken as a raw material, ethanol is taken as an extracting agent, and a hyperconcentrated solution with the solid content of more than 40 percent and the ethanol content of less than or equal to 0.1 percent is obtained through vacuum concentration; adding distilled water into the super-concentrated solution, and uniformly mixing to obtain a first concentrated solution with lower solid content. Preparation of the second concentrated solution refers to the preparation method of the first concentrated solution. The formulas of the reconstituted tobacco raw materials used in the first concentrated solution and the second concentrated solution are the same, and the formulas of the reconstituted tobacco raw materials used in the first concentrated solution and the second concentrated solution are the same as the formula of the reconstituted tobacco raw material used in the alcohol extract to be detected.
The addition amount of the ethanol in the step (2) is the same, and S1=S2=S3……SnThe ethanol concentration C in the step (2)nSolid content DnAnd density ρnThe calculation methods are respectively as follows:
wherein: cnThe concentration (mass concentration) of ethanol in the solution after the ethanol is added for the nth time is percent; dnAdding ethanol for the nth time, and then, adding the solid content of the solution in percent; rhonThe density of the solution after the addition of ethanol for the nth time is g/m L, n is the cumulative times of the addition of ethanol, S is the addition amount of ethanol for each time, g is the mass of the concentrated solution without the addition of ethanol, D is the solid content of the concentrated solution without the addition of ethanol, V is the solid content of the concentrated solution without the addition of ethanol0Volume of concentrate, m L.
The volume of the solution was measured by stirring it well, standing and maintaining the temperature at 20 ℃.
The specific test method is as follows;
accurately weighing 50g of reconstituted tobacco raw material alcohol-extracted concentrated solution with the same formula and 42.50% of solid content (obtained by oven method detection), measuring the volume of the concentrated solution, calculating the density of the concentrated solution, and detecting by gas chromatography until no ethanol is detected in the concentrated solution; gradually adding ethanol into the ethanol extractive solution for 5 times, wherein the addition amount is 40g, measuring the volume of the solution after adding ethanol each time, and calculating to obtain ethanol concentration C of the mixed solution after adding ethanol for the nth timenSolid content DnAnd density ρn(ii) a Taking the reconstituted tobacco raw material alcohol extraction concentrated solution with the solid content of 10.00 percent in the same formula, repeating the experiment to obtain another group of detection data: ethanol concentration Cn', solid content Dn' and density ρn', combine two sets of experimental data as follows:
taking the solid content and the density as independent variables and the ethanol concentration as dependent variables, and performing multiple regression analysis by using excel software, wherein the analysis result is as follows;
the results of the anova were as follows:
from the analysis results, the relationship between the ethanol concentration and the solid content of the solution and the density of the solution can be fitted as follows:
Ca=-12.9577+37.13601D-41.6316Ct-24.7215D2-28.0836Ct2+52.49434Ct*D
wherein: concentration/% by mass of ethanol in the Ca-solution; ct-solution solids/%; d-density of solution/g/ml.
The regression statistical result shows that all variables in the equation are highly correlated, and the fitting degree of the regression equation is good. The analysis of variance results show that: the significance statistic of SignificanceF, namely F is 2.79E-8, which is greatly smaller than the significance level of 0.05, and the regression effect of the regression equation is significant. Regression parameter analysis shows that the P value of each variable is less than 0.05, so that the influence of each variable on the ethanol concentration of the solution is obvious.
And respectively taking alcohol extract concentrated solution samples at different times during the process of vacuum concentration of the reconstituted tobacco raw material alcohol extract with the same formula for solid content and density detection, calculating the alcohol concentration of the alcohol extract by using a regression equation, and simultaneously detecting the alcohol concentration of the samples by using a standard method of YC/T242-2008 gas chromatography for measuring the content of the essence ethanol, 1, 2-propylene glycol and glycerol for cigarettes. The results of the detection are as follows.
According to the data, the error between the ethanol concentration of the alcohol extract measured by the method and the ethanol concentration measured by the gas chromatography is in a reasonable range.
Example 2
The experimental procedure in this example is as described in example 1, except that the amounts of ethanol added in the step (2) are different, and S1 ≠ S2 ≠ S3 … … Sn, the methods for calculating the ethanol concentration Cn, the solid content Dn, and the density ρ n in the step (2) are respectively as follows:
the invention discloses a method for rapidly detecting the ethanol content of an alcohol extract of a reconstituted tobacco raw material, and solves the problem that the ethanol content of the alcohol extract cannot be timely fed back on site in a concentration process. The method does not need to use professional chemical analysis equipment, is convenient and fast to operate, has high result accuracy, is suitable for online detection of a production line and research in a laboratory, and can objectively represent the ethanol content of the reconstituted tobacco raw material ethanol extract.
The present invention is not limited to the above-described specific embodiments, and various modifications and variations are possible. Any modifications, equivalents, improvements and the like made to the above embodiments in accordance with the technical spirit of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method for rapidly detecting the ethanol content of an alcohol extract of a reconstituted tobacco raw material is characterized by comprising the following steps:
(1) weighing a first concentrated solution of a reconstituted tobacco raw material with the mass of A and the solid content of D to obtain a volume of V0And simultaneously calculating the density rho of the first concentrated solution0；
(2) Adding ethanol into the first concentrated solution for n times, wherein the addition amount is S1、S2、S3……Sng, volume V of solution measured after each addition of ethanol1、V2、V3、……VnN is more than or equal to 5, and the ethanol concentration C of the mixed solution after the ethanol is added for the nth time is calculatednSolid content DnAnd density ρn；
(3) Taking a second concentrated solution of the reconstituted tobacco raw material with the solid content of D 'and the mass of A' extracted from the same reconstituted tobacco raw material, and repeating the step (1) and the step (2) to obtain the solution with the ethanol concentration of Cn', solid content Dn' and density ρn’；
(4) And combining the two groups of experimental data, performing multiple regression analysis by taking the solid content and the density as independent variables and the ethanol concentration as dependent variables to obtain a regression equation, and quickly detecting the ethanol concentration of the reconstituted tobacco ethanol extract sample by using the regression equation.
2. The method for rapidly detecting the ethanol content in the reconstituted tobacco raw material ethanol extract according to claim 1, wherein the reconstituted tobacco raw material is one or more than two of tobacco fragments, tobacco powder, tobacco stems, waste tobacco leaves, waste tobacco shreds and tobacco powder rods.
3. The method for rapidly detecting the ethanol content in the reconstituted tobacco raw material ethanol extract according to claim 1, wherein the preparation of the first concentrated solution comprises the following steps: ethanol is used as an extracting agent, and a hyperconcentrated solution with the solid content of more than 40 percent and the ethanol content of less than or equal to 0.1 percent is obtained by vacuum concentration; adding distilled water into the super-concentrated solution, and mixing uniformly to obtain a first concentrated solution.
4. The method for rapidly detecting the ethanol content in the alcohol extract of the reconstituted tobacco raw material according to claim 3, wherein the ethanol is added in the step (2) in the same amount, and S is1=S2=S3……Sn。
5. The method for rapidly detecting the ethanol content of the reconstituted tobacco raw material ethanol extract according to claim 4, wherein the ethanol concentration C in the step (2)nSolid content DnAnd density ρnThe calculation methods are respectively as follows:
wherein: cnThe concentration of ethanol in the solution after the ethanol is added for the nth time is percent; dnAdding ethanol for the nth time, and then, adding the solid content of the solution in percent; rhonThe density of the solution after the addition of ethanol for the nth time is g/m L, n is the cumulative addition time of ethanol, and S is the addition amount of ethanol for each time, g.
6. The method for rapidly detecting the ethanol content in the alcohol extract of the reconstituted tobacco raw material according to claim 3, wherein the ethanol is added in different amounts in the step (2), and S is1≠S2≠S3……Sn。
7. The method for rapidly detecting the ethanol content in the reconstituted tobacco raw material ethanol extract according to claim 6, wherein the calculation methods of the ethanol concentration Cn, the solid content Dn and the density ρ n in the step (2) are respectively as follows:
the method for rapidly detecting the ethanol content in the reconstituted tobacco raw material ethanol extract according to claim 1, wherein ethanol is added in the step (2) n times, and the total amount of the finally added ethanol is 3-4 times of the mass A of the concentrated solution.
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Application publication date: 20200728 |