CN107287031B - Method for preparing tobacco additive by separating aroma-developing components of Maillard reactant of aromatic tobacco and application - Google Patents
Method for preparing tobacco additive by separating aroma-developing components of Maillard reactant of aromatic tobacco and application Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
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Abstract
The invention provides a method for preparing a tobacco additive by separating the aroma-developing components of Maillard reactants of an aromatic tobacco and application thereof. The preparation method of the tobacco additive comprises the steps of chopping aromatic tobacco, adding ethanol for extraction, filtering and concentrating to obtain aromatic tobacco extract, then adding reducing sugar and amino acid for Maillard reaction under continuous stirring, adding reactants into a molecular distillation instrument for I-stage distillation, retaining I-stage distillate flowing out along the wall of a vacuum cavity, and continuing II-stage distillation to obtain aroma-showing substances, namely the tobacco additive. The aroma-displaying substance is sprayed into the cigarette tobacco shreds, so that the smoke quality can be improved, the cigarette aroma can be increased, the cigarette smoke is rich, sweet and mellow, the prickling is inhibited, the impurities are reduced, the characteristics of enriching the smoke aroma, enhancing the sweet feeling of the smoke and the like are achieved.
Description
Technical Field
The invention relates to the field of tobacco, in particular to a method for preparing a tobacco additive by separating the aroma-developing components of Maillard reactants of aromatic tobacco and the field of applying the novel tobacco essence and aroma.
Background
At present, cigarette markets at home and abroad require cigarette commodities with the attributes of high fragrance, high concentration and low tar. With the increasing social attention on smoking and health, the cigarette safety is improved, and the development of low-tar cigarettes becomes the main attack direction and development trend of the tobacco industry, but the loss and the reduction of the smoke aroma are often caused while the cigarette tar is reduced, so that the aroma of the cigarettes must be compensated by a flavoring means, and the smoking requirement of consumers is met.
Aromatic tobacco is a tobacco type rich in various fragrant substances, and is a necessary raw material for producing various famous cigarettes, especially high-grade mixed cigarettes. Many studies at home and abroad indicate that the contents of specific aroma substances such as labdane compounds, beta-methylvaleric acid, isovaleric acid, beta-damascenone, solanone and the like in the aromatic tobacco are several times or even ten times higher than those of other types of tobacco, and the ingredients are considered to form important components of unique aroma and taste of the aromatic tobacco.
The Maillard reaction is a series of reactions such as condensation, dehydration, degradation, oxidation reduction and the like of amino acid and reducing sugar or carbonyl compound. Chemical substances with rich varieties and large molecular weight can be generated through the Maillard reaction, so that the whole reactant is full in fragrance, and in addition, the Maillard reactant contains a large amount of fragrant substances and most of the fragrant substances are coordinated with tobacco fragrance, so that the Maillard reaction becomes a good tobacco flavor.
The flavoring and feeding technology is an effective way for improving the smoke concentration and the fragrance of the cigarettes. The tobacco aroma substances obtained by molecular distillation separation can be endowed with natural aroma, so that the aroma substances of the cigarettes are richer, the overall quality of the cigarettes is improved, and a new way is opened up for utilizing the rich natural resources in China. At present, the research on the application of the tobacco additive prepared by treating the aromatic tobacco Maillard reaction extract by molecular distillation in tobacco is rarely reported.
Although the Maillard reactant of the aromatic tobacco extract obtained by the Maillard reaction can well compensate the tobacco fragrance, as the aroma components are not selectively separated, the Maillard reactant contains substances which are not beneficial to the smoking taste of the cigarettes, the side effects of increasing the tobacco fragrance, increasing the smoking taste discomfort, the rough feeling, the dry feeling and the like are also brought. Therefore, substances which are unfavorable for cigarette smoking taste in maillard reactants of the aromatic tobacco extract need to be separated and removed by a molecular distillation device.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for separating the aroma-showing components of Maillard reactants of aromatic tobacco to obtain a novel tobacco essence and flavor and application of the tobacco additive. The light component of the aromatic tobacco extract is sprayed into cigarette tobacco shreds, so that the smoke quality can be improved, the cigarette aroma can be increased, the cigarette smoke is rich, sweet and mellow, the thorns and impurities are reduced, the characteristics of enriching the smoke aroma, enhancing the sweet feeling of the smoke and the like are achieved, and the heavy component can be used for slice feeding and low-grade cigarette feeding. The method provides an effective way for improving the taste of the cigarettes and increasing the amount of the cigarette aroma, and simultaneously reduces resource waste and environmental pollution and improves the additional value of the cigarettes.
The technical scheme of the invention is as follows: the method for preparing the tobacco additive by separating the aroma-developing components of the maillard reaction product of the aromatic tobacco and the application thereof comprise the following steps:
a. chopping aromatic tobacco, adding 50% ethanol into the aromatic tobacco according to the addition amount of 8-12 mL of ethanol added into each gram of aromatic tobacco, extracting for 1-3 h at 50-70 ℃, filtering and concentrating to obtain aromatic tobacco extract;
b. b, mixing the aromatic tobacco extract, reducing sugar and amino acid obtained in the step a according to the mass part ratio of 1: 0.2-0.4: 0.1-0.3, and continuously stirring for carrying out Maillard reaction for 4-6 hours at the temperature of 85-105 ℃ to obtain an aromatic tobacco extract Maillard reactant; wherein the reducing sugar is glucose or fructose, and the amino acid is proline, glutamic acid or alanine;
c. b, adding the Maillard reactant of the aromatic tobacco extract obtained in the step b into a molecular distillation apparatus for I-grade distillation, setting the distillation temperature of the molecular distillation apparatus to be 50-70 ℃, the material flow rate to be 1-2 ml/min, the film scraping rotation speed to be 40-60 r/min, the vacuum degree to be 20-30 Pa, and keeping I-grade distillate flowing out along the wall of the vacuum cavity;
d. c, continuously carrying out II-stage distillation on the I-stage distillate obtained in the step c in a molecular distillation instrument to obtain a light component and a heavy component, namely the tobacco additive; wherein the distillation temperature of the secondary distillation is set to be 65-80 ℃, the material flow rate is 1-3 ml/min, the film scraping rotation speed is 100-150 r/min, and the vacuum degree is 15-20 Pa.
The invention has the following excellent technical scheme: and (b) adding 10mL of 50% ethanol into each gram of aromatic tobacco in the step (a), wherein the extraction temperature is 65 ℃, and the density of the aromatic tobacco extract after filtration and concentration relative to water is 1.150-1.200.
The invention has the following excellent technical scheme: in the step b, the mass part ratio of the aromatic tobacco extract to the reducing sugar to the amino acid is 1: 0.3: 0.2, the reducing sugar is glucose, the amino acid is proline, and the Maillard reaction temperature is controlled at 100 ℃.
The invention has the following excellent technical scheme: in the step c, the distillation temperature of the I-stage molecular distillation is 60 ℃, the material flow rate is 2ml/min, the film scraping rotation speed is 60r/min, and the vacuum degree is 25 Pa; the distillation temperature of the II-grade molecular distillation is 75 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 120r/min, and the vacuum degree is 15 Pa.
The volume ratio of the mass of the aromatic tobacco to the added ethanol with the concentration of 50 percent is a feed-liquid ratio, and the feed-liquid ratio of the invention adopts the corresponding addition of 50 percent ethanol milliliter per gram of aromatic tobacco. Adding 8-12 mL of 50% ethanol into each gram of aromatic tobacco, wherein the ratio of the aromatic tobacco to the 50% ethanol is 8-12.
The invention provides another technical scheme, which is a method for preparing a tobacco additive by separating the aroma-developing components of Maillard reactants of an aromatic tobacco and an application thereof, and is characterized in that: and spraying the II-grade distilled light component obtained by the method into tobacco shreds used for preparing middle-high grade cigarettes, and preparing the middle-high grade cigarettes according to the existing cigarette preparation method, wherein the addition amount of the II-grade distilled light component is 0.05-0.1% of the total weight of the tobacco shreds.
The aromatic tobacco extract generates chemical substances with rich types and large molecular weight through Maillard reaction, and aromatic substances of Maillard reactants of the aromatic tobacco collected by molecular distillation equipment are applied to cigarettes to improve the aroma quality and grade of the cigarettes, increase the aroma of the tobacco, enrich, sweet and mellow smoke, suppress thorns and reduce impurities.
The aroma-showing substance prepared by separation is pure natural spice, has great market potential, is simple and convenient to apply, is easy to realize in the existing cigarette processing technology, and can improve the smoking quality of cigarettes. The patent provides technical and theoretical guidance for tobacco essence.
The invention has the beneficial effects that:
(1) the aroma of the aroma-showing substance prepared by the invention has pleasant caramel-like aroma and aromatic cigarette characteristic aroma, and the aroma is lasting.
(2) The prepared aromatic substance is used in tobacco charging, can improve the quality and grade of cigarette aroma, add the herbal aroma of the cigarette, make the smoke rich, sweet, mellow, stabbing and reducing impurities.
(3) The method has mild reaction conditions, low cost and easy industrial production; in addition, the method provided by the invention does not need to add other chemical reagents, thereby avoiding other potential safety hazards and bad smell caused by the addition of components.
Detailed Description
The technical solution of the present invention is described below with reference to specific examples, but the scope of the present invention is not limited thereto:
example 1, a method for preparing a tobacco additive by separating the flavor-developing components of maillard reactants of an aromatic tobacco and an application thereof, comprising the following steps:
a. pulverizing 10kg aromatic tobacco, adding 100L 50% ethanol, stirring and extracting for 2 hr at 65 deg.C; filtering the extracting solution, taking out the filtrate, and concentrating the filtrate in vacuum at 50 ℃ to obtain an aromatic tobacco extract, wherein the density of the aromatic tobacco extract relative to water is 1.150-1.200;
b. carrying out Maillard reaction on the obtained aromatic tobacco extract: weighing 100g of the aromatic tobacco extract prepared in the step a, 30g of glucose and 20g of proline, then uniformly mixing the aromatic tobacco extract, putting the mixture into a conventional small-sized reaction kettle, controlling the temperature at 100 ℃, and carrying out Maillard reaction for 6 hours under continuous stirring to obtain a Maillard reactant of the aromatic tobacco extract;
c. adding the Maillard reactant of the aromatic tobacco extract obtained in the step b into a molecular distillation apparatus for I-grade distillation: the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation are preliminarily determined by experiments as follows: the distillation temperature is 60 ℃, the material flow rate is 2ml/min, the film scraping rotation speed is 60r/min, and the vacuum degree is 25 Pa; keeping the I-stage distillation light component flowing out along the wall of the vacuum cavity, and detecting that the density of the I-stage distillation light component relative to water is 1.075;
d. and (c) carrying out II-stage distillation on the I-stage distillation light component obtained in the step c, and preliminarily determining the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation through experiments as follows: the distillation temperature is 75 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 120r/min, and the vacuum degree is 15 Pa; collecting the II-grade distillation aroma-showing substances, and detecting that the density of the II-grade distillation aroma-showing substances relative to water is 1.038.
Example 2, a method for preparing a tobacco additive by separating the flavor-developing components of maillard reactants of an aromatic tobacco and an application thereof, comprising the following steps:
a. crushing 10kg of aromatic tobacco, adding 80L of 50% ethanol, stirring and extracting for 3h at the extraction temperature of 50 ℃, filtering the extracting solution, taking out the filtrate, and concentrating the filtrate in vacuum at the temperature of 50 ℃ to obtain aromatic tobacco extract, wherein the density of the aromatic tobacco extract relative to water is 1.150-1.200;
b. carrying out Maillard reaction on the obtained aromatic tobacco extract: weighing 100g of aromatic tobacco extract prepared in the step a, 20g of glucose and 30g of tryptophan, uniformly mixing, putting into a conventional small-sized reaction kettle, controlling the temperature at 90 ℃, and carrying out Maillard reaction for 5 hours under continuous stirring to obtain Maillard reactant of the aromatic tobacco extract;
c. adding the Maillard reactant of the aromatic tobacco extract obtained in the step b into a molecular distillation apparatus for I-grade distillation: the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation are preliminarily determined by experiments as follows: the distillation temperature is 50 ℃, the material flow rate is 2ml/min, the film scraping rotation speed is 50r/min, and the vacuum degree is 20 Pa; keeping the I-stage distilled light component flowing out along the wall of the vacuum cavity, and detecting that the density of the I-stage distilled light component relative to water is 1.073;
d. and (3) carrying out second-stage distillation on the obtained I-stage distillation light component, and preliminarily determining the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation through experiments as follows: the distillation temperature is 75 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 120r/min, and the vacuum degree is 15 Pa; collecting the II-grade distillation aroma-showing substances, and detecting that the density of the II-grade distillation aroma-showing substances relative to water is 1.037.
Example 3, a method for preparing a tobacco additive by separating the flavor-developing components of the maillard reaction products of the aromatic tobacco and an application thereof, comprising the following steps:
a. crushing 10kg of aromatic tobacco, adding 120L of 50% ethanol, stirring and extracting for 2h at the extraction temperature of 70 ℃, filtering the extracting solution, taking out the filtrate, and concentrating the filtrate in vacuum at the temperature of 50 ℃ to obtain aromatic tobacco extract, wherein the density of the aromatic tobacco extract relative to water is 1.150-1.200, and the aromatic tobacco extract is obtained;
b. carrying out Maillard reaction on the obtained aromatic tobacco extract: weighing 100g of aromatic tobacco extract, 30g of fructose and 30g of alanine, uniformly mixing, putting into a conventional small reaction kettle, controlling the temperature at 100 ℃, and carrying out Maillard reaction for 5 hours under continuous stirring to obtain Maillard reactant of the aromatic tobacco extract;
c. adding the Maillard reactant of the obtained aromatic tobacco extract into a molecular distillation apparatus for I-grade distillation: the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation are preliminarily determined by experiments as follows: the distillation temperature is 55 ℃, the material flow rate is 2ml/min, the film scraping rotation speed is 50r/min, and the vacuum degree is 30 Pa; keeping the I-stage distillation light component flowing out along the wall of the vacuum cavity, and detecting that the density of the I-stage distillation light component relative to water is 1.076;
d. and (3) carrying out second-stage distillation on the obtained I-stage distillation light component, and preliminarily determining the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation through experiments as follows: the distillation temperature is 70 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 130r/min, and the vacuum degree is 18 Pa; collecting the II-grade distillation aroma-showing substances, and detecting that the density of the II-grade distillation aroma-showing substances relative to water is 1.039.
Example 4 method and application of preparation of tobacco additive by separation of maillard reactant flavor-developing components of aromatic tobacco, comprising the following steps:
a. crushing 10kg of aromatic tobacco, adding 100L of 50% ethanol, stirring and extracting for 2h at the extraction temperature of 65 ℃, filtering the extracting solution, taking out the filtrate, and concentrating the filtrate in vacuum at the temperature of 50 ℃ to obtain an aromatic tobacco extract, wherein the density of the aromatic tobacco extract relative to water is 1.150-1.200;
b. carrying out Maillard reaction on the obtained aromatic tobacco extract: weighing 100g of aromatic tobacco extract, 20g of fructose and 10g of tryptophan prepared in the step a, uniformly mixing, putting into a conventional small-sized reaction kettle, controlling the temperature at 100 ℃, and carrying out Maillard reaction for 4 hours under continuous stirring to obtain Maillard reactant of the aromatic tobacco extract;
c. adding the Maillard reactant of the obtained aromatic tobacco extract into a molecular distillation apparatus for I-grade distillation: the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation are preliminarily determined by experiments as follows: the distillation temperature is 60 ℃, the material flow rate is 2ml/min, the film scraping rotation speed is 60r/min, and the vacuum degree is 26 Pa; keeping the I-stage distilled light component flowing out along the wall of the vacuum cavity, and detecting that the density of the I-stage distilled light component relative to water is 1.074;
d. and (3) carrying out second-stage distillation on the obtained I-stage distillation light component, and preliminarily determining the optimal conditions for preparing the aromatic tobacco Maillard reactant by molecular distillation through experiments as follows: the distillation temperature is 80 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 150r/min, and the vacuum degree is 20 Pa; collecting the II-grade distillation aroma-developing substance, and detecting that the density of the II-grade distillation aroma-developing substance relative to water is 1.041.
The aromatic tobacco extract, the maillard reaction product of the aromatic tobacco extract, the class II distilled light component and the heavy component obtained in the above example 1 were analyzed by GC-MS, and searched by the WILEY and MAINLIB spectral libraries, thereby identifying 26, 35, 40 and 24 volatile components, respectively.
TABLE 1 comparison of aromatic tobacco extract, Maillard reaction product of aromatic tobacco extract and chemical components of II-level distillation light component and heavy component main aroma-showing substance
In the table I, the cembranes include solanone, cembrane and cembrane triene diol, the labdanes include ambergris ether, oxykerol, ambroxal, 8, 12-epoxy-14-labdane-13-alcohol and ambroxol lactone, the carotenoids include damascenone, hexahydro-farnesone, megastigmatrienone, dihydroactinidiolide and 3-oxo-alpha-ionol, and the other fragrant substances include furfural, furanone, acetyl pyrrole, neophytadiene, ethyl linolenate, methyl palmitate, benzyl alcohol and phenethyl alcohol.
The fragrance characteristics of the fragrance-showing substances can be obtained through the first table, and the fragrance has pleasant caramel-like fragrance, the fragrance characteristics of the aromatic tobacco are fragrant, and the fragrance is lasting.
The aromatic tobacco extract, the maillard reactant of the aromatic tobacco extract and the II-grade distillation light component prepared in the example 1 are added with materials and flavored, the application proportion is the same under the same condition, the applied samples are subjected to sensory comparison and smoking evaluation, 9 members of a sensory smoking panel adopt GB5606.4-2005, the smoking evaluation result is averaged, and the result is detailed in tables 2, 3 and 4. The application proportion is the weight percentage of the tobacco shreds.
Table 2: sensory evaluation result at an application rate of 0.05%
| Sample (I) | Gloss of | Fragrance | Coordination of | Miscellaneous qi | Stimulation of | Aftertaste | Total up to |
| Reference cigarette | 5 | 24.1 | 4.0 | 7.9 | 15.0 | 20.0 | 76.0 |
| Aromatic tobacco extract | 5 | 24.5 | 4.7 | 8.1 | 16.2 | 20.2 | 78.7 |
| Aromatic tobacco extract MaillardReactants | 5 | 24.6 | 4.7 | 8.2 | 16.3 | 20.6 | 79.4 |
| II-stage distillation aroma-showing substance | 5 | 25.2 | 4.9 | 8.5 | 16.7 | 20.9 | 81.2 |
Table 3: sensory evaluation result at an application rate of 0.10%
| Sample (I) | Gloss of | Fragrance | Coordination of | Miscellaneous qi | Stimulation of | Aftertaste | Total up to |
| Reference cigarette | 5 | 24.1 | 4.0 | 7.9 | 15.0 | 20.0 | 76.0 |
| Aromatic tobacco extract | 5 | 24.6 | 4.7 | 8.2 | 16.4 | 20.2 | 79.1 |
| Maillard reactant of aromatic tobacco extract | 5 | 24.8 | 4.7 | 8.2 | 16.3 | 20.6 | 79.6 |
| II-stage distillation aroma-showing substance | 5 | 25.3 | 4.9 | 8.5 | 16.7 | 20.9 | 81.3 |
Table 4 sensory test results with an application rate of 0.15%
| Sample (I) | Gloss of | Fragrance | Coordination of | Miscellaneous qi | Stimulation of | Aftertaste | Total up to |
| Reference cigarette | 5 | 24.1 | 4.0 | 7.9 | 15.0 | 20.0 | 76.0 |
| Aromatic tobacco extract | 5 | 24.6 | 4.7 | 7.9 | 15.4 | 20.2 | 77.8 |
| Maillard reactant of aromatic tobacco extract | 5 | 24.8 | 4.7 | 8.0 | 15.3 | 20.3 | 78.1 |
| II-stage distillation aroma-showing substance | 5 | 24.9 | 4.7 | 8.0 | 15.7 | 20.2 | 78.5 |
From the sensory evaluation results in tables 2-4, compared with Maillard reactants of tobacco flavor tobacco extracts and tobacco flavor tobacco extracts, the grade II distillation aroma-showing substances can improve the aroma quality and grade of cigarettes, increase the herbal aroma of the cigarettes, enable the smoke to be rich, sweet, mellow and pure, suppress the thorns and reduce impurities when being applied in a ratio of 0.05-0.1%, and enhance the aroma and the sweet return of the cigarettes when being used on low-tar cigarettes. The II-grade distillation aroma-displaying substance solves the problems of slight irritation, astringent feeling, slight miscellaneous gas, heavy smoke granular residue and smoke emission caused by applying the aromatic tobacco extract and the Maillard reaction product of the aromatic tobacco extract to the tobacco flavoring.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above examples, and any other modifications without departing from the scope of the present invention should be replaced by equivalents, and all such modifications are included in the scope of the present invention.
Claims (1)
1. The application of the tobacco additive in tobacco is characterized in that the tobacco additive is prepared by the following specific steps:
a. chopping aromatic tobacco, adding 50% ethanol into the aromatic tobacco according to the addition amount of 10mL of ethanol added into each gram of aromatic tobacco, extracting for 1-3 h at 65 ℃, filtering and concentrating until the density of relative water is 1.150-1.200 to obtain aromatic tobacco extract;
b. mixing the aromatic tobacco extract, glucose and proline in a mass ratio of 1: 0.3: 0.2, and continuously stirring for carrying out Maillard reaction for 4-6 hours at 100 ℃ to obtain an aromatic tobacco extract Maillard reactant;
c. b, adding the Maillard reactant of the aromatic tobacco extract obtained in the step b into a molecular distillation apparatus for I-stage distillation, setting the distillation temperature of the molecular distillation apparatus to be 60 ℃, the material flow rate to be 2ml/min, the film scraping rotation speed to be 60r/min and the vacuum degree to be 25Pa, and keeping I-stage distillate flowing out along the wall of the vacuum cavity;
d. c, continuously carrying out II-stage distillation on the I-stage distillate obtained in the step c in a molecular distillation instrument to obtain a light component and a heavy component, namely the tobacco additive; wherein the distillation temperature of the secondary distillation is set to be 75 ℃, the material flow rate is 1ml/min, the film scraping rotation speed is 120r/min, and the vacuum degree is 15 Pa;
collecting the II-grade distillation light component aroma-displaying substances, detecting that the density of the II-grade distillation light component aroma-displaying substances relative to water is 1.038, spraying the II-grade distillation light component aroma-displaying substances obtained by the method into the cut tobacco of the cigarette to prepare the medium-grade and high-grade cigarette, wherein the adding amount of the medium-grade and high-grade cigarette is 0.05-0.1% of the total weight of the cut tobacco.
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