CN112075657B - A kind of preparation method and application of tobacco stem extract - Google Patents

Abstract

The invention belongs to the technical field of cigarette production, and mainly relates to a preparation method and application of a tobacco stem extract, which comprises the following steps: crushing tobacco stems into stem powder, adding the stem powder into a reaction kettle, adding water, stirring and heating to a temperature; adding a compound enzyme preparation for enzymatic reaction; adding ethanol after the reaction is finished, refluxing and extracting, cooling and extruding, and reserving filtrate for later use; returning filter residue to the reaction kettle, adding ethanol into the filter residue, performing reflux extraction, cooling and squeezing, retaining filtrate, and discarding the filter residue; mixing the filtrates, centrifuging to obtain supernatant, adding propylene glycol into the supernatant, concentrating under reduced pressure, and transferring into a reaction kettle; stirring, heating in water bath or oil bath, adding amino compound and carbonyl compound, reflux reacting, and cooling to room temperature to obtain tobacco stem extract. The method greatly improves the smoking quality of the tobacco through substance conversion and impurity gas removal.

Description

A kind of preparation method and application of tobacco stem extract

technical field

The invention belongs to the technical field of cigarette production, and particularly relates to a preparation method and application of a tobacco stem extract.

Background technique

Tobacco stems are the thick and hard veins of tobacco leaves, accounting for about 25% to 30% of the weight of tobacco leaves, and are the main by-products of the tobacco industry. As a big tobacco producing country, about hundreds of thousands of tons of tobacco stem waste in my country is discarded without proper treatment every year. It not only pollutes the environment, but also wastes natural resources. Tobacco stems are the main raw material components of reconstituted tobacco leaves, and the manufacture of tobacco sheets is the main method for high-value utilization of tobacco stems. In the production process of paper-making tobacco sheet, the extraction and separation of raw materials is an important process step to ensure product yield, quality and cost. The tobacco stem extract obtained by the traditional process is mainly composed of macromolecules such as polysaccharides and proteins. Sugar will affect the burning speed and completeness of combustion. The amount of tar produced during the burning process is large, and the burning of protein will produce an odor like burning feathers. odor, and is a precursor of smoke harmful substances, including quinoline, HCN and other nitrogen-containing compounds. As a result, the tobacco sheet has poor taste quality, heavy air and other taste defects, which affects the use effect and addition amount of the sheet in cigarette industrial products.

Domestic and foreign studies have shown that through microbial fermentation, the green and miscellaneous gas of tobacco leaves can be significantly eliminated, the irritation can be reduced, and the aroma quality of tobacco leaves can be improved to a certain extent. The enzyme preparation can obviously degrade the protein, starch, cell wall substances and pectin in tobacco leaves and increase the aroma. The combination of the three techniques of the Maillard reaction is an important reaction to form the characteristic flavor of tobacco, and it is widely used in the synthesis of tobacco flavors. At present, the three technologies have been relatively maturely applied to the treatment of tobacco leaves, but either in a single form or in a combination of two forms, and there are almost no reports on the combination of the three technologies. However, it still has great limitations in the removal of miscellaneous gas or other negative substances.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a preparation method and application of tobacco stem extract, which are used to solve the problem of high-quality preparation of tobacco stem extract in the actual production process.

For realizing the above-mentioned technical purpose, the technical scheme adopted in the present invention is as follows:

A method for preparing tobacco stem extract, comprising the steps:

S1, pulverize the tobacco stems into 20-100 mesh ends, add them into the reaction kettle, add water according to 5-9 times the quality of the stem ends, stir and heat up to 40-80°C;

S2. After 10-50 minutes, the compound enzyme preparation with a mass fraction of 0.05-10% is added, and the enzymatic reaction is carried out for 2-8 hours;

S3, add 2-6 times of 80-95% ethanol of 5% ethyl stem powder quality after the reaction is finished, reflux extraction for 0.5-3 hours, extrude after cooling, and the filtrate is for use;

S4, the filter residue is returned to the reaction kettle, 20-60% ethanol of 2-8 times the quality of the end of the stem is added to the filter residue, refluxed for 1-4 hours, squeezed after cooling, the filtrate is retained, and the filter residue is discarded;

S5, merge the filtrate and centrifuge to get the supernatant, add the propylene glycol of 0.5-2 times the quality of the end of the stem in the supernatant, and transfer to the reactor after concentrating under reduced pressure;

S6, turn on stirring, heat the temperature of water bath or oil bath to 90-150°C, add 0.5-2% amino compound and 0.5-5% carbonyl compound of stem end quality respectively after 20 minutes, reflux reaction for 1-5 hours, cool to room temperature to obtain tobacco stem extract.

Further, the compound preparation in the step S2 is one or more of solid or liquid protease, amylase, pectinase, cellulase, glucanase, saccharification enzyme, glycosidase, and xylanase. A combination of species, the addition ratio is 0.1-5%.

Further, the S3 step is specifically implemented as follows:

After the reaction, add 90-95% ethanol with 3-5 times the mass of 5% ethyl stem powder, reflux for extraction for 1-2 hours, extrude after cooling, and use the filtrate for use.

Further, the specific implementation of the step S4 is as follows:

The filter residue is returned to the reaction kettle, 30-50% ethanol with 3-5 times the mass of the end of the stem is added to the filter residue, refluxed for 1-2 hours, and squeezed after cooling, the filtrate is retained, and the filter residue is discarded.

Further, the S6 step is specifically implemented as follows:

Turn on stirring, heat the temperature of water bath or oil bath to 95-105°C, add 0.5-1% amino compound and 0.5-3% carbonyl compound respectively after 20 minutes, reflux reaction for 2-4 hours, cool to room temperature , to obtain tobacco stem extract.

Further, in the step S6, the amino compound is a combination of one or more substances of protein, peptide, amine, ammonia and amino acid.

Further, in the step S6, the carboxyl compound is a combination of one or more substances of reducing sugar, lipid, aldehyde, ketone, polyphenol, ascorbic acid and steroid.

Further, the S2 step also includes the following steps:

Add titanium dioxide microsphere particles with a mass of 1:1 with the compounded enzyme preparation, and keep the pH value of the reaction solution in the range of 4.5-5.0;

The inside of the titanium dioxide microsphere particles has a hollow structure and is coated with suspendable activated carbon particles;

When 80-90% of the activated carbon particles in the titanium dioxide microsphere particles are suspended in the upper layer of the solution, all the activated carbon particles are filtered out from the reaction solution.

Titanium dioxide is a metal alkaline oxide. The main purpose of adding titanium dioxide in the present invention is that a large amount of acidic substances will be produced during the enzymatic hydrolysis of the organic matter during the enzymatic reaction, which will cause the reaction solution to become an acidic environment, thereby inhibiting the final effect of the enzymatic activity. If the reaction is not sufficient, the titanium dioxide particles can adjust the pH value of the solution to an appropriate range through the reaction to ensure a sufficient reaction.

At the same time, the titanium dioxide microsphere particles have a hollow structure inside and are coated with suspendable activated carbon particles. The activated carbon particles in this structure are mainly used for the adsorption and removal of wood gas or other impurities to further optimize the purity of the filtrate.

Further, the step S3 also includes the following steps:

After the titanium dioxide microsphere particles are added to the reaction solution, the solution is subjected to ultraviolet light irradiation treatment of 400-600 nm, and the treatment time is 2-5 hours.

In the present invention, by irradiating the reaction solution with ultraviolet light, the photocatalytic properties of the titanium dioxide particles are excited to realize the degradation of the polluting organic matter, and further realize the purification of the filtrate.

Use of the prepared tobacco stem extract for use in tobacco products.

By improving and optimizing the Maillard reaction, the present invention further improves the process reaction efficiency, improves the purity and quality of the tobacco stem extract, and enables the prepared tobacco product to have better quality.

Detailed ways

The present invention will be described in detail below with reference to specific embodiments.

A method for preparing tobacco stem extract, comprising the steps:

S1, pulverize the tobacco stems into 20-100 mesh ends, add them into the reaction kettle, add water according to 5-9 times the quality of the stem ends, stir and heat up to 40-80°C;

S2. After 10-50 minutes, the compound enzyme preparation with a mass fraction of 0.05-10% is added, and the enzymatic reaction is carried out for 2-8 hours;

S3, add 2-6 times of 80-95% ethanol of 5% ethyl stem powder quality after the reaction is finished, reflux extraction for 0.5-3 hours, extrude after cooling, and the filtrate is for use;

S4, the filter residue is returned to the reaction kettle, 20-60% ethanol of 2-8 times the quality of the end of the stem is added to the filter residue, refluxed for 1-4 hours, squeezed after cooling, the filtrate is retained, and the filter residue is discarded;

S5, merge the filtrate and centrifuge to get the supernatant, add the propylene glycol of 0.5-2 times the quality of the end of the stem in the supernatant, and transfer to the reactor after concentrating under reduced pressure;

S6, turn on stirring, heat the temperature of water bath or oil bath to 90-150°C, add 0.5-2% amino compound and 0.5-5% carbonyl compound of stem end quality respectively after 20 minutes, reflux reaction for 1-5 hours, cool to room temperature to obtain tobacco stem extract.

Example 1:

The dried tobacco stems were pulverized to 40 mesh, the end of the stems was weighed according to Table 1 and added to a 20L reactor, 10kg of water was added, stirring was started, the temperature was raised to 55°C, and the enzyme was added after 30 minutes.

According to Table 1, the enzyme preparation was weighed and added to the reaction kettle, and the reaction was carried out for 3.5 hours.

After the reaction, take out and add 6.5kg of 95% ethanol, and extract under reflux for 1.5 hours.

Cool and strain. The filtrate is used for later use, and the filter residue is returned to the reaction kettle.

7.0kg of 45% ethanol was added to the filter residue, and the mixture was refluxed for 1 hour.

Cool and strain. The filtrate was retained, and the filter residue was discarded.

The filtrates were combined, centrifuged, and the supernatant was taken.

1.8 kg of propylene glycol was added to the supernatant and concentrated under reduced pressure.

Transfer the concentrate into the reaction kettle, turn on stirring, heat the water bath to 96°C, and add materials according to Table 2 after 20 minutes. The reaction was refluxed for 3.5 hours.

Cool to room temperature to prepare YGMLD001.

Table 1 The amount of stem end and compound enzyme amount

Unit: g

Numbering end of stem Cellulase pectinase Xylanase amylase Glycosylase glucanase protease YGMLD001 1600 3.2 2.4 1.6 3.2 2.4 3.2 1.6

Table 2 Enzymatic hydrolysis time and consumption of amino compounds and carbonyl compounds

Unit: g

Numbering Alanine Xylose Vitamin C YGMLD001 10.6 18.6 0.9

Example 2:

To the above-prepared tobacco stem Maillard reaction product YGMLD01, add shredded tobacco according to 0.5% of the mass of the shredded tobacco, numbered TJ01, and add the same amount of distilled water to the blank control, numbered CK01. Cigarette sensory evaluation experts (9 people) with sensory evaluation qualifications were used to evaluate smoking according to the cigarette industry standard (the evaluation method for sensory comfort of cigarettes YC/T496-2014) (see Table 3 for the evaluation results).

Table 3 Sensory evaluation effect

It can be seen from Table 3 that the addition of the sample improves the perception of the oral cavity, nasal cavity, throat and smoke, and the roasted sweet aroma is more prominent and the intensity is increased.

Example 3:

The final products of Maillard reaction in tobacco stem (YGCK), Maillard reaction product (YGMLD), spiked sample (TJ) and blank control (CK) were determined by GC/MS gas chromatography.

Sample treatment: The Maillard reaction product was directly extracted with 40 mL of dichloromethane by shaking for 2 h. Take tobacco stems, cut tobacco samples and blank control samples and place them in an oven at 40°C for drying for 2 hours, pulverize, pass through a 40-mesh sieve, accurately weigh 25.0 g of tobacco powder samples (2 in parallel), and put them into the simultaneous distillation and extraction device at one end. In a 1000mL round-bottom flask, add 350mL saturated NaCl solution and a certain amount of internal standard compound (phenethyl acetate), and heat with an electric heating mantle; the other end of the device is a 100mL round-bottom flask containing 40mL of dichloromethane. Heated in a water bath at ℃ for 3 h while distilling extraction; after the direct extraction and distillation extraction were completed, an appropriate amount of anhydrous sodium sulfate was added to the extract and dried overnight; it was concentrated under reduced pressure to 1 mL at 40 ℃, and the concentrate was using Agilent7890B/5977BMSD GC/MS. The analysis was carried out with an analyzer, and the obtained chromatogram was searched and characterized by the computer spectral library (NIST14), and the relative content was calculated by the internal standard method.

GC/MS analysis conditions: chromatographic column is HP-5MS (30m×0.25mm×0.25μm) capillary column; carrier gas: He; flow rate: 1.0mL/min; inlet temperature: 250°C; heating program: 50°C Hold for 2 minutes, rise to 200°C at 3°C/min, hold for 2 minutes, then rise to 260°C at 6°C/min, hold for 5 minutes; injection volume 1.0 μL; split ratio: 10:1; interface temperature 280°C; solvent The delay time is 2min; the mass spectrum data acquisition speed is 5Hz; the ion source: EI source; the electron energy: 70eV; the ion source temperature: 230°C; the mass number range: 35-455amu.

The measurement results of aroma components are shown in Tables 4 and 5.

It can be seen from Table 4 that the Maillard reaction products of tobacco stems have a larger proportion of the small-molecule products of Maillard reaction than tobacco stems, with the lowest being 82.53% and the highest being 503.62.

It can be seen from Table 5 that after adding the stem Maillard reaction product to the cut tobacco, the proportion of the small-molecule products of the Maillard reaction also increased significantly, all reaching more than 20%, which is also consistent with the obvious increase in the roasted sweetness in the sensory evaluation.

Table 4 Maillard small molecule end product 1

YGCK(μg/g) YGMLD01(μg/g) Increase ratio (%) total acid 20.12 40.23 99.95 total aldehydes 30.23 55.18 82.53 total ketones 32.25 60.58 87.84 total amount of pyrazine 26.36 84.26 219.65 total amount of pyridines 19.36 60.35 211.73 Total amount of pyrroles 26.13 52.98 102.76 Total furans 11.87 71.65 503.62

Table 5 Maillard small molecule end product 2

The preparation method and application of the tobacco stem extract provided by the present invention are described in detail above. The description of the specific embodiment is only used to help understand the method and the core idea of the present invention. It should be pointed out that for those skilled in the art, without departing from the principle of the present invention, several improvements and modifications can also be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.

Claims (8)

1. A preparation method of a tobacco stem extract is characterized by comprising the following steps:

s1, crushing tobacco stems into stem powder of 20-100 meshes, adding the stem powder into a reaction kettle, adding water according to 5-9 times of the mass of the stem powder, stirring and heating to 40-80 ℃;

s2, adding 0.05-10% of compound enzyme preparation in percentage by mass after 10-50 minutes, and carrying out enzymatic reaction for 2-8 hours;

the step of S2 further includes the steps of: the mass of the added and compounded enzyme preparation is 1: 1, keeping the pH value of the reaction solution within the range of 4.5-5.0;

the interior of the titanium dioxide microsphere particles is of a hollow structure and is coated with suspensible activated carbon particles;

when 80-90% of the active carbon particles in the titanium dioxide microsphere particles are suspended and on the upper layer of the solution, all the active carbon particles are filtered from the reaction solution;

s3, adding 80-95% ethanol 2-6 times the mass of 5% of the stem powder of the Chinese wild cabbage after the reaction is finished, performing reflux extraction for 0.5-3 hours, cooling and extruding, and obtaining filtrate for later use;

the step of S3 further includes the steps of: after the reaction solution is added with titanium dioxide microsphere particles, the solution is subjected to 400-600nm ultraviolet irradiation treatment for 2-5 hours;

s4, returning filter residues to the reaction kettle, adding 20-60% ethanol with the mass 2-8 times that of the stems into the filter residues, performing reflux extraction for 1-4 hours, cooling, extruding, reserving filtrate, and discarding the filter residues;

s5, combining the filtrates, centrifuging to obtain supernatant, adding propylene glycol with the mass of 0.5-2 times of that of the stem powder into the supernatant, concentrating under reduced pressure, and transferring into a reaction kettle;

s6, starting stirring, heating to 90-150 ℃ in a hot water bath or oil bath, respectively adding 0.5-2% of amino compound and 0.5-5% of carbonyl compound by mass of stem powder after 20 minutes, carrying out reflux reaction for 1-5 hours, and cooling to room temperature to obtain the tobacco stem extract.

2. The method for preparing tobacco stem extract according to claim 1, wherein the compounded enzyme preparation in the step of S2 is one or more of solid or liquid protease, amylase, pectinase, cellulase, glucanase, glucoamylase, glycosidase and xylanase, and is added in a ratio of 0.1-5%.

3. The method for preparing the tobacco stem extract as claimed in claim 2, wherein the step of S3 is implemented as follows:

adding 90-95% ethanol 3-5 times the weight of 5% of the powder of the caulis et folium Chrysanthemi Segeti, reflux extracting for 1-2 hours, cooling, squeezing, and filtering to obtain filtrate.

4. The method for preparing tobacco stem extract according to claim 3, wherein the step S4 is realized as follows:

returning the filter residue to the reaction kettle, adding 30-50% ethanol with the mass of 3-5 times of the stem powder into the filter residue, reflux extracting for 1-2 hours, cooling, squeezing, reserving the filtrate, and discarding the filter residue.

5. The method for preparing the tobacco stem extract as claimed in claim 4, wherein the step of S6 is realized as follows:

stirring, heating to 95-105 deg.C with hot water bath or oil bath, adding amino compound 0.5-1% and carbonyl compound 0.5-3% of the weight of stem powder after 20 min, reflux reacting for 2-4 hr, and cooling to room temperature to obtain tobacco stem extract.

6. The method for preparing tobacco stem extract as claimed in claim 5, wherein the amino compound in step S6 is one or more of protein, peptide, amine, ammonia and amino acid.

7. The method for preparing tobacco stem extract as claimed in claim 6, wherein the carboxyl compound in step S6 is one or more of reducing sugar, lipid, aldehyde, ketone, polyphenol, ascorbic acid and steroid.

8. Use of a tobacco stem extract prepared according to the method of any one of claims 1 to 7 in a tobacco product.