CN112538401A - Preparation method of corn spice for cigarettes - Google Patents

Preparation method of corn spice for cigarettes Download PDF

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Publication number
CN112538401A
CN112538401A CN202011303305.1A CN202011303305A CN112538401A CN 112538401 A CN112538401 A CN 112538401A CN 202011303305 A CN202011303305 A CN 202011303305A CN 112538401 A CN112538401 A CN 112538401A
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corn
steep liquor
fermented
flavor
extract
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张婷婷
冯颖杰
杨宗灿
杨永锋
刘文召
王高杰
胡少东
张展
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China Tobacco Henan Industrial Co Ltd
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China Tobacco Henan Industrial Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B15/00Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
    • A24B15/18Treatment of tobacco products or tobacco substitutes
    • A24B15/28Treatment of tobacco products or tobacco substitutes by chemical substances
    • A24B15/30Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
    • A24B15/302Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Engineering & Computer Science (AREA)
  • Agronomy & Crop Science (AREA)
  • Botany (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

本发明公开了一种烟用玉米香料的制备方法,包括如下步骤:将玉米粒制浆后灭菌,得到玉米浆;将苏云金芽孢杆菌XC‑3接种至培养基中,得到淀粉降解菌种子液;将淀粉降解菌种子液接种至玉米浆中,发酵得到发酵玉米浆;根据有机溶剂和发酵玉米浆的体积质量比为(6‑10):1,混合后进行回流提取操作,得到玉米发酵提取物;对玉米发酵提取物减压浓缩至密度为1.15g/ml‑1.30g/ml,得到浓缩玉米提取物;根据乙醇和浓缩玉米提取物的体积质量比为(8‑12):1稀释,滤液减压浓缩至密度为1.15±0.005g/mL,即得到烟用玉米香料。本公开的烟用玉米香料不但在保留原料中香味物质成分前提下定向降解淀粉大分子,有效降低玉米提取物的刺激性,而且发酵产物中新的香味物质可提升烟用玉米香料的品质。The invention discloses a method for preparing corn flavor for tobacco, which comprises the following steps: sterilizing corn kernels to obtain corn steep liquor; inoculating Bacillus thuringiensis XC-3 into a culture medium to obtain a starch degrading bacteria seed liquid Inoculate the starch degrading bacteria seed liquid into the corn steep liquor, and ferment to obtain fermented corn steep liquor; according to the volume-to-mass ratio of the organic solvent and the fermented corn steep liquor (6-10): 1, carry out a reflux extraction operation after mixing to obtain the corn fermented extraction The corn fermented extract is concentrated under reduced pressure to a density of 1.15g/ml-1.30g/ml to obtain concentrated corn extract; according to the volume-to-mass ratio of ethanol and concentrated corn extract, it is (8-12): 1 dilution, The filtrate is concentrated under reduced pressure to a density of 1.15±0.005g/mL, thereby obtaining corn flavor for tobacco. The corn flavor for tobacco of the present disclosure not only directionally degrades starch macromolecules on the premise of retaining the flavor components in the raw material, and effectively reduces the irritation of the corn extract, but also the new flavor substances in the fermentation product can improve the quality of the corn flavor for tobacco.

Description

Preparation method of corn spice for cigarettes
Technical Field
The invention relates to the field of preparation of tobacco flavors, and in particular relates to a preparation method of a corn flavor for tobacco.
Background
In tobacco products, the aroma and mouthfeel of tobacco is of paramount importance. The cigarette flavor is a key link in the cigarette process and is one of effective means for improving the product style and the cigarette aroma quality, and the cigarette flavor is added to provide more aroma and cigarette products with satisfactory mouthfeel for consumers.
At present, most of tobacco flavors added in tobacco in China are prepared by adopting a traditional method, namely, the tobacco flavors are prepared by mixing natural extract monomers and synthetic monomers. The tobacco flavor prepared in the way has the defects of monotonous aroma and unobvious effect of improving the smoking quality of cigarettes although the preparation method is simple.
Corn is a gramineous plant, is an important food crop and feed source, and is the highest-yield food crop all over the world. The corn extract can be used as tobacco additive, and has effects of softening smoke, increasing aroma, and sweetening. However, the content of starch-based polysaccharide macromolecules in corn is as high as 60-73%, and the addition of the starch-based polysaccharide macromolecules to cigarettes can cause negative effects of increasing irritation.
Therefore, how to provide a method capable of effectively reducing the irritation of the corn extract becomes a technical problem to be solved in the field.
Disclosure of Invention
The invention aims to provide a novel technical scheme of a preparation method of a corn flavor for cigarettes, which can effectively reduce the irritation of a corn extract.
According to the first aspect of the invention, a preparation method of corn flavor for tobacco is provided.
The preparation method of the corn flavor for the cigarettes comprises the following steps:
step (1): pulping corn kernels and then sterilizing to obtain corn steep liquor;
step (2): inoculating bacillus thuringiensis XC-3 into a culture medium to obtain a starch degrading bacterium seed solution;
and (3): inoculating the starch degrading bacteria seed liquid into corn steep liquor, and fermenting for 2d-5d at 35-40 ℃ to obtain fermented corn steep liquor;
and (4): mixing the organic solvent and the fermented corn steep liquor according to the volume-mass ratio of (6-10) to 1, and performing reflux extraction operation to obtain a corn fermented extract, wherein the volume of the organic solvent is mL, and the mass of the fermented corn steep liquor is g;
and (5): concentrating the supernatant after centrifuging the corn fermentation extract under reduced pressure to a density of 1.15g/ml-1.30g/ml to obtain a concentrated corn extract;
and (6): diluting the concentrated corn extract according to the volume-mass ratio of ethanol to the concentrated corn extract (8-12):1, and concentrating the filtered filtrate under reduced pressure to the density of 1.15 +/-0.005 g/mL to obtain the corn flavor for cigarettes, wherein the volume of ethanol is mL, and the mass of the concentrated corn extract is g.
Optionally, the step (1) is specifically as follows:
cleaning corn kernels, mixing and pulping the corn kernels and water according to the mass ratio of the corn kernels to the water of 1 (10-20), sterilizing at 120 ℃ for 15min, and cooling to room temperature to obtain corn steep liquor.
Optionally, the step (2) is specifically as follows:
inoculating Bacillus thuringiensis XC-3 into a culture medium, and performing shake culture at 37 ℃ and 150rpm for 24h to obtain a starch degrading bacteria seed solution.
Optionally, the culture medium in the step (2) is LB culture medium cooled after being autoclaved at 120 ℃ for 15 min.
Optionally, the step (3) is specifically as follows:
inoculating the starch degrading bacteria seed liquid into the corn steep liquor according to the volume ratio of the starch degrading bacteria seed liquid to the corn steep liquor of (2-5) to 100, and fermenting for 2d-5d at 35-40 ℃ to obtain the fermented corn steep liquor.
Optionally, the organic solvent in the step (4) is isopropanol.
Optionally, the step (4) is specifically as follows:
mixing the organic solvent and the fermented corn steep liquor according to the volume-mass ratio of (6-10) to 1, and performing reflux extraction at 85 ℃ for 2-4 h to obtain a corn fermented extract, wherein the volume of the organic solvent is mL, and the mass of the fermented corn steep liquor is g.
Optionally, the reflux extraction in the step (4) is repeated for 3 times, and the 3 times of extracting solutions are combined to obtain the corn fermentation extract.
Optionally, the ethanol in the step (6) is 95% ethanol.
Optionally, the volume-to-mass ratio of the ethanol to the concentrated corn extract in the step (6) is 10: 1.
According to the corn spice for the cigarette, the corn steep liquor is fermented by the starch degrading bacteria, starch macromolecules are directionally degraded on the premise of keeping the components of the fragrant substances in the raw materials, the irritation of the corn extract is effectively reduced, and the quality of the corn spice for the cigarette can be improved by the new fragrant substances in the fermentation product.
Detailed Description
Various exemplary embodiments of the present invention will now be described in detail. It should be noted that: the relative arrangement of the components and steps, the numerical expressions and numerical values set forth in these embodiments do not limit the scope of the present invention unless specifically stated otherwise.
The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses.
Techniques, methods, and apparatus known to those of ordinary skill in the relevant art may not be discussed in detail but are intended to be part of the specification where appropriate.
In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The preparation method of the corn flavor for the cigarettes comprises the following steps:
step (1): and (4) pulping the corn kernels and then sterilizing to obtain corn steep liquor.
The step (1) may be specifically as follows:
cleaning corn kernels, mixing and pulping the corn kernels and water according to the mass ratio of the corn kernels to the water of 1 (10-20), sterilizing at 120 ℃ for 15min, and cooling to room temperature to obtain corn steep liquor. The room temperature may be, for example, 20 ℃ to 25 ℃.
Step (2): inoculating bacillus thuringiensis XC-3 into a culture medium to obtain a starch degrading bacterium seed solution. The Bacillus thuringiensis XC-3 is XC-3 strain for degrading starch in tobacco leaves, belongs to Bacillus and has a preservation name as follows: the Bacillus thuringiensis XC-3 is classified as Bacillus thuringiensis XC-3, is preserved in the Wuhan Chinese type culture collection in 2017, 6 months and 30 days, and has the preservation number of CCTCC NO: m2017352.
The step (2) may be specifically as follows:
inoculating Bacillus thuringiensis XC-3 into a culture medium, and performing shake culture at 37 ℃ and 150rpm for 24h to obtain a starch degrading bacteria seed solution.
Further, the medium in the step (2) was LB medium (Luria-Bertani medium) cooled after autoclaving at 120 ℃ for 15 min.
And (3): inoculating the starch degrading bacteria seed liquid into corn steep liquor, and fermenting for 2d-5d at 35-40 ℃ to obtain fermented corn steep liquor.
The step (3) may be embodied as follows:
inoculating the starch degrading bacteria seed liquid into the corn steep liquor according to the volume ratio of the starch degrading bacteria seed liquid to the corn steep liquor of (2-5) to 100, and fermenting for 2d-5d at 35-40 ℃ to obtain the fermented corn steep liquor.
And (4): mixing the organic solvent and the fermented corn steep liquor according to the volume-mass ratio of (6-10):1, and performing reflux extraction to obtain the corn fermented extract, wherein the volume of the organic solvent is mL, and the mass of the fermented corn steep liquor is g.
The organic solvent in step (4) may be isopropanol.
The step (4) may be embodied as follows:
mixing the organic solvent and the fermented corn steep liquor according to the volume-mass ratio of (6-10) to 1, and performing reflux extraction at 85 ℃ for 2-4 h to obtain a corn fermented extract, wherein the volume of the organic solvent is mL, and the mass of the fermented corn steep liquor is g.
Further, in order to improve the quality of the corn flavor for the cigarettes, the reflux extraction in the step (4) is repeated for 3 times, and the 3 extracting solutions are combined to obtain the corn fermentation extract.
And (5): concentrating the supernatant of the corn fermentation extract after centrifugation to a density of 1.15g/ml-1.30g/ml under reduced pressure to obtain the concentrated corn extract.
And (6): diluting the concentrated corn extract according to the volume-mass ratio of ethanol to the concentrated corn extract (8-12):1, and concentrating the filtered filtrate under reduced pressure to the density of 1.15 +/-0.005 g/mL to obtain the corn flavor for cigarettes, wherein the volume of ethanol is mL, and the mass of the concentrated corn extract is g. The ethanol can be 95% ethanol by volume or 75% ethanol by volume.
The ethanol in step (6) may be 95% ethanol.
In order to improve the quality of the corn flavor for cigarettes, the volume-to-mass ratio of the ethanol to the concentrated corn extract in the step (6) is 10: 1.
The experimental procedures used in the examples below are conventional unless otherwise specified, the materials and reagents used therein are commercially available, and the equipment used in the experiments are well known to those skilled in the art without otherwise specified.
Example 1
1. Sterilizing LB culture medium at 120 deg.C under high pressure for 15min, inoculating starch degrading bacteria (Bacillus thuringiensis XC-3) into the sterilized and cooled culture medium, and culturing at 37 deg.C and 150rpm for 24h to obtain starch degrading bacteria seed solution.
2. Cleaning corn kernels, pulping according to the mass ratio of the corn kernels to water of 1:15, sterilizing at 120 ℃ for 15min, and cooling to room temperature to obtain corn steep liquor.
3. Inoculating the starch degrading bacteria seed liquid to the corn steep liquor according to the volume ratio of the starch degrading bacteria seed liquid to the corn steep liquor of 3:100, and fermenting for 4d at 37 ℃ to obtain the fermented corn steep liquor.
4. According to the volume-to-mass ratio of the isopropanol to the fermented corn steep liquor of 6:1, uniformly mixing the isopropanol and the fermented corn steep liquor, setting the temperature to 85 ℃ for reflux extraction for 2 hours, repeating reflux extraction for 3 times, and combining the 3 times of extracting solutions to obtain the corn fermented extract.
5. Centrifuging the fermented corn extract, collecting supernatant, and concentrating under reduced pressure to density of 1.20g/ml to obtain concentrated corn extract.
6. Diluting the concentrated corn extract according to the volume-to-mass ratio of 95% ethanol (mL) to the concentrated corn extract (g) of 10:1, performing suction filtration, and concentrating under reduced pressure to obtain the corn flavor for cigarettes, which is recorded as T1, with the density of 1.15 +/-0.005 g/mL.
Comparative example 1
1. Cleaning corn kernels, pulping according to the mass ratio of the corn kernels to water of 1:15, sterilizing at 120 ℃ for 15min, and cooling to room temperature to obtain corn steep liquor.
2. According to the volume-to-mass ratio of the isopropanol to the corn steep liquor of 6:1, uniformly mixing the isopropanol and the corn steep liquor, setting the temperature to 85 ℃, performing reflux extraction for 2 hours, repeating reflux extraction for 3 times, and combining the 3 times of extracting solutions to obtain the corn extract.
3. Centrifuging semen Maydis extract to obtain supernatant, and concentrating under reduced pressure to density of 1.20g/ml to obtain concentrated semen Maydis extract.
4. Diluting the concentrated corn extract according to the volume-to-mass ratio of 95% ethanol (mL) to the concentrated corn extract (g) of 10:1, performing suction filtration, and concentrating under reduced pressure to obtain the corn flavor for cigarettes, which is recorded as T0, with the density of 1.15 +/-0.005 g/mL.
Conventional chemical components of the corn steep liquor before and after fermentation are detected, and main aroma substance components of T1 and T0 are detected.
Table 1 shows the results of conventional chemical compositions of corn steep liquor before and after fermentation. As can be seen from Table 1, after the fermentation by the starch degrading bacteria, the content of starch and protein in the corn steep liquor is reduced, and the content of total sugar, reducing sugar and amino acid is increased, which indicates that the starch is degraded into soluble sugar in the fermentation process, so that the content of total sugar and reducing sugar is increased, and protein substances are degraded into amino acid in the process.
TABLE 1 content of conventional chemical components of corn steep liquor before and after fermentation (unit: mg/mL)
Sample (I) Amino acids Total sugar Reducing sugar Starch Protein
Before fermentation 8.13 172.78 120.32 630.21 7.75
After fermentation 12.67 326.52 238.55 380.45 3.11
Table 2 shows the main aroma components of T1 and T0. As can be seen from Table 2, after fermentation by starch degrading bacteria, the contents of various flavor substances of the corn flavor for tobacco are all obviously improved, which shows that the tobacco flavor prepared by fermented corn steep liquor can reduce the content of macromolecular substances, and the macromolecular substances are converted into flavor substances, thereby being beneficial to reducing the irritation of the flavor, and further effectively improving the quality of the corn flavor for tobacco.
TABLE 2 analysis of the main aroma components in corn extract (content. mu.g/mL)
Sample (I) Alcohol(s) Acids (acids) Aldehyde ketones Esters and lactones Phenols Heterocycles Total of
T0 52.83 535.51 214.63 59.34 20.52 152.28 1035.66
T1 97.24 818.68 363.87 105.76 32.57 253.64 1671.76
Although some specific embodiments of the present invention have been described in detail by way of examples, it should be understood by those skilled in the art that the above examples are for illustrative purposes only and are not intended to limit the scope of the present invention. It will be appreciated by those skilled in the art that modifications may be made to the above embodiments without departing from the scope and spirit of the invention. The scope of the invention is defined by the appended claims.

Claims (10)

1.一种烟用玉米香料的制备方法,其特征在于,包括如下步骤:1. a preparation method of corn spice for tobacco, is characterized in that, comprises the steps: 步骤(1):将玉米粒制浆后灭菌,得到玉米浆;Step (1): sterilize the corn kernels after pulping to obtain corn steep liquor; 步骤(2):将苏云金芽孢杆菌XC-3接种至培养基中,得到淀粉降解菌种子液;Step (2): inoculate Bacillus thuringiensis XC-3 into the culture medium to obtain starch degrading bacteria seed solution; 步骤(3):将淀粉降解菌种子液接种至玉米浆中,在35℃-40℃下发酵2d-5d,得到发酵玉米浆;Step (3): inoculate the starch-degrading bacteria seed liquid into corn steep liquor, and ferment at 35°C-40°C for 2d-5d to obtain fermented corn steep liquor; 步骤(4):根据有机溶剂和发酵玉米浆的体积质量比为(6-10):1,将有机溶剂和发酵玉米浆混合后进行回流提取操作,得到玉米发酵提取物,其中,有机溶剂的体积的单位为mL,发酵玉米浆的质量的单位为g;Step (4): according to the volume-to-mass ratio of the organic solvent and the fermented corn steep liquor is (6-10): 1, after the organic solvent and the fermented corn steep liquor are mixed, a reflux extraction operation is carried out to obtain a corn fermented extract, wherein the The unit of volume is mL, and the unit of mass of fermented corn steep liquor is g; 步骤(5):对玉米发酵提取物离心后的上清液减压浓缩至密度为1.15g/ml-1.30g/ml,得到浓缩玉米提取物;Step (5): the supernatant after the centrifugation of the corn fermented extract is concentrated under reduced pressure to a density of 1.15g/ml-1.30g/ml to obtain a concentrated corn extract; 步骤(6):根据乙醇和浓缩玉米提取物的体积质量比为(8-12):1稀释浓缩玉米提取物,过滤后的滤液减压浓缩至密度为1.15±0.005g/mL,即得到烟用玉米香料,其中,乙醇的体积的单位为mL,浓缩玉米提取物的质量的单位为g。Step (6): according to the volume mass ratio of ethanol and concentrated corn extract, it is (8-12): 1 diluted concentrated corn extract, and the filtered filtrate is concentrated under reduced pressure to a density of 1.15 ± 0.005g/mL, to obtain smoke. With corn flavor, the unit of volume of ethanol is mL, and the unit of mass of concentrated corn extract is g. 2.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(1)具体如下:2. the preparation method of corn flavor for tobacco according to claim 1, is characterized in that, described step (1) is as follows: 将玉米粒洗净,根据玉米粒和水的质量比为1:(10-20)将玉米粒和水混合打浆,在120℃条件下灭菌15min,冷却至室温,得到玉米浆。Wash the corn kernels, mix and beat the corn kernels and water according to the mass ratio of corn kernels and water as 1:(10-20), sterilize at 120° C. for 15 minutes, and cool to room temperature to obtain corn steep liquor. 3.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(2)具体如下:3. the preparation method of corn flavor for tobacco according to claim 1, is characterized in that, described step (2) is as follows: 将苏云金芽孢杆菌XC-3接种至培养基中,在37℃和150rpm的条件下振荡培养24h,得到淀粉降解菌种子液。Bacillus thuringiensis XC-3 was inoculated into the medium, and cultured with shaking at 37° C. and 150 rpm for 24 hours to obtain the seed liquid of starch degrading bacteria. 4.根据权利要求3所述的烟用玉米香料的制备方法,其特征在于,所述步骤(2)中的培养基为在120℃下高压灭菌15min后冷却的LB培养基。4. The preparation method of corn flavor for tobacco according to claim 3, wherein the medium in the step (2) is the LB medium cooled after autoclaving at 120° C. for 15 min. 5.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(3)具体如下:5. the preparation method of corn flavor for tobacco according to claim 1, is characterized in that, described step (3) is as follows: 根据淀粉降解菌种子液和玉米浆的体积比为(2-5):100将淀粉降解菌种子液接种至玉米浆中,在35℃-40℃下发酵2d-5d,得到发酵玉米浆。According to the volume ratio of starch degrading bacteria seed liquid and corn steep liquor (2-5):100, the starch degrading bacteria seed liquid was inoculated into corn steep liquor, and fermented at 35°C-40°C for 2d-5d to obtain fermented corn steep liquor. 6.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(4)中的有机溶剂为异丙醇。6. the preparation method of corn flavor for tobacco according to claim 1, is characterized in that, the organic solvent in described step (4) is isopropanol. 7.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(4)具体如下:7. the preparation method of corn flavor for tobacco according to claim 1, is characterized in that, described step (4) is as follows: 根据有机溶剂和发酵玉米浆的体积质量比为(6-10):1,将有机溶剂和发酵玉米浆混合后在85℃下回流提取2h-4h,得到玉米发酵提取物,其中,有机溶剂的体积的单位为mL,发酵玉米浆的质量的单位为g。According to the volume-to-mass ratio of the organic solvent and the fermented corn steep liquor (6-10): 1, the organic solvent and the fermented corn steep liquor were mixed and then refluxed and extracted at 85°C for 2h-4h to obtain the corn fermented extract. The unit of volume is mL, and the unit of mass of fermented corn steep liquor is g. 8.根据权利要求7所述的烟用玉米香料的制备方法,其特征在于,所述步骤(4)中的回流提取重复3次,并将3次提取液合并,得到玉米发酵提取物。8 . The preparation method of corn flavor for tobacco according to claim 7 , wherein the reflux extraction in the step (4) is repeated 3 times, and the 3 extractions are combined to obtain the corn fermented extract. 9 . 9.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(6)中的乙醇为95%乙醇。9. The preparation method of corn flavor for tobacco according to claim 1, wherein the ethanol in the step (6) is 95% ethanol. 10.根据权利要求1所述的烟用玉米香料的制备方法,其特征在于,所述步骤(6)中乙醇和浓缩玉米提取物的体积质量比为10:1。10. The preparation method of corn flavor for cigarettes according to claim 1, characterized in that, in the step (6), the volume-to-mass ratio of ethanol and concentrated corn extract is 10:1.
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