CN116042315A - Yellow Jiang Huaxiang material, preparation method thereof and application thereof in tobacco products - Google Patents

Yellow Jiang Huaxiang material, preparation method thereof and application thereof in tobacco products Download PDF

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Publication number
CN116042315A
CN116042315A CN202211667929.0A CN202211667929A CN116042315A CN 116042315 A CN116042315 A CN 116042315A CN 202211667929 A CN202211667929 A CN 202211667929A CN 116042315 A CN116042315 A CN 116042315A
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membrane
stage
turmeric
extract
jiang
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Inventor
张文娟
杨春强
杨国涛
杨伟平
徐秀娟
马骥
何保江
范武
霍现宽
姬凌波
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Zhengzhou Tobacco Research Institute of CNTC
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Zhengzhou Tobacco Research Institute of CNTC
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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
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58Multistep processes

Abstract

The invention relates to a yellow Jiang Huaxiang material, a preparation method thereof and application thereof in tobacco products, and belongs to the technical field of tobacco processing. (1) Leaching the crushed or crushed turmeric flower with ethanol solution, and carrying out solid-liquid separation to obtain ethanol extract; (2) Carrying out multistage membrane separation on the alcohol extract by adopting an organic membrane and/or a ceramic membrane, and carrying out step-by-step separation according to the pore diameter of the membrane from large to small to obtain all-grade trapped fluid or part-grade trapped fluid, thereby obtaining yellow Jiang Huachun extract; the molecular weight cut-off of the organic membrane is from 3000Da to 200000Da, and the membrane pore diameter of the ceramic membrane is from 5nm to 200nm. According to the preparation method of the turmeric flower spice, the crushed turmeric flowers are leached by ethanol solution and then subjected to multistage membrane separation for fine separation, so that the ethanol extract separated matters with different aroma dimensions of the focused turmeric flowers are obtained as the primarily extracted spice, and base liquid is provided for further obtaining homologous refined products such as yellow Jiang Huachun refined matters, turmeric flower essential oil, yellow Jiang Huashui refined liquid and the like.

Description

Yellow Jiang Huaxiang material, preparation method thereof and application thereof in tobacco products
Technical Field
The invention relates to a yellow Jiang Huaxiang material, a preparation method thereof and application thereof in tobacco products, and belongs to the technical field of tobacco processing.
Background
Huang Jianghua (Hedychium flavum Roxb.) is perennial herb-like fragrant flower of Zingiberaceae, and has rich fragrance, pure sweetness, and good taste, and is used for fresh cut flower and garden greening. The flower mainly contains aroma components such as 1, 8-eucalyptol, linalool, beta-caryophyllene, nerolidol and the like. Although the extract extracted from Huang Jianghua is mentioned in the literature as a high-grade flavoring material, there are few reports of specific preparation processes.
Huang Jianghua natural perfume components are complex, and all the perfume components overlap with each other, so that the preparation of high-quality perfume products is difficult, and the aim of industrially preparing perfumes with obvious characteristic flavors of turmeric flowers is more rare in the prior art. In addition, the flavor extracted by Huang Jianghua is used for processing tobacco products, so that the richness and the comfort level of smoke during smoking can be improved, and brand new feeling and experience are brought to consumers.
Disclosure of Invention
The invention aims to provide a preparation method of a turmeric flower spice, which solves the problems of complex ingredients, insufficient focusing of product flavor and difficult preparation of high-quality spice in the prior art.
The second object of the invention is to provide the turmeric flower spice prepared by the preparation method.
The third purpose of the invention is to provide an application of the turmeric flower spice in tobacco products, and in order to develop the special spice which can highlight the flavor of yellow Jiang Huaxiang and is suitable for various flavoring modes of the tobacco products.
In order to achieve the above purpose, the preparation method of the turmeric flower spice adopts the following technical scheme:
(1) Leaching the crushed or crushed turmeric flower with ethanol solution, and carrying out solid-liquid separation to obtain ethanol extract;
(2) Carrying out multistage membrane separation on the alcohol extract by adopting an organic membrane and/or a ceramic membrane, and carrying out step-by-step separation according to the pore diameter of the membrane from large to small to obtain all-grade trapped fluid or part-grade trapped fluid, thereby obtaining yellow Jiang Huachun extract; the molecular weight cut-off of the organic membrane is from 3000Da to 200000Da, and the membrane pore diameter of the ceramic membrane is from 5nm to 200nm.
Wherein the turmeric flower in the step (1) can be fresh flowers, dried flowers or a combination thereof.
The multistage membrane separation in the step (2) can be carried out by using an organic membrane or a ceramic membrane alone or by combining the two membranes alternately, but the separation from large to small membrane pore size is followed.
According to the preparation method of the turmeric flower spice, the smashed turmeric flowers are leached by ethanol solution, and then the ethanol extract is subjected to multistage membrane separation for fine separation, so that the ethanol extract separated matters with different aroma dimensions of the focused turmeric flowers are obtained as the spice which is primarily extracted by yellow Jiang Huaxiang material, and base liquid is provided for further obtaining homologous refined products such as yellow Jiang Huachun refined matters, turmeric flower essential oil, yellow Jiang Huashui refined liquid and the like. The preparation method provided by the invention is simple and easy to operate, low in cost, high in added value of products and suitable for large-scale production and application.
In the preparation method of the turmeric flower spice, the solid-liquid separation can adopt conventional means such as centrifugation, filtration, standing and the like, and the solid-liquid separation means of filtration is optimized and selected for improving the separation efficiency.
In the preparation method of the turmeric flower spice, the multi-stage membrane separation refers to the sequential use of membrane components or membrane equipment with large-to-small pore diameters, wherein the permeate of each stage of membrane separation is used as the raw material for the separation of the next stage of membrane, and each stage of membrane can intercept substances with different molecular weights. As a further optimized scheme, three-to-six-stage membrane separation can be adopted, taking four-stage membrane separation as an example, wherein the first-stage membrane is a ceramic membrane with the aperture of 50-200 nm, the second-stage membrane is a ceramic membrane with the aperture of 15-20 nm or an organic membrane with the molecular weight cutoff of 80000-200000 Da, the third-stage membrane is a ceramic membrane with the aperture of 5-10 nm or an organic membrane with the molecular weight cutoff of 10000-20000 Da, and the fourth-stage membrane is an organic membrane with the molecular weight cutoff of 3000-5000 Da.
According to the preparation method of the turmeric flower spice, based on obtaining the turmeric Jiang Huachun extract spice, the preparation method is further optimized, so that the flavor style of the turmeric flower spice is more abundant and natural, and the turmeric Jiang Huachun extract is obtained. In order to better highlight the flavor of Huang Jianghua, sensory evaluation is carried out, the membrane separation component is recombined, the essence is taken to remove the dregs, and preferably, the trapped liquid of the first-stage membrane, the third-stage membrane and the fourth-stage membrane in the Huang Jianghua alcohol extraction separation is compounded to obtain the yellow Jiang Huachun extract.
It is further preferred that the retentate of the first, third and fourth stage membranes is reconstituted at a dry matter mass ratio of (10-12): 5-6): 1.
According to the preparation method of the turmeric flower spice, on the basis of obtaining the turmeric Jiang Huachun refined spice, the final-stage permeate of membrane separation is subjected to post-treatment to obtain the turmeric flower essential oil spice which is the most valuable in turmeric flowers. Preferably, the method further comprises the following steps: concentrating the membrane separation final-stage permeate in the step (2), removing the solvent, then carrying out molecular distillation at the temperature of 40-70 ℃, and collecting light components to obtain the turmeric essential oil.
Preferably, the molecular distillation is carried out at a pressure of from 0.01 to 0.1mbar.
According to the preparation method of the turmeric flower spice, yellow Jiang Huachun extract and separation products showing different aroma dimensions of turmeric flowers are firstly obtained as basic spice, and then yellow Jiang Huachun extract and separation product spice with rich natural yellow Jiang Huaxiang gas flavor and turmeric flower essential oil with high added value are further obtained. On the basis, in order to maximize the resource utilization of the turmeric flower raw material and improve the economic value, yellow Jiang Hualiao slag leached by ethanol solution is used, and the fragrant substances in the yellow Jiang Hualiao slag are further extracted by water. Preferably, the preparation method further comprises the following steps:
a. soaking and extracting the slag obtained by the solid-liquid separation in the step (1) with water, and performing solid-liquid separation to obtain water extract;
b. performing multistage membrane separation on the water extract by adopting a ceramic membrane and/or an organic membrane, and performing stepwise separation according to the pore diameter of the membrane from large to small to obtain all-grade trapped fluid and final-grade permeate, thereby obtaining yellow Jiang Huashui extract; the membrane aperture of the ceramic membrane is from 5 to 200nm, and the molecular weight cut-off of the organic membrane is from 10000 to 200000Da.
As a further optimized scheme, three-to-six-stage membrane separation can be adopted, taking three-stage membrane separation as an example, wherein the first-stage membrane is a ceramic membrane with the aperture of 200nm, the second-stage membrane is a ceramic membrane with the aperture of 15-20 nm or an organic membrane with the molecular weight cutoff of 80000-200000 Da, and the third-stage membrane is a ceramic membrane with the aperture of 5-10 nm or an organic membrane with the molecular weight cutoff of 10000-20000 Da.
In order to better show the flavor of Huang Jianghua after water extraction, preferably, the dry matter mass ratio of the second-stage membrane, the interception liquid of the third-stage membrane and the penetrating liquid of the third-stage membrane in the yellow ginger flower water extraction separation product is (8-10): 1 (15-20) is compounded to obtain yellow Jiang Huashui refined liquid.
In order to save cost while ensuring maximum extraction of floral components, preferably the concentration of the ethanol solution is 75-95% (V/V); the mass ratio of the leached liquid in the step (1) is 1:4-15.
Further, when the fresh turmeric flower is used as a raw material, the mass ratio of the feed liquid is 1:6-10; when the dried yellow ginger flowers are used as raw materials, the mass ratio of the feed liquid is 1:4-15.
In order to improve the leaching efficiency of the ethanol solution, preferably, the leaching is performed under the condition of heating to 60-80 ℃ for 2-6 h. Further preferably, each time of leaching is carried out for 1-2 hours, leaching is carried out for 2-3 times, and the extracting solutions are combined for a plurality of times to obtain an alcohol extracting solution.
In order to increase the contact area between water and slag and achieve better extraction effect, preferably, the mass ratio of the water extracted feed liquid in the step a is 1:5-15.
Preferably, the water extraction is carried out under the condition of heating at 70-90 ℃ for 1-7 h. Further preferably, the water is used for extraction for 1 to 2 times, each time for 1 to 3 hours, and the water extract is obtained by combining the plurality of times of extraction.
The invention adopts the technical scheme that:
the turmeric flower spice is prepared by the method.
The turmeric flower spice disclosed by the invention is prepared by treating the same raw material by using a preparation method, so that 3 or 4 turmeric flower spices are obtained, the spices fully highlight the fragrance style of turmeric flowers from different dimensions, and the requirements of flavoring different tobacco products can be met. Meanwhile, the diversity of homologous natural perfume products is improved, the characteristic natural perfume with focused functions and multiple components is obtained, and high-quality perfume is provided for accurate perfume mixing and digital product design.
The application of the turmeric flower spice adopts the technical scheme that:
the use of a turmeric flower flavoring in a tobacco product, which is a conventional cigarette, a heated non-combustible cigarette, or a tube cigarette.
Detailed Description
The technical scheme of the invention is further described below with reference to the specific embodiments.
1. The yellow Jiang Huaxiang material and the preparation method thereof of the invention are as follows:
example 1
The preparation method of the turmeric flower spice in the embodiment comprises the following steps:
s1, raw material treatment: taking fresh flowers of turmeric as a raw material, removing impurities and crushing.
S2, ethanol extraction: heating and extracting with 95% (V/V) ethanol solution for 2 times at 60deg.C at a mass ratio of 1:10 for 2 hr, filtering to obtain extractive solution, and extracting residues for the second time; extracting for 1h with the mass ratio of the feed liquid of the second extraction being 1:6, and filtering after the extraction is finished to obtain an extracting solution; mixing the two extractive solutions to obtain yellow Jiang Huachun extractive solution.
S3, multistage membrane separation of alcohol extract: separating the supernatant by high-speed centrifugation of Huang Jianghua ethanol extract, namely a first-stage membrane, namely a ceramic membrane with the aperture of 50nm, and respectively collecting first-stage trapped fluid and permeate; the first-stage permeate is further passed through a second-stage membrane, namely a coiled organic membrane with the molecular weight cut-off of 80000Da, and the second-stage cut-off and the permeate are respectively collected; then the second-stage permeate is further passed through a third-stage membrane, namely a coiled organic membrane with the molecular weight cutoff of 20000Da, and the third-stage retentate and the permeate are respectively collected; then the third-stage permeate is further passed through a fourth-stage membrane, namely a coiled organic membrane with a molecular weight cutoff of 5000Da, and the fourth-stage retentate and the permeate are respectively collected; obtaining all levels of components separated by the alcohol extract membrane, namely yellow Jiang Huachun extract.
S4, recombining and compounding alcohol extract membrane separation components: and (3) selecting the first-stage trapped fluid, the third-stage trapped fluid and the fourth-stage trapped fluid for compounding, namely mixing and compounding the 50nm trapped fluid, the 20000Da trapped fluid and the 5000Da trapped fluid according to a dry matter mass ratio of 10:5:1 to obtain the yellow Jiang Huachun refined product.
The three trapped fluids and the proportion thereof are obtained by sensory evaluation, and the specific operation process is as follows: the solvent content of 8 membrane separation components, namely 50nm trapped fluid, permeate fluid, 80000Da trapped fluid, permeate fluid, 20000Da trapped fluid, permeate fluid, 5000Da trapped fluid and permeate fluid, is measured by adopting a standard method, and the mass fractions of the dry matters are calculated. The dry mass fractions of the component solutions were adjusted to be the same with 90% ethanol. And (3) respectively injecting the solutions with the same mass fractions of the dry matters into blank cigarettes without flavoring by adopting a cigarette flavoring injector, wherein the injection quantity of each solution is equal, and then carrying out comparative evaluation on the sample cigarettes by a professional cigarette sensory evaluation personnel. The evaluation results are as follows: after the 50nm trapped fluid, the 20000Da trapped fluid and the 5000Da trapped fluid are applied to cigarettes, different dimensions of yellow Jiang Huaxiang gas styles can be well reflected, the tobacco fragrance is enriched, and the quality of the cigarettes is improved. In addition, the 5000Da permeation solution is rich in volatile aroma components, and has good sensory effect. In order to further obtain essential oil products with higher added values, 5000Da permeate is not added during the recombination and compounding of the alcohol extract membrane separation components. The specific evaluation results are shown in Table 1.
TABLE 1 sensory impact score of yellow Jiang Huachun extract film separation component and alcohol extract concentrate applied to blank cigarettes
Figure SMS_1
S5, preparing essential oil by molecular distillation: distilling the yellow Jiang Huachun extractive solution with 5000Da membrane separation membrane under reduced pressure to remove volatile solvent, separating concentrate with molecular distillation instrument at 70deg.C under 0.1mbar, and collecting light component to obtain Curcuma rhizome essential oil.
S6, extracting slag with water: and (2) further heating and extracting the yellow Jiang Hualiao slag subjected to alcohol extraction in the step (S2) by using water, wherein the mass ratio of the feed liquid is 1:15, heating to 90 ℃ and extracting for 1 time, extracting for 2 hours, and filtering out the extracting solution to obtain yellow Jiang Huashui extracting solution.
S7, multistage membrane separation of water extract: huang Jianghua the residue water extract is centrifuged at a high speed to obtain clear liquid, the centrifugated clear liquid is separated by a first-stage membrane, namely a ceramic membrane with the aperture of 200nm, and the first-stage trapped fluid and the permeate are respectively collected; separating the first-stage permeate by a second-stage membrane, namely a ceramic membrane with the aperture of 15nm, and respectively collecting second-stage trapped fluid and permeate; then the second-stage permeate is further separated by a third-stage membrane, namely a coiled organic membrane with the molecular weight cutoff of 20000Da, and the trapped fluid and the permeate are respectively collected; and obtaining all levels of components separated by the water extract membrane, namely yellow Jiang Huashui extract.
S8, recombining and compounding water extract membrane separation components: the trapped fluid of the second stage and the third stage is selected to be compounded with the penetrating fluid of the third stage, namely, the trapped fluid of 15nm, the trapped fluid of 20000Da and the penetrating fluid of 20000Da are mixed and compounded according to the mass ratio of dry matters of 10:1:20, and the yellow Jiang Huashui refined liquid is obtained.
The two trapped fluids, one permeate and the proportion thereof are obtained through sensory evaluation, and the specific operation process is as follows: the solvent content of the 6 membrane separation components of the 200nm trapped fluid, the permeate, the 15nm trapped fluid, the 20000Da trapped fluid and the permeate is measured respectively, the mass fractions of the dry matters are calculated, and the solutions of the components are adjusted to be the solutions with the same mass fractions of the dry matters by water. And (3) respectively injecting the solutions with the same mass fractions of the dry matters into blank cigarettes without flavoring by adopting a cigarette flavoring injector, wherein the injection quantity of each solution is equal, and then carrying out comparative evaluation on the sample cigarettes by a professional cigarette sensory evaluation personnel. The evaluation results show that: after the 15nm trapped fluid, the 20000Da trapped fluid and the 20000Da permeation fluid are applied to the cigarettes, the fragrance of the cigarettes can be improved to different degrees, the smoke richness is increased, and the cigarettes are coordinated with the fragrance of the cigarettes. The specific evaluation results are shown in Table 2.
TABLE 2 sensory impact score of yellow Jiang Huashui extract film separation component and aqueous extract concentrate applied to blank cigarettes
Figure SMS_2
The water extracted and refined solution of the yellow ginger flowers is concentrated by a reverse osmosis membrane, and then 10 percent of propylene glycol is added for uniform mixing, so that the water extracted and refined solution can be used for resisting corrosion and bacteria, and meanwhile, the propylene glycol can also play the role of a humectant.
The turmeric flower perfume of this example is yellow Jiang Huachun extract obtained in step S3, yellow Jiang Huachun extract obtained in step S4, turmeric flower essential oil obtained in step S5, yellow Jiang Huashui extract obtained in step S7, and yellow Jiang Huashui extract obtained in step S8.
Example 2
The preparation method of the turmeric flower spice in the embodiment comprises the following steps:
s1, raw material treatment: taking dried flowers of Curcuma rhizome as raw materials, removing impurities and pulverizing.
S2, ethanol extraction: heating and extracting with 75% (V/V) ethanol solution at a mass ratio of 1:4, heating to 80deg.C for 3 times, extracting for 1.5 hr for the first time, extracting for 1 hr for the second time, and mixing the 3 times extractive solutions to obtain yellow Jiang Huachun extractive solution.
S3, multistage membrane separation of alcohol extract: centrifuging Huang Jianghua ethanol extract to obtain clear liquid, separating the centrifugated clear liquid with a first-stage membrane (ceramic membrane with aperture of 200 nm), and collecting first-stage trapped fluid and permeate respectively; separating the first-stage permeate by a second-stage membrane, namely a ceramic membrane with the aperture of 20nm, and respectively collecting second-stage trapped fluid and permeate; then the second-stage permeate is further passed through a third-stage membrane, namely a coiled organic membrane with the cutoff molecular weight of 10000Da, and the third-stage cutoff liquid and the permeate are respectively collected; then the third-stage permeate is further passed through a fourth-stage membrane, namely a coiled organic membrane with a molecular weight cutoff of 5000Da, and the fourth-stage retentate and the permeate are respectively collected; obtaining all levels of components separated by the alcohol extract membrane, namely yellow Jiang Huachun extract.
S4, recombining and compounding alcohol extract membrane separation components: and (3) selecting the first-stage trapped fluid, the third-stage trapped fluid and the fourth-stage trapped fluid for compounding, namely mixing and compounding the 200nm trapped fluid, the 10000Da trapped fluid and the 5000Da trapped fluid according to a dry matter mass ratio of 12:6:1 to obtain the yellow Jiang Huachun refined product.
The three trapped fluids and the dry matter mass ratio are obtained through sensory evaluation, and the specific operation process is as follows: the solvent content of the 8 membrane separation components of the 200nm trapped fluid, the permeate, the 20nm trapped fluid, the 10000Da trapped fluid, the permeate, the 5000Da trapped fluid and the permeate are respectively measured, and 75% ethanol is used for adjusting the dry matter mass fractions of the component solutions to be the same. The solutions are respectively and equally applied to the non-flavored fed heated non-burnt cigarette tobacco shreds of the same leaf group formula, and then the comparison evaluation is carried out on the sample cigarettes by professional cigarette sensory evaluation personnel. The evaluation results show that: after the 200nm trapped fluid, the 10000Da trapped fluid and the 5000Da trapped fluid are applied to the heated nonflammable cigarettes, different dimensions of the yellow Jiang Huaxiang air style can be well reflected, the fragrance quantity is increased, the fragrance is enriched, the fragrance is coordinated with the tobacco fragrance, and the aftertaste is comfortable. In addition, the sensory effect of the 5000Da permeate is also better. In order to further obtain essential oil products with higher added values, 5000Da permeate is not added during the recombination and compounding of the alcohol extract membrane separation components. The specific evaluation results are shown in Table 3.
TABLE 3 sensory impact score of yellow Jiang Huachun extract film separation component and alcohol extract concentrate applied to heated nonflammable cigarettes
Figure SMS_3
S5, preparing essential oil by molecular distillation: reverse osmosis concentrating the permeate of 5000Da membrane separation of yellow Jiang Huachun extract by reverse osmosis membrane to remove most of solvent; then the reverse osmosis trapped fluid is further distilled under reduced pressure to remove volatile solvent, the concentrate is separated by a molecular distillation instrument, the molecular distillation temperature is 40 ℃, the distillation pressure is 0.01mbar, and the light component is collected, namely the turmeric essential oil.
S6, extracting slag with water: extracting the yellow Jiang Hualiao slag after the alcohol extraction in the step S2 with water in a mass ratio of 1:5, heating to 70 ℃ for 2 times, extracting for 1.5 hours for the first time, extracting for 1 hour for the second time, and combining the two extracting solutions to obtain yellow Jiang Huashui extracting solution;
s7, multistage membrane separation of water extract: centrifuging Huang Jianghua residue water extract to obtain clear liquid, separating the centrifuged clear liquid by a first-stage membrane, namely a ceramic membrane with the aperture of 200nm, and respectively collecting first-stage trapped fluid and permeate; the first-stage permeate liquid further passes through a second-stage membrane, namely a ceramic membrane with the aperture of 20nm, and second-stage trapped fluid and permeate liquid are respectively collected; then the second-stage permeate is further separated by a third-stage membrane, namely a ceramic membrane with the aperture of 10nm, and third-stage trapped fluid and permeate are respectively collected; and obtaining all levels of components separated by the water extract membrane, namely yellow Jiang Huashui extract.
S8, recombining and compounding water extract membrane separation components: and (3) selecting the trapped fluid of the second stage and the third-stage penetrating fluid for compounding, namely mixing and compounding the trapped fluid of 20nm, the trapped fluid of 10nm and the penetrating fluid of 10nm according to a dry matter mass ratio of 8:1:15 to obtain yellow Jiang Huashui refined liquid.
The mass ratio of the two trapped fluids, one permeate and the dry matter thereof is obtained through sensory evaluation, and the specific operation process is as follows: the solvent contents of the 6 membrane separation components of the 200nm trapped fluid, the permeate, the 20nm trapped fluid, the permeate, the 10nm trapped fluid and the permeate are respectively measured, and the dry mass fractions of the component solutions are adjusted to be the same by water. And 6 parts of tobacco shreds of the same batch are taken, the solutions are respectively and equally applied to 6 parts of tobacco shreds of the same batch, and after a period of time of tobacco shred storage (sealed placement under the condition of constant temperature and constant humidity), the sample tobacco shreds are subjected to comparison evaluation by a professional cigarette sensory evaluation personnel. The evaluation results show that: after the 20nm trapped fluid, the 10nm trapped fluid and the 10nm penetrating fluid are applied to the cut tobacco of the pipe tobacco, the fragrance of the cut tobacco of the pipe tobacco during burning and sucking can be improved to different degrees, the smoke richness is increased, the aftertaste is improved, and the smoke state is improved. The specific evaluation results are shown in Table 4.
TABLE 4 sensory impact score of yellow Jiang Huashui extract film separation component and aqueous extract concentrate applied to cut filler
Figure SMS_4
The water extracted and refined solution of the yellow ginger flowers is prepared into extractum for use after being decompressed and concentrated, or is added with 5 percent of propylene glycol for uniform mixing, so that the water extracted and refined solution can be used for preventing and inhibiting bacteria, and meanwhile, the propylene glycol can also play the role of a humectant.
The turmeric flower perfume of this example is yellow Jiang Huachun extract obtained in step S3, yellow Jiang Huachun extract obtained in step S4, turmeric flower essential oil obtained in step S5, yellow Jiang Huashui extract obtained in step S7, and yellow Jiang Huashui extract obtained in step S8.
Example 3
The preparation method of the turmeric flower spice in the embodiment comprises the following steps:
s1, raw material treatment: taking dried flowers of Curcuma rhizome as raw materials, removing impurities and pulverizing.
S2, ethanol extraction: heating and extracting with 85% (V/V) ethanol solution at a mass ratio of 1:15, heating to 70deg.C, extracting for 1 time for 4 hr, and filtering to obtain yellow Jiang Huachun extractive solution.
S3, multistage membrane separation of alcohol extract: centrifuging Huang Jianghua ethanol extract to obtain clear liquid, separating the centrifugated clear liquid with a first-stage membrane (ceramic membrane with aperture of 50 nm), and collecting first-stage trapped fluid and permeate respectively; the first-stage permeate is further passed through a second-stage membrane, namely a ceramic membrane with the aperture of 15nm, and the second-stage retentate and the permeate are respectively collected; then the second-stage permeate is further passed through a third-stage membrane, namely a ceramic membrane with the aperture of 5nm, and the third-stage trapped fluid and the permeate are respectively collected; then the third-stage permeate is further passed through a fourth-stage membrane, namely a coiled organic membrane with a cut-off molecular weight of 3000Da, and the fourth-stage cut-off liquid and the permeate are respectively collected; obtaining all levels of components separated by the alcohol extract membrane, namely yellow Jiang Huachun extract.
S4, recombining and compounding alcohol extract membrane separation components: and (3) selecting the first-stage trapped fluid, the third-stage trapped fluid and the fourth-stage trapped fluid for compounding, namely mixing and compounding the 50nm trapped fluid, the 5nm trapped fluid and the 3000Da trapped fluid according to a dry matter mass ratio of 11:5:1 to obtain the yellow Jiang Huachun refined product.
The three trapped fluids and the recombination proportion thereof are obtained by sensory evaluation, and the specific operation process comprises the following steps: the solvent contents of 8 membrane separation components, namely 50nm trapped fluid, permeate fluid, 15nm trapped fluid, permeate fluid, 5nm trapped fluid, permeate fluid, 3000Da trapped fluid and permeate fluid, are respectively measured, and the dry mass fractions of the component solutions are adjusted to be the same by using 85% ethanol. And (3) respectively injecting the solutions with the same mass fractions of the dry matters into blank cigarettes without flavoring and feeding by adopting a cigarette flavoring injector, wherein the injection quantity of each solution is equal. And then, carrying out comparison evaluation on the sample cigarettes by a professional cigarette sensory evaluation personnel. The evaluation results show that: after the 50nm trapped fluid, the 5nm trapped fluid and the 3000Da trapped fluid are applied to cigarettes, different dimensions of yellow Jiang Huaxiang gas styles can be well reflected, the fragrance quantity is increased, the fragrance notes are enriched, and the quality of the cigarettes is improved. In addition, the sensory effect of the 3000Da permeate is also better. In order to further obtain essential oil products with higher added values, 3000Da permeate is not added during the recombination and compounding of the alcohol extract membrane separation components. The specific evaluation results are shown in Table 5.
TABLE 5 sensory impact score of yellow Jiang Huachun extract film separation component and alcohol extract concentrate applied to blank cigarettes
Figure SMS_5
Figure SMS_6
S5, preparing essential oil by molecular distillation: reverse osmosis concentrating the permeate of 3000Da membrane separation of yellow Jiang Huachun extract by reverse osmosis membrane to remove most of solvent; then the reverse osmosis trapped fluid is further distilled under reduced pressure to remove volatile solvent, the concentrate is separated by a molecular distillation instrument, the molecular distillation temperature is 50 ℃, the distillation pressure is 0.05mbar, and the light component is collected, namely the turmeric essential oil.
S6, extracting slag with water: further heating and extracting the yellow Jiang Hualiao slag after the alcohol extraction in the step S2 with water, wherein the mass ratio of the feed liquid is 1:10, heating to 80 ℃ and extracting for 1 time, extracting for 3 hours, and filtering to obtain an extracting solution, namely yellow Jiang Huashui extracting solution;
s7, multistage membrane separation of water extract: huang Jianghua, centrifuging the water extract of the slag to obtain clear liquid, separating the centrifuged clear liquid by using a first-stage membrane which is a ceramic membrane with the aperture of 200nm, and respectively collecting first-stage trapped fluid and permeate; the first-stage permeate is further passed through a second-stage membrane, namely a roll-type organic membrane with the molecular weight cut-off of 80000Da, and the second-stage cut-off and permeate are respectively collected; then the second-stage permeate is further passed through a third-stage membrane, namely a ceramic membrane with the aperture of 5nm, and the third-stage trapped fluid and the permeate are respectively collected; and obtaining all levels of components separated by the water extract membrane, namely yellow Jiang Huashui extract.
S8, recombining and compounding water extract membrane separation components: the trapped fluid of the second stage and the third stage is selected to be compounded with the penetrating fluid of the third stage, namely, the trapped fluid of 80000Da, the trapped fluid of 5nm and the penetrating fluid of 5nm are mixed and compounded according to the dry matter mass ratio of 9:1:18, and the yellow Jiang Huashui refined liquid is obtained.
The two trapped fluids, a penetrating fluid and the compound proportion thereof are obtained through sensory evaluation, and the specific operation process is as follows: the solvent contents of the 6 membrane separation components of the 200nm trapped fluid, the permeate, the 80000Da trapped fluid, the 5nm trapped fluid and the permeate are respectively measured, and the dry mass fractions of the component solutions are adjusted to be the same by water. And 6 parts of the same batch of cigarette tobacco shreds are taken, and the solutions are uniformly sprayed on 6 parts of the tobacco shreds in equal quantity respectively. After a period of time of cut tobacco storage (sealed placement under the conditions of constant temperature and constant humidity), the 6 sample cut tobacco are respectively made into cigarettes by a cigarette making device, and the sample cigarettes are subjected to comparison evaluation by professional cigarette sensory evaluation personnel. The evaluation results show that: after 80000Da trapped fluid, 5nm trapped fluid and 5nm penetrating fluid are applied to cut tobacco of cigarettes, the aroma amount of the cigarettes during smoking can be improved to different degrees, the smoke richness is increased, the stimulation is reduced, and the smoke state is improved. The specific evaluation results are shown in Table 6.
TABLE 6 organoleptic score of yellow Jiang Huashui extract film separation component and aqueous extract concentrate applied to cut tobacco of cigarettes
Figure SMS_7
The water extracted and refined solution of the yellow ginger flowers is prepared into extractum for use after being decompressed and concentrated, or 7 percent of propylene glycol is added for even mixing, so that the water extracted and refined solution can be used for preventing and inhibiting bacteria, and meanwhile, the propylene glycol can also play the role of a humectant.
The turmeric flower perfume of this example is yellow Jiang Huachun extract obtained in step S3, yellow Jiang Huachun extract obtained in step S4, turmeric flower essential oil obtained in step S5, yellow Jiang Huashui extract obtained in step S7, and yellow Jiang Huashui extract obtained in step S8.
2. Examples of the use of the turmeric flower flavor of the present invention in tobacco products
Example 4
The yellow Jiang Huachun extract, the yellow ginger flower essential oil and the yellow Jiang Huashui extract prepared in examples 1-3 are adopted to perfume tobacco products such as cigarettes, non-combustible cigarettes when heated, tobacco shreds of tube cigarettes and the like, and can be used singly or mixed with the three components or mixed with other spices to form essence. Depending on the solubility of the extract, it may be used in oil-soluble systems or water-soluble systems, respectively. The specific application mode is as follows:
the water extracted refined solution of the yellow ginger flowers can be sprayed onto tobacco shreds in a feeding link of cigarette production after being diluted; huang Jianghua the refined extract of alcohol extraction and the essential oil of turmeric flower can be mixed with other spices to prepare essence, and then sprayed onto tobacco shreds in the flavoring link of cigarette production; huang Jianghua the essential oil can be dissolved in caprylic/capric glyceride to prepare explosive beads (aromatic beads) for the cigarette filter stick, and the explosive beads are filled in the center of the filter stick; or the turmeric essential oil is applied to the filter stick forming process to prepare a fragrant line so as to realize the flavoring of the cigarette filter stick; the water extraction refined solution of the yellow ginger flowers can be coated on cigarette paper to realize the flavoring of the cigarette paper; huang Jianghua ethanol extract refined product, curcuma rhizome essential oil and yellow Jiang Huashui extract refined solution can also be applied to flavoring and perfuming process of tobacco shred; huang Jianghua the refined extract and the turmeric essential oil can be applied to the flavoring link of the heating non-burning cigarettes.

Claims (15)

1. The preparation method of the turmeric flower spice is characterized by comprising the following steps of:
(1) Leaching the crushed or crushed turmeric flower with ethanol solution, and carrying out solid-liquid separation to obtain ethanol extract;
(2) Carrying out multistage membrane separation on the alcohol extract by adopting an organic membrane and/or a ceramic membrane, and carrying out step-by-step separation according to the pore diameter of the membrane from large to small to obtain all-grade trapped fluid or part-grade trapped fluid, thereby obtaining yellow Jiang Huachun extract; the molecular weight cut-off of the organic membrane is from 3000Da to 200000Da, and the membrane pore diameter of the ceramic membrane is from 5nm to 200nm.
2. The method for preparing the turmeric flower perfume according to claim 1, wherein the multi-stage membrane separation in the step (2) is a four-stage membrane separation, wherein the first stage membrane is a ceramic membrane with a pore diameter of 50-200 nm, the second stage membrane is a ceramic membrane with a pore diameter of 15-20 nm or an organic membrane with a molecular weight cut-off of 80000-200000 Da, the third stage membrane is a ceramic membrane with a pore diameter of 5-10 nm or an organic membrane with a molecular weight cut-off of 10000-20000 Da, and the fourth stage membrane is an organic membrane with a molecular weight cut-off of 3000-5000 Da.
3. The preparation method of the turmeric flower spice as defined in claim 2, wherein the trapped fluid of the first-stage membrane, the third-stage membrane and the fourth-stage membrane in the Huang Jianghua alcohol extract is compounded to obtain the turmeric Jiang Huachun extract.
4. The method for preparing the turmeric flower perfume according to claim 3, wherein the dry matter mass ratio of the trapped fluid of the first-stage membrane, the third-stage membrane and the fourth-stage membrane is (10-12): 5-6): 1.
5. The method for preparing the turmeric flower fragrance according to claim 1, further comprising the steps of: concentrating the permeate liquid of the final stage of membrane separation in the step (2), removing the solvent, then carrying out molecular distillation at the temperature of 40-70 ℃ and collecting light components to obtain the turmeric flower essential oil.
6. The method for preparing a turmeric flower fragrance as claimed in claim 5, characterized in that the pressure of the molecular distillation is 0.01-0.1 mbar.
7. The method for preparing a turmeric flower fragrance as defined in claim 1 or 5, further comprising the steps of:
a. soaking and extracting the slag obtained by the solid-liquid separation in the step (1) with water, and performing solid-liquid separation to obtain water extract;
b. performing multistage membrane separation on the water extract by adopting a ceramic membrane and/or an organic membrane, and performing stepwise separation according to the pore diameter of the membrane from large to small to obtain partial level trapped fluid and final level permeate, thereby obtaining yellow Jiang Huashui extract; the membrane aperture of the ceramic membrane is from 5 to 200nm, and the molecular weight cut-off of the organic membrane is from 10000 to 200000Da.
8. The method for preparing the turmeric flower perfume according to claim 7, wherein the multi-stage membrane separation in the step b is three-stage membrane separation, wherein the first stage membrane is a ceramic membrane with a pore diameter of 200nm, the second stage membrane is a ceramic membrane with a pore diameter of 15-20 nm or an organic membrane with a molecular weight cutoff of 80000-200000 Da, and the third stage membrane is a ceramic membrane with a pore diameter of 5-10 nm or an organic membrane with a molecular weight cutoff of 10000-20000 Da.
9. The method for preparing a yellow ginger flower perfume according to claim 8, wherein the second-stage membrane, the third-stage membrane retentate and the third-stage membrane permeate in the yellow ginger flower water extract are compounded according to the dry matter mass ratio of (8-10): 1 (15-20) to obtain yellow Jiang Huashui extract.
10. The method for preparing a turmeric flower fragrance according to claim 1, wherein the concentration of the ethanol solution is 75 to 95% (V/V); the mass ratio of the leached liquid in the step (1) is 1:4-15.
11. The method for preparing the turmeric flower fragrance according to claim 1 or 10, wherein the leaching is performed under the condition of heating at 60 to 80 ℃ for 2 to 6 hours.
12. The preparation method of the turmeric flower spice according to claim 7, wherein the mass ratio of the water extracted in the step a is 1:5-15.
13. The method for preparing the turmeric flower spice according to claim 12, wherein the water extraction is performed under the condition of heating at 70-90 ℃, and the water extraction time is 1-7 h.
14. A turmeric flower spice characterized by being prepared by the preparation method of any one of claims 1-13.
15. Use of a turmeric flower flavor as defined in claim 14 in a tobacco product, wherein said tobacco product is a conventional cigarette, a heated non-burning cigarette or a tube cigarette.
CN202211667929.0A 2022-12-23 2022-12-23 Yellow Jiang Huaxiang material, preparation method thereof and application thereof in tobacco products Pending CN116042315A (en)

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