CN109090700B - Efficient preparation method and application of coffee absolute - Google Patents
Efficient preparation method and application of coffee absolute Download PDFInfo
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- CN109090700B CN109090700B CN201811097793.8A CN201811097793A CN109090700B CN 109090700 B CN109090700 B CN 109090700B CN 201811097793 A CN201811097793 A CN 201811097793A CN 109090700 B CN109090700 B CN 109090700B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for extraction
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/10—Chemical features of tobacco products or tobacco substitutes
- A24B15/16—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes
- A24B15/167—Chemical features of tobacco products or tobacco substitutes of tobacco substitutes in liquid or vaporisable form, e.g. liquid compositions for electronic cigarettes
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
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- A24F47/008—
Abstract
The invention discloses a preparation method of coffee absolute, which uses the following devices: an ultrasonic extraction tank (1); a chromatography column (2); an air compressor (3); a concentration tank (4); a reverse resin column (5); a condenser (6); a vacuum pump (8); a solvent recovery tank (7); the method comprises the following steps: ultrasonically extracting coffee raw materials; purifying through a chromatographic column (2); thirdly, concentration; purifying through a reverse resin column (5); and fifthly, removing ethanol under reduced pressure to obtain the coffee absolute. The device can efficiently extract and purify the coffee absolute, and the obtained coffee absolute is used for melting cigarettes, electronic cigarettes or heating non-burning cigarettes, so that the smoking comfort of the cigarettes is effectively improved.
Description
Technical Field
The invention belongs to the field of preparation of tobacco essence and flavor, and particularly relates to a method for efficiently preparing coffee absolute and application of the coffee absolute in perfuming cigarettes, electronic cigarettes and heating non-combustible cigarettes.
Background
Cigarette flavoring is a core technology for strengthening the style characteristics of cigarettes, particularly in recent years, the continuous promotion of tar and harm reduction work of tobacco gradually reduces the tar release amount of the cigarettes, and the fragrance and the taste of the cigarettes are reduced along with the tar release amount, so that the sensory quality of the cigarettes is ensured and improved by means of flavoring, and the pursuit of consumers for the fragrance and the taste of the cigarettes is met. In addition, with the development of novel tobacco products such as electronic cigarettes, heating non-combustible cigarettes and the like, the novel natural plant spice component has strong demand for flavoring, the natural plant spice component is used for replacing synthetic spices to blend the fragrance of the tobacco products, the richness of the product fragrance is improved, and the requirements of consumers on different tastes can be better met.
Coffee (coffea. spp.) is the second trade product in the world, Rubiaceae (Rubiaceae), coffea (coffea) evergreen shrub or small tree, and tea, cocoa and is known as the world's three major beverage. The coffee beans gradually generate volatile flavor oil in the processes of stacking fermentation and deep baking, so that various flavors are perfectly balanced.
At present, coffee extract is used as tobacco additive, main products comprise extractum, tincture, absolute oil and the like, and traditional coffee extract preparation methods mainly comprise solvent extraction, supercritical extraction, molecular distillation and other methods, and the methods have high production cost and low absolute oil rate. In addition, the existing coffee extract is complex in components, so that the existing coffee extract is used in a novel tobacco product, and the smoking experience of electronic cigarettes and heating non-combustible cigarettes is influenced.
Disclosure of Invention
The invention designs a method for preparing coffee absolute by column chromatography separation aiming at the defects in the prior art. Compared with the traditional solvent extraction and molecular distillation methods, the production cost is obviously reduced, and the yield and the quality of the absolute oil are improved. The obtained coffee absolute can be used for flavoring a traditional cigarette, and can also be used for novel tobacco products (such as an electronic cigarette or a non-combustion cigarette), so that the special characteristics of roasting aroma and nut aroma of the coffee of the cigarette, the electronic cigarette or the non-combustion cigarette can be effectively enhanced, the richness and aftertaste of the aroma can be improved, the miscellaneous gas of product smoking can be covered, the smoking comfort of the cigarette, the electronic cigarette or the non-combustion cigarette can be improved, the smoke quality can be improved, and the better smoking feeling can be provided for consumers.
The technical scheme of the invention is as follows:
the invention discloses a preparation method of coffee absolute, which uses the following devices:
an ultrasonic extraction tank 1, the upper part of which is provided with a feed inlet 11 and the lower part of which is provided with a discharge outlet 14, and the upper part of the discharge outlet 14 is provided with a filter sieve plate 13;
-a chromatography column 2;
-an air compressor 3;
-a concentration tank 4;
-a reverse resin column 5;
-a condenser 6;
-a vacuum pump 8;
-a solvent recovery tank 7;
the connection mode of each part is as follows:
the ultrasonic extraction tank 1 is communicated with an inlet at the upper part of the chromatographic column 2 through a discharge hole 14 of the ultrasonic extraction tank, and an outlet at the lower part of the chromatographic column 2 is communicated with the upper part of the concentration tank 4; the upper part of the concentration tank 4 is communicated with an inlet of the condenser 6, and an outlet at the upper end of the condenser 6 is communicated with the vacuum pump 8; the outlet at the lower end of the condenser 6 is communicated with the solvent recovery tank 7; the air compressor 3 is respectively communicated with the upper port of the ultrasonic extraction tank 1 and the upper port of the concentration tank 4; the outlet at the lower part of the concentration tank 4 is communicated with the reverse resin column 5;
the preparation method comprises the following steps:
adding coffee raw materials into the ultrasonic extraction tank 1, sealing a feeding port and a discharging port, adding methyl acetate 4-6 times of the weight of the coffee raw materials, and performing ultrasonic extraction at 40-50 ℃ for 30-40 min;
secondly, starting an air compressor 3 after extraction is finished, pressurizing the ultrasonic extraction tank 1 in the step I, and enabling the extract to enter a concentration tank 4 through a chromatographic column 2 through a filter sieve plate 13 of a discharge port 14;
thirdly, heating the concentration tank 4 to 75-85 ℃, starting the vacuum pump 8 and the condenser 6, and concentrating the extract liquor under reduced pressure until the methyl acetate is evaporated to dryness to obtain a paste extracted from coffee;
fourthly, 95 wt% of ethanol is added into the concentration tank 4 to completely dissolve the paste obtained in the third step, and an air compressor 3 is started to pressurize the concentration tank 4 to ensure that the liquid completely passes through a reverse resin column 5;
fifthly, adding propylene glycol with the weight 3-5 times of that of the paste into the liquid obtained in the step (iv), and removing ethanol through reduced pressure evaporation to obtain the coffee absolute.
Preferably, the diameter and height of the chromatographic column 2 are 2:1, silica gel particles and anhydrous sodium sulfate particles are filled in the chromatographic column, and the particle diameters of the silica gel particles and the anhydrous sodium sulfate particles are respectively 100-200 meshes; the reverse resin column 5 is filled with BOSHI reverse resin; the diameter of the BOSHI reverse phase resin filling is 1:2, and the particle size of the BOSHI reverse phase resin filling is 35-75 mu m.
Preferably, the upper end of the ultrasonic extraction tank 1 is communicated with a first pump B1; the upper end of the concentration tank 4 is communicated with a second pump B2; all the parts are communicated through a pipeline, and the pipeline is provided with a valve F.
Preferably, before the extract liquid is concentrated under reduced pressure, the method further comprises the step of washing the ultrasonic extraction tank 1 by using methyl acetate, and then feeding a methyl acetate washing liquid into the concentration tank 4 through the chromatographic column 2.
Preferably, before removing ethanol by evaporation under reduced pressure, the method further comprises washing the concentration tank 4 with 95 wt% ethanol of 1/5-1/4 of the weight of the paste, passing the ethanol washing solution through a reverse resin column 5, and removing ethanol by evaporation under reduced pressure.
The invention also discloses the application of the coffee absolute oil prepared by the preparation method in perfuming cigarettes, electronic cigarettes or non-burning cigarettes.
The steps of the method for preparing the coffee absolute oil of the invention are described below with reference to the accompanying drawings, in which:
A. extraction of coffee materials
For extracting aroma components in coffee raw materials, common solvents comprise ethanol, petroleum ether, ethyl acetate and the like, the ethyl acetate has moderate polarity, can dissolve most aroma components and glycoside compounds thereof, and the dissolution of carbohydrate compounds with high content in coffee is extremely low, so that the ethyl acetate is an ideal extraction solvent, but the boiling point of the ethyl acetate is high, reaches 77.5 ℃, the energy consumption is high in the sample concentration process, and the ethyl acetate is easy to remain. Therefore, methyl acetate is used as an extraction solvent instead of ethyl acetate, the methyl acetate and the ethyl acetate have very similar chemical properties, but the boiling point is only 57.8 ℃, the energy consumption of sample concentration is greatly reduced compared with the ethyl acetate, and solvent residue cannot be caused in the sample.
The coffee raw material used is Yunnan small-grained coffee, the sample is fermented, roasted and crushed to 15-20 meshes, the sample is added into an ultrasonic extraction tank from a feed inlet 11 of a constant-temperature ultrasonic extraction tank 1 shown in figure 1, the feed inlet and a discharge outlet are sealed, a first pump B1 is started, methyl acetate with the weight 4-6 times of that of the coffee raw material is added, and then ultrasonic extraction is carried out for 30-40min at the temperature of 40-50 ℃. After extraction, the valve F2 in fig. 1 is opened, and the air compressor 3 is started to pressurize the ultrasonic extraction tank 1, so that the coffee extract passes through the filtering sieve 13 on the discharge port 14 and is led to the chromatographic column 2 with silica gel particles 22 of anhydrous sodium sulfate particles 21.
B. Purification of coffee extract by anhydrous sodium sulfate particle and silica gel particle composite chromatographic column 2
Since the coffee material contains water, water and a small amount of highly polar components such as saccharides are also dissolved in the coffee extract during the extraction of the absolute coffee oil. In the invention, the extraction liquid is purified by adopting a chromatographic column 2 compounded by anhydrous sodium sulfate particles and silica gel particles.
Diameter of the column 2: the height is 2:1, the size of the chromatographic column 2 is matched with the feeding amount of the coffee sample, wherein the particle size of the silica gel particles 22 is 100-200 meshes, the loading amount of the silica gel particles 22 is 1/50 of the feeding amount of the coffee sample, the particle size of the anhydrous sodium sulfate particles 21 is also 100-200 meshes, and the loading amount of the anhydrous sodium sulfate particles 21 is 1/4 of the silica gel. When the extract passes through the chromatographic column 2, moisture in the extract is adsorbed and removed by the anhydrous sodium sulfate particles 21, and large polar components such as sugar eluted in a small amount are adsorbed and removed by the silica gel particles 22, whereby the effect of efficiently purifying the extract can be achieved by passing through the chromatographic column 2. The extract liquid purified by the anhydrous sodium sulfate particle and silica gel particle composite chromatographic column is transferred to a concentration tank 4.
C. Concentration of the extract
And after the extract is transferred into a concentration tank, heating the concentration tank to 75-85 ℃, starting a condensation pipe 6 and a vacuum pump 8 at the same time, and concentrating the extract under reduced pressure until the methyl acetate is evaporated to dryness to obtain the paste of the coffee extract. The methyl acetate solvent is cooled again by the condenser 6 and then enters the solvent recovery tank 7 for next extraction of coffee materials.
D. Coffee raw material washing
Returning the recovered methyl acetate after sample concentration to the ultrasonic extraction tank again, performing ultrasonic extraction at 40-50 deg.C for 20-30min, passing through chromatographic column 2 according to the above method, and transferring to concentration tank 4. The concentrating tank 4 was again started and the methyl acetate was evaporated to dryness under reduced pressure to give a paste of absolute coffee oil. The methyl acetate obtained by the concentration can be used for the next coffee extraction.
E. Purification of coffee extract by reversed phase resin column chromatography
Because the methyl acetate extract of coffee contains a large amount of small polar components such as wax, fatty acid and the like which are unfavorable for cigarette sense, the extract product needs to be further purified by reversed-phase resin column chromatography to remove wax and fatty acid impurities so as to improve the quality of the obtained absolute oil. In the invention, the resin filling diameter of the BOSHI reversed-phase resin chromatographic column 5 for removing impurities such as wax, fatty acid and the like is 1:2, the particle size of the resin is 35-75 mu m, and the filling amount of the resin is 1/2-1/3 of the obtained paste.
The purification operation of the reversed phase resin column chromatography is as follows: heating the concentration tank to 50-60 ℃, adding 95 wt% of ethanol into the concentration tank 4 through a second pump B2 in the figure 1, wherein the addition amount is enough to completely dissolve the obtained paste, opening a valve F4 after completely dissolving the paste, starting an air compressor 3 to pressurize the concentration tank, opening a valve F8, and allowing the ethanol solution after dissolving the paste to pass through a reversed-phase resin chromatographic column 5; after passing through the column, 95 wt% ethanol is added again to the concentration tank 4 to wash the concentration tank 4, the 95 wt% ethanol is added in an amount of 1/5-1/4 which is the first addition amount, and the washing solution is passed through the reversed phase resin chromatography column 5.
In the step, 95 w% ethanol solution of the paste passes through the chromatographic column 5, and 95 wt% ethanol is used for washing the chromatographic column 5, so that aroma components in the absolute coffee oil are not retained on the reverse resin chromatographic column 5, and impurity components such as wax, fatty acid and the like can be retained on the reverse resin chromatographic column, and the effect of separating the aroma components from the impurities such as wax, fatty acid and the like in the absolute coffee oil can be effectively achieved, thereby improving the quality of the absolute coffee oil.
Mixing the above 95 wt% ethanol solutions, adding 3-5 times of propylene glycol into the solution, and evaporating under reduced pressure to remove ethanol to obtain the coffee absolute. The propylene glycol is added to improve the fluidity of the absolute coffee oil and stabilize the coffee aroma components in the absolute coffee oil.
The yield of the obtained coffee absolute is 5.2-6.3%. The obtained coffee absolute is uniform and transparent brown oily fluid with strong coffee characteristic aroma, and the aroma is elegant and comfortable; the tobacco additive has good solubility in solvents such as ethanol and propylene glycol, and is an ideal tobacco additive.
F. Recovery of residual methyl acetate
After the sample is completely extracted, methyl acetate is remained in the extracted coffee waste residue, and the method can recycle the part of methyl acetate so as to reduce the environmental pollution in the production process and save the production consumption. The solvent recovery process comprises the following steps: and (3) closing the valve F1 and the valve F5, sealing the feeding port 11, heating the ultrasonic extraction tank 1 to 90-100 ℃, evaporating methyl acetate in the extraction tank, transferring the evaporated methyl acetate vapor to a concentration tank through an anhydrous sodium sulfate and silica gel composite chromatographic column, condensing and recovering the methyl acetate vapor by a condenser, and then feeding the methyl acetate vapor into a solvent recovery tank 7. In the process, methyl acetate vapor passes through the anhydrous sodium sulfate and silica gel composite chromatographic column 2, and then the residual methyl acetate in the chromatographic column 2 is also taken out, so that the effect of effectively recovering the residual solvent is achieved. The recovered methyl acetate was available for the next extraction of coffee samples.
G. Regeneration of reversed-phase resin chromatographic column
In the invention, the anhydrous sodium sulfate and silica gel composite chromatographic column is disposable, and needs to be refilled and replaced when clean oil is produced next time. The BOSHI reversed-phase resin chromatographic column 5 can be reused for multiple times (at least 6000 times), and the used BOSHI reversed-phase resin chromatographic column 5 is eluted by acetone with the volume 2-3 times of the column volume, and can be reused after being regenerated after waxiness and fatty acid adsorbed on the column are removed.
H. Application of obtained coffee absolute in cigarette flavoring
a. The coffee absolute oil prepared by the method is used in cigarette tobacco shreds, the coffee absolute oil is added to the cigarette tobacco shreds according to the proportion of five to one ten thousandth of the weight of the tobacco shreds, and the tobacco shreds are made into cigarette finished products for evaluation smoking. The results show that: the coffee absolute prepared by the invention can effectively endow the cigarette product with special roast flavor and nut flavor of coffee, improve the quality of the flavor and aroma sucked by the cigarette, cover the impure flavor sucked by the cigarette, improve the comfort sucked by the cigarette, and is superior to a control sample (namely the cigarette without the coffee absolute prepared by the invention).
Or the like, or, alternatively,
b. in the process of forming a cigarette filter, the absolute coffee oil obtained by the invention is added into triacetyl glycerine according to the amount which is 1-1.5 wt% of the amount of triacetyl glycerine of a plasticizer, the triacetyl glycerine added with the absolute coffee oil is uniformly sprayed on filter tow according to 6-8 wt% of the weight of the filter tow to prepare a filter rod, and then the filter rod is prepared into a cigarette through conventional cigarette rolling to carry out sensory evaluation and smoking. The results show that: the cigarette added with the coffee absolute of the invention has better aroma quantity, aroma richness and elegance than a control cigarette, has the characteristic of roast aroma and nut aroma peculiar to coffee and is better than a control sample (namely, the cigarette without the coffee absolute of the invention). Or the like, or, alternatively,
c. in the preparation process of cigarette paper, the coffee absolute prepared by the invention is uniformly coated on the cigarette paper according to the proportion of 0.8-1.2 times of the weight of the cigarette paper, and then the cigarette paper coated with the coffee absolute is rolled into cigarettes for sensory evaluation and smoking evaluation. The results show that: the cigarette added with the coffee absolute of the invention has outstanding coffee characteristic smell, and the amount of aroma, quality and comfort of cigarette smoking are superior to those of a control sample (namely, the cigarette without the coffee absolute of the invention).
I. Application of obtained coffee absolute in electronic cigarette tobacco tar
In the process of preparing the cigarette liquid of the electronic cigarette, the coffee absolute prepared by the invention is added into the cigarette liquid of the electronic cigarette in a proportion of 1-7 wt%, wherein the preferred proportion is 5 wt%. The coffee absolute can also be used in electronic cigarette liquid such as fruit coffee, mint coffee, etc. in a proportion of 0.1-3 wt%. The results show that: the electronic cigarette containing the electronic cigarette tobacco tar has higher total smoking score, and is mainly characterized by good aroma quality and sufficient aroma amount; and the following characteristics that the offensive odor is light, the aftertaste is cleaner, and the electronic cigarette is superior to a control sample (namely the electronic cigarette without the coffee absolute oil obtained by the invention).
J. Application of obtained coffee absolute in heating non-burning cigarette
In the process of making the cigarette without burning by heating, the coffee absolute oil prepared by the invention is added to the slice of the cigarette without burning by heating according to the proportion of one to five parts per million, and the coffee absolute oil prepared by the invention is not added to be used as a reference sample for sensory evaluation. The results show that: the heating non-combustion cigarette coffee added with the coffee absolute has the advantages of prominent characteristic of roasted aroma and nut aroma, more sufficient aroma amount and improved smoking quality, and is superior to a control sample (namely the heating non-combustion cigarette without the coffee absolute obtained by the invention).
The invention has the beneficial effects that:
1. the invention adopts methyl acetate as an extracting agent. The methyl acetate has moderate polarity, not only can dissolve most aroma components in the tobacco leaf sample, but also can not extract large polar components such as saccharides and the like in the coffee in the extraction process, and the obtained coffee absolute has high purity. In addition, the methyl acetate has low boiling point, is easy to volatilize, has low energy consumption in the sample concentration and solvent recovery processes, is not easy to cause solvent residue, and improves the production cost and the product safety compared with other methods.
2. The device skillfully adopts the anhydrous sodium sulfate-silica gel composite chromatographic column and the reversed-phase resin column chromatography to purify the coffee absolute oil efficiently, the anhydrous sodium sulfate-silica gel composite chromatographic column can effectively remove moisture and high-polarity components, and the reversed-phase resin column chromatography can effectively remove small-polarity components such as wax, fatty acid and the like. Compared with the traditional solvent extraction method for producing the absolute coffee oil, the operation process is simplified, the loss of aroma components in the production process is less, and the yield of the absolute coffee oil is obviously improved. Compared with the traditional molecular distillation method, the method can ensure that a large amount of nonvolatile aroma component glycoside compounds (namely aroma compounds) in the coffee are retained in the coffee absolute, effectively avoids the loss of the aroma components, and can release the aroma compounds through the breakage of glycosidic bonds in the combustion process of tobacco, thereby effectively improving the quality of smoke.
3. The device of the invention is provided with a reversed-phase resin column, and the coffee absolute can be refined by using the chromatography reversed-phase resin column. The BOSHI reversed-phase resin is a polystyrene-divinylbenzene copolymerization material, is designed based on the modern HPLC liquid chromatography separation technology, has smaller particles and higher separation performance, and is used for separating, refining and purifying the coffee absolute for the first time. The reverse resin can be reused more than 6000 times after regeneration, can also keep good column efficiency, and has far lower actual production cost than other column chromatography separation processes.
4. Compared with the existing extraction process, the extraction device provided by the invention has the advantages that the energy consumption in the extraction process is reduced and the extraction is more complete. The device can realize the automatic operation of solvent addition, chromatographic column purification and sample concentration, and has simple production process operation and low labor cost consumption. In addition, the solvent used in each step can be effectively recycled by adopting the device of the invention. The solvent consumption in the production process is greatly reduced, the solvent cost is saved, the environmental pollution is greatly reduced, and the safety of production operation is obviously improved.
5. The coffee absolute obtained by using the device of the invention has higher purity, is used in cigarettes or novel tobacco products (such as electronic cigarettes or non-burning cigarettes), effectively strengthens the coffee aroma characteristics of the cigarettes, the electronic cigarettes or the cigarettes which are not burnt by heating, covers up the miscellaneous gas of the product smoking, promotes and improves the smoking comfort of the cigarettes, the electronic cigarettes or the cigarettes which are not burnt by heating, and gives better smoking feeling to consumers.
Drawings
FIG. 1 is a schematic view of an extraction and refining apparatus of the present invention.
The reference signs are: 1. an ultrasonic extraction tank; 2. a chromatography column; 3. an air compressor; 4. a concentration tank; 5. a reverse resin column; 6. a condenser; 7. a solvent recovery tank; 8. a vacuum pump; 11. a feed inlet; 12. a plant material; 13. filtering the sieve plate; 14. a discharge port; 21. anhydrous sodium sulfate particles; 22. silica gel particles; b1, a first pump; b2, a second pump; f (F1-F8) and a valve.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The extraction raw material is prepared by fermenting and baking Yunnan small-particle coffee, crushing to 15 meshes, adding 200kg of the raw material into an ultrasonic extraction tank 1, sealing a feeding port and a discharging port, adding methyl acetate which is 5 times of the weight of a coffee sample, performing ultrasonic extraction at 45 ℃ for 35min, starting an air compressor to pressurize the ultrasonic extraction tank after extraction is finished, and leading the extraction liquid to a chromatographic column for purification through a filter sieve plate at the discharging port.
And transferring the extract passing through the chromatographic column into a concentration tank, heating the concentration tank to 80 ℃, starting a vacuum pump, and concentrating the extract until the methyl acetate is evaporated to dryness. Returning the recovered methyl acetate after the sample is concentrated to the ultrasonic extraction tank 1 again, performing ultrasonic extraction on the raw material for 25min at the temperature of 45 ℃, and enabling the washing liquid to pass through the chromatographic column again and transferring the washing liquid to the concentration tank; the methyl acetate was again evaporated to dryness under reduced pressure to give a paste.
Heating the concentration tank to 55 ℃, adding 95 wt% of ethanol into the concentration tank, wherein the ethanol is added in an amount which can completely dissolve the obtained paste; the concentration tank was then pressurized with an air compressor, and then 95 wt% ethanol dissolved matter was passed through the reversed phase resin chromatography column 5. After the column was completed, the concentration tank was washed by adding the above-mentioned 95 wt% ethanol solution of 1/4 in an amount to completely dissolve the paste, and the washing solution was passed through a reversed-phase resin chromatography column to wash the column. Mixing ethanol solutions, adding propylene glycol 4 times of the weight of the obtained paste, and evaporating under reduced pressure to remove ethanol to obtain the absolute coffee oil with yield of 6.0%. The obtained coffee absolute is uniform and transparent brown oily fluid, has strong coffee characteristic aroma, has good solubility in solvents such as ethanol and propylene glycol, and is an ideal additive for cigarettes.
Example 2
The coffee absolute oil prepared by the method is used in the cut tobacco of the cigarette, the coffee absolute oil is added to the cut tobacco of the cigarette according to the proportion of five hundred thousandth of the weight of the cut tobacco, and the cut tobacco is made into the finished cigarette product for evaluation. The results show that: the coffee absolute prepared by the invention can effectively endow cigarettes with unique roasting aroma and nut aroma characteristics of elegant and natural coffee, improve the aroma quantity and aroma quality of cigarette smoking, cover up the offensive odor of cigarette smoking, improve the comfort of cigarette smoking, and is superior to a control sample (namely, the cigarettes without the coffee absolute prepared by the invention).
Or the like, or, alternatively,
in the process of forming a cigarette filter, the absolute coffee oil obtained by the invention is added into glycerol triacetate according to the amount of 1 wt% of the glycerol triacetate as a plasticizer, then the glycerol triacetate added with the absolute coffee oil is uniformly sprayed on the filter tow according to 7 wt% of the weight of the filter tow to prepare a filter stick, and then the filter stick is prepared into a cigarette through conventional cigarette rolling to carry out sensory evaluation and smoking. The results show that: the cigarette added with the coffee absolute of the invention has better aroma quantity, aroma richness and elegance than a control cigarette (namely, the cigarette without the coffee absolute of the invention). Or the like, or, alternatively,
in the preparation process of cigarette paper, the coffee absolute oil prepared by the invention is uniformly coated on the cigarette paper according to the proportion of 1.0 time of the weight of the cigarette paper, and then the cigarette paper coated with the coffee absolute oil is rolled into cigarettes for sensory evaluation and smoking evaluation. The results show that: the cigarette added with the coffee absolute of the invention has outstanding coffee characteristic smell, and the amount of aroma, quality and comfort of cigarette smoking are superior to those of a control sample (namely, the cigarette without the coffee absolute of the invention).
Example 3
In the preparation process of the electronic cigarette liquid, the coffee absolute oil is added into the coffee-flavored electronic cigarette liquid in a proportion of 5% by weight. The results show that: the coffee absolute oil has higher total score, and has the advantages of good aroma quality and sufficient aroma quantity; and the following characteristics that the offensive odor is light, the aftertaste is cleaner, and the electronic cigarette is superior to a control sample (namely the electronic cigarette without the coffee absolute oil obtained by the invention).
Example 4
In the process of making the cigarette without burning by heating, the coffee absolute prepared by the invention is added to the slice of the cigarette without burning by heating in a ten-thousandth ratio, and sensory evaluation is carried out by taking the coffee absolute prepared by the invention as a reference sample. The results show that: the heating non-combustion cigarette coffee added with the coffee absolute of the invention has the advantages of prominent characteristic of roasted aroma and nut aroma, more sufficient aroma amount and improved smoking quality, and is superior to a control sample (namely, the non-combustion cigarette without the coffee absolute of the invention).
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. The application of the coffee absolute to perfuming of cigarettes, electronic cigarettes or non-burning cigarettes is characterized in that the preparation method of the coffee absolute uses the following devices:
-an ultrasonic extraction tank (1) with a feed inlet (11) in the upper part and a discharge outlet (14) in the lower part, and a filter sieve plate (13) in the upper part of the discharge outlet (14);
-a chromatography column (2);
-an air compressor (3);
-a concentration tank (4);
-a reverse resin column (5);
-a condenser (6);
-a vacuum pump (8);
-a solvent recovery tank (7);
the connection mode of each part is as follows:
the ultrasonic extraction tank (1) is communicated with an inlet at the upper part of the chromatographic column (2) through a discharge hole (14) of the ultrasonic extraction tank, and an outlet at the lower part of the chromatographic column (2) is communicated with the upper part of the concentration tank (4); the upper part of the concentration tank (4) is communicated with an inlet of the condenser (6), and an outlet at the upper end of the condenser (6) is communicated with the vacuum pump (8); the outlet at the lower end of the condenser (6) is communicated with the solvent recovery tank (7); the air compressor (3) is respectively communicated with the upper port of the ultrasonic extraction tank (1) and the upper port of the concentration tank (4); the outlet at the lower part of the concentration tank (4) is communicated with the reverse resin column (5);
the preparation method comprises the following steps:
adding coffee raw materials into the ultrasonic extraction tank (1), sealing a feeding port and a discharging port, adding methyl acetate 4-6 times of the weight of the coffee raw materials, and performing ultrasonic extraction at 40-50 ℃ for 30-40 min;
secondly, starting an air compressor (3) after extraction is finished, pressurizing the ultrasonic extraction tank (1) in the step I, and enabling the extraction liquid to enter a concentration tank (4) through a chromatographic column (2) through a filter sieve plate (13) of a discharge port (14);
thirdly, heating the concentration tank (4) to 75-85 ℃, starting a vacuum pump (8) and a condenser (6), and concentrating the extract liquor under reduced pressure until the methyl acetate is evaporated to dryness to obtain a paste extracted from coffee;
adding 95 wt% ethanol into the concentration tank (4) to completely dissolve the paste obtained in the step (c), starting an air compressor (3) to pressurize the concentration tank (4), and allowing the liquid to completely pass through a reverse resin column (5);
fifthly, adding propylene glycol with the weight 3-5 times of that of the paste into the liquid obtained in the step IV, and removing ethanol by reduced pressure evaporation to obtain the coffee absolute;
the diameter of the chromatographic column (2) is 2:1, silica gel particles and anhydrous sodium sulfate particles are filled in the chromatographic column, and the particle sizes of the silica gel particles and the anhydrous sodium sulfate particles are respectively 100-200 meshes; BOSHI reversed-phase resin is filled in the reversed-phase resin column (5); the diameter of the BOSHI reverse phase resin filling is 1:2, and the particle size of the BOSHI reverse phase resin filling is 35-75 mu m.
2. Use according to claim 1, characterized in that the upper end of the ultrasonic extraction tank (1) is in communication with a first pump (B1); the upper end of the concentration tank (4) is communicated with a second pump (B2); all the parts are communicated through a pipeline, and a valve (F) is arranged on the pipeline.
3. The use of claim 1, wherein the step (c) is performed before the extract is concentrated under reduced pressure, and the method further comprises the steps of washing the ultrasonic extraction tank (1) by using methyl acetate, and then feeding the methyl acetate washing solution into the concentration tank (4) through the chromatographic column (2).
4. The use according to claim 1, wherein before said removing ethanol by evaporation under reduced pressure, the method further comprises washing the concentration tank (4) with 95 wt% ethanol of 1/5-1/4 by weight of said paste, and passing the ethanol washing solution through a reverse resin column (5) to remove ethanol by evaporation under reduced pressure.
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| CN112473174A (en) * | 2020-12-09 | 2021-03-12 | 海南一哟食品有限公司 | Method for accelerating coffee extraction by adopting ultrasonic waves |
| CN114259079B (en) * | 2022-02-14 | 2023-05-12 | 云南中烟工业有限责任公司 | Method for improving quality of dry tobacco by co-fermentation of coffee feature extract and sweet wormwood |
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| JP5565896B2 (en) * | 2009-06-17 | 2014-08-06 | 小川香料株式会社 | Extract extraction apparatus and extract production method |
| CN202705336U (en) * | 2012-05-04 | 2013-01-30 | 发泰（天津）科技有限公司 | Separating and collecting device for volatile oil in natural plants |
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| CN204816541U (en) * | 2015-08-25 | 2015-12-02 | 王婧婧 | Apparatus for producing of thermal response essence |
| CN205699574U (en) * | 2016-06-29 | 2016-11-23 | 重庆骄王天然产物股份有限公司 | A kind of efficient concentration equipment produced for coffee-extract |
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