CN109181876B - Efficient preparation method of rose absolute for flavoring tobacco - Google Patents
Efficient preparation method of rose absolute for flavoring tobacco Download PDFInfo
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- CN109181876B CN109181876B CN201811097791.9A CN201811097791A CN109181876B CN 109181876 B CN109181876 B CN 109181876B CN 201811097791 A CN201811097791 A CN 201811097791A CN 109181876 B CN109181876 B CN 109181876B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention discloses a preparation method of rose 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: firstly, carrying out ultrasonic extraction on a rose raw material; purifying through a chromatographic column (2); thirdly, concentration; purifying through a reverse resin column (5); fifthly, removing ethanol under reduced pressure to obtain the rose absolute. The device can be used for efficiently extracting and purifying the rose absolute, and the obtained rose 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 essence and spice for cigarettes, and particularly relates to a method for efficiently preparing rose absolute and application of the rose 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.
The rose plant is a deciduous bush with dense stems and sharp spines, has both color and fragrance, and is an economic flower integrating appreciation, eating and medicinal functions. The rose oil is the crown of fresh flower oil, has elegant, soft, exquisite, sweet and honey fragrance, has the fragrance of rose flowers with fragrance overflowing, has very strong fragrance, has the effects of bacteriostasis, antioxidation, anti-sensitivity, moisture preservation, cell regeneration promotion and the like, has better effects on the aspects of respiratory system, digestive system, circulatory system and reproductive system, has the effects of suppressing, reducing pressure, improving sleep, resisting conflict, relieving tension, resisting depression and the like on the aspect of emotion, has high price, is equivalent to gold in international market price, has the reputation of 'essential oil queen' and 'liquid gold', is the most important and most common famous and precious flower fragrance raw material in fragrance blending, is widely used in foods, high-grade cosmetics and tobaccos, and can also be used as a medicinal and food additive.
The traditional rose extract is mainly used for perfuming cigarettes with products such as extractum, absolute oil, essential oil and the like. The existing preparation method of rose absolute oil for perfuming cigarettes mainly adopts methods such as a solvent extraction method, a supercritical extraction method, a molecular distillation method and the like, and the methods have high production cost and low absolute oil rate. In addition, the existing rose extract is used in a novel rose product due to complex components, so that the smoking experience of electronic cigarettes and cigarettes which are not combusted by heating is influenced.
Disclosure of Invention
The invention designs a method for preparing rose 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 rose absolute can be used for flavoring traditional cigarettes, and can also be used for novel tobacco products (such as electronic cigarettes or non-combustible cigarettes), so that the rose essential aroma characteristics of the cigarettes, the electronic cigarettes or the cigarettes which are not combusted when heated are effectively enhanced, the richness and aftertaste of aroma are improved, the miscellaneous gas of the products for smoking is covered, the smoking comfort of the cigarettes, the electronic cigarettes or the cigarettes which are not combusted when heated is improved, the smoke quality is improved, and the consumers are better in smoking feeling.
The technical scheme of the invention is as follows:
the invention discloses a preparation method of rose 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 rose 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 rose 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 the rose;
fourthly, 95wt% 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 by reduced pressure evaporation to obtain the rose 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 95wt% 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 application of the rose absolute oil prepared by the preparation method in perfuming cigarettes, electronic cigarettes or non-combustible cigarettes.
The steps of the method for preparing the rose absolute oil are described in the following by combining the attached drawings, and specifically the steps are as follows:
A. extraction of rose raw material
For extracting aroma components in rose raw materials, common solvents comprise ethanol, petroleum ether, ethyl acetate and the like, the ethyl acetate has moderate polarity, can dissolve most of the aroma components and glycoside compounds thereof, and the dissolution of saccharide compounds with large content in rose is extremely low, so that the solvent is an ideal extraction solvent, but the ethyl acetate has high boiling point which reaches 77.5 ℃, and has high energy consumption and easy residue in the sample concentration process. 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 rose raw material used is Yunnan plateau rose. Freeze drying flos Rosae Rugosae, pulverizing into 15-20 mesh, adding into ultrasonic extraction tank from feed inlet 11 of constant temperature ultrasonic extraction tank 1 shown in figure 1, sealing feed inlet and discharge outlet, starting first pump B1, adding methyl acetate 4-6 times of flos Rosae Rugosae raw material, and performing ultrasonic extraction at 40-50 deg.C for 30-40 min. After extraction, a valve F2 in FIG. 1 is opened, an air compressor 3 is started to pressurize the ultrasonic extraction tank 1, and the rose extract passes through a filtering sieve plate 13 on a discharge port 14 and is led to a chromatographic column 2 of silica gel particles 22 with anhydrous sodium sulfate particles 21.
B. Purification of rose extract by using anhydrous sodium sulfate particle and silica gel particle composite chromatographic column 2
Because the rose raw material contains water, the water and a small amount of large-polarity components such as sugar are dissolved in the rose extract in the extraction process of the rose essential 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 rose 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 rose 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 liquor is transferred to 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 liquor under reduced pressure until methyl acetate is evaporated to dryness to obtain a paste of the rose extract. The solvent methyl acetate is cooled by the condenser 6 again and then enters the solvent recovery tank 7 for the next extraction of the rose sample.
D. Rose 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. Starting the concentration tank 4 again and evaporating the methyl acetate to dryness under reduced pressure to obtain the paste of rose essential oil. The methyl acetate obtained by the concentration can be used for extracting the rose sample next time.
E. Reversed phase resin column chromatography purification of rose extract
Because the methyl acetate extract of the rose contains a large amount of small polar components such as wax, fatty acid and the like which are unfavorable for the cigarette sense, the extract product needs to be further purified by reversed-phase resin column chromatography to remove the 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 95wt% 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, 95wt% ethanol is added again to the concentration tank 4 to wash the concentration tank 4, the 95wt% 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 95wt% ethanol is used for washing the chromatographic column 5, so that the fragrance components in the rose essential oil are not retained on the reverse resin chromatographic column 5, and the 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 fragrance components from the impurities such as wax, fatty acid and the like in the rose essential oil can be effectively achieved, thereby improving the quality of the rose essential oil.
Mixing the 95wt% ethanol solutions, adding 3-5 times of propylene glycol into the solution, and evaporating under reduced pressure to remove ethanol to obtain the rose absolute. The propylene glycol is added to increase the fluidity of the rose absolute and stabilize the rose essential fragrance component in the rose absolute.
The yield of the obtained rose absolute oil is 3.2-4.8%. The obtained rose absolute oil is uniform and transparent brown oily fluid with rich rose 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 rose 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 can be used for extracting the rose sample next time.
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 rose absolute oil in cigarette flavoring
a. The rose absolute oil prepared by the method is used in the cut tobacco of the cigarette, the rose absolute oil is added to the cut tobacco of the cigarette according to the proportion of five to one ten thousandth of the weight of the cut tobacco, and the cut tobacco is made into the finished product of the cigarette for evaluation. The results show that: the rose absolute oil prepared by the invention can effectively endow cigarette products with elegant and natural rose characteristic fresh and sweet fragrance, improve the fragrance quantity and quality of cigarette smoking, cover up the miscellaneous gas of cigarette smoking, improve the comfort of cigarette smoking, and is superior to a control sample (namely, the cigarette without the rose absolute oil prepared by the invention). Or the like, or, alternatively,
b. in the process of forming a cigarette filter, the rose absolute oil obtained by the invention is added into triacetyl glycerine according to the amount which is 1-1.5 wt% of the amount of the triacetyl glycerine of the plasticizer, then the triacetyl glycerine added with the rose absolute oil is uniformly sprayed on filter tow according to 6-8 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 rose absolute oil has better fragrance quantity, fragrance richness and elegance than a control cigarette, has the unique fresh and sweet fragrance characteristic of roses, and is better than a control sample (namely the cigarette without the rose absolute oil obtained by the invention). Or the like, or, alternatively,
c. in the preparation process of the cigarette paper, the rose absolute oil 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 rose absolute oil is rolled into a cigarette for sensory evaluation and smoking evaluation. The results show that: the cigarette with the rose absolute oil added into the cigarette paper has the advantages that the rose fragrance is very outstanding, and the amount of fragrance, quality and comfort of cigarette smoking are superior to those of a control sample (namely, the cigarette without the rose absolute oil obtained by the invention).
I. Application of obtained rose absolute in electronic cigarette smoke oil
In the process of preparing the cigarette liquid of the electronic cigarette, the rose absolute oil 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 rose absolute can also be used in the electronic cigarette liquid such as fruit rose, mint rose and the like in a proportion of 0.1-3 wt%. The results show that: the electronic cigarette containing the electronic cigarette tar has higher total smoking score, and is mainly characterized in that the quality of aroma is good, the amount of aroma is sufficient, and the burnt feeling of product smoking is obviously improved; and the following characteristics that the mixed gas is light, the aftertaste is cleaner, and the electronic cigarette is superior to a control sample (namely the electronic cigarette without the rose absolute oil obtained by the invention).
J. Application of rose absolute in heating non-burning cigarette
In the manufacturing process of the cigarette without burning by heating, the rose absolute oil prepared by the invention is added to the sheet of the cigarette without burning by heating according to the proportion of one to five parts per million, and the rose absolute oil prepared by the invention is not added to be used as a reference sample for sensory evaluation. The results show that: the rose absolute oil added into the cigarette without burning after heating has the advantages of prominent unique fresh and sweet fragrance characteristic of rose, more sufficient fragrance amount and improved smoking quality, and is superior to a control sample (namely, the cigarette without burning without adding the rose absolute oil 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 of aroma components in the tobacco leaf sample, but also can not extract large polar components such as saccharides and the like in the rose in the extraction process, and the obtained rose absolute oil 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 rose essential oil efficiently, the anhydrous sodium sulfate-silica gel composite chromatographic column can effectively remove moisture and large-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 rose absolute, the operation process is simplified, the loss of aroma components in the production process is less, and the yield of the obtained rose absolute 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 latent aroma compounds) in the roses are retained in the rose absolute, effectively avoids the loss of the aroma components, and the latent aroma compounds can be released 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 rose essential oil 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 rose essential oil 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 rose essential oil obtained by using the device disclosed by the invention has higher purity, is used in cigarettes or novel tobacco products (such as electronic cigarettes or non-combustible cigarettes), effectively strengthens the rose essential aroma characteristics of the cigarettes, the electronic cigarettes or the cigarettes which are not combusted when heated, covers the miscellaneous gas of product smoking, promotes and improves the smoking comfort of the cigarettes, the electronic cigarettes or the cigarettes which are not combusted when heated, 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 materials are prepared by freezing Yunnan plateau rose, crushing the frozen Yunnan plateau rose into 15 meshes, feeding the frozen Yunnan plateau rose into 200kg, crushing a sample into 15-20 meshes, adding the crushed Yunnan plateau rose 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 the rose 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 95wt% 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 95wt% 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 95wt% 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 the ethanol solutions, adding propylene glycol 4 times the weight of the paste, and evaporating under reduced pressure to remove ethanol to obtain the rose absolute with a yield of 4.2%. The obtained rose absolute is uniform and transparent brown oily fluid, has strong rose characteristic fragrance, has good solubility in solvents such as ethanol, propylene glycol and the like, and is an ideal cigarette additive.
Example 2
The rose absolute oil prepared by the method is used in cigarette tobacco shreds, the rose absolute oil is added to the cigarette tobacco shreds according to the proportion of five hundred thousandth of the weight of the tobacco shreds, and the tobacco shreds are made into cigarette finished products for evaluation. The results show that: the rose absolute oil prepared by the invention can effectively strengthen the rose intrinsic fragrance characteristic of cigarette products, improve the fragrance quantity and the fragrance quality of cigarette smoking, cover the impure gas of cigarette smoking, and improve the comfort of cigarette smoking, and is superior to a control sample (namely, the cigarette without the rose absolute oil prepared by the invention). Or the like, or, alternatively,
in the process of forming a cigarette filter, the rose absolute oil obtained by the invention is added into triacetyl glycerine according to the amount of 1 wt% of the plasticizer triacetyl glycerine, then the triacetyl glycerine added with the rose absolute oil is uniformly sprayed on 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 rose absolute oil has better fragrance quantity, fragrance richness and elegance than a control cigarette and better than a control sample (namely the cigarette without the rose absolute oil obtained by the invention). Or the like, or, alternatively,
in the preparation process of the cigarette paper, the rose absolute oil 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 rose absolute oil is rolled into a cigarette for sensory evaluation and smoking evaluation. The results show that: the cigarette with the rose absolute oil added into the cigarette paper has the advantages that the rose fragrance is very outstanding, and the amount of fragrance, quality and comfort of cigarette smoking are superior to those of a control sample (namely, the cigarette without the rose absolute oil obtained by the invention).
Example 3
In the preparation process of the electronic cigarette liquid, the rose absolute oil is added into the rose-flavor electronic cigarette liquid according to the proportion of 5% by weight. The results show that: the rose absolute oil has higher total score and has the advantages of good quality and sufficient fragrance; and the following characteristics that the mixed gas is light, the aftertaste is cleaner, and the electronic cigarette is superior to a control sample (namely the electronic cigarette without the rose absolute oil obtained by the invention).
Example 4
In the process of manufacturing the cigarette without burning by heating, the rose absolute oil prepared by the invention is added to the slice of the cigarette without burning by heating in a ten-thousandth ratio, and the rose absolute oil prepared by the invention is not added to be used as a reference sample for sensory evaluation. The results show that: the rose absolute oil added into the cigarette without burning after heating has the advantages of prominent unique fresh and sweet fragrance characteristic of rose, more sufficient fragrance amount and improved smoking quality, and is superior to a control sample (namely, the cigarette without burning without adding the rose absolute oil obtained by 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 rose absolute to perfuming of cigarettes, electronic cigarettes or non-burning cigarettes is characterized in that the preparation method of the rose 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 rose 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 rose 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 the rose;
adding 95wt% 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 which is 3-5 times of the weight of the paste into the liquid obtained in the step IV, and removing ethanol by reduced pressure evaporation to obtain the rose 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 and height of the BOSHI reversed-phase resin filling are 1:2, and the particle size of the BOSHI reversed-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 95wt% 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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