CN111808681A - Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes - Google Patents
Preparation method of lycium ruthenicum murr spice for cigarettes and application of lycium ruthenicum murr spice in cigarettes Download PDFInfo
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- CN111808681A CN111808681A CN202010699764.XA CN202010699764A CN111808681A CN 111808681 A CN111808681 A CN 111808681A CN 202010699764 A CN202010699764 A CN 202010699764A CN 111808681 A CN111808681 A CN 111808681A
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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
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
- B01D61/146—Ultrafiltration comprising multiple ultrafiltration steps
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Abstract
The invention provides a preparation method of a lycium ruthenicum spice for cigarettes, which comprises the following steps: crushing and sieving the lycium ruthenicum, adding sucrose with the mass ratio of 3%, then taking ethanol as a solvent, extracting by a Soxhlet extraction method, performing ultrasonic extraction, filtering, and concentrating to obtain a lycium ruthenicum extract; dissolving the Lycium ruthenicum Murr extract with ethanol, and filtering with ceramic membrane to remove macromolecular substances; filtering the ceramic membrane permeate by an organic membrane to remove small molecular substances affecting the fragrance and the taste of the filtered part, and distilling and concentrating the intercepted part of the organic membrane under reduced pressure to obtain the Lycium ruthenicum Murr spice. The invention also provides the application of the spice in cigarettes: diluting fructus Lycii spice for cigarette, and spraying onto tobacco shred to make cigarette. After the perfume is added, the irritation and miscellaneous gas can be obviously reduced, the sweet feeling is increased, and the aftertaste is comfortable.
Description
Technical Field
The invention belongs to the technical field of preparation of cigarette additives, and particularly relates to a preparation method of a lycium ruthenicum spice for cigarettes and application of the lycium ruthenicum spice in cigarettes.
Background
Lycium ruthenicum Murr is a special wild plant in northwest China, and mature fruits of the Lycium ruthenicum Murr are rich in anthocyanin, lycium barbarum polysaccharide, amino acid, vitamin and trace elements. Loshuting et al measure the volatile components in Lycium ruthenicum Murr by SPME-GC/MS method. The results show that the volatile components in Lycium ruthenicum Murr contain fragrance substances such as limonene, caryophyllene, citral, beta-ionone, ethyl laurate, farnesyl acetaldehyde and the like, and many of the volatile components are important components of natural perfume. The application of Lycium ruthenicum Murr products in cigarettes is rarely reported.
The natural fragrant components extracted by the conventional extraction method, such as the Soxhlet extraction method and the like, inevitably contain impurities, such as protein, starch, wax and the like, which not only affect the quality of natural spices, but also affect the perfuming effect of cigarettes, and simultaneously have certain influence on the smoking safety of the cigarettes.
Membrane separation technology refers to a technology in which a mixture of molecules of different particle sizes on a molecular level is selectively separated while passing through a semipermeable membrane. The membrane separation technology can effectively remove macromolecular substances which have negative influence on the sensory quality of smoke while keeping the original characteristic fragrance of the extract, thereby achieving the purpose of improving the quality of the extract. However, the preparation of the tobacco flavor by separating the lycium ruthenicum extract by using a membrane separation technology is not seen.
The prepared lycium ruthenicum extract is separated and purified by a membrane separation technology, so that impurities such as protein, starch, wax and the like in the extract can be removed, meanwhile, small molecular substances influencing the fragrance can be removed by ultrafiltration or nanofiltration membrane separation and interception, and refined natural perfume components are obtained.
Disclosure of Invention
The invention aims to provide a preparation method of lycium ruthenicum murr spice for cigarettes, which has an obvious aroma enhancement effect and few impurities, aiming at the defects of the existing preparation method of the spice for cigarettes, particularly the lycium ruthenicum murr spice for cigarettes. The invention is realized by the following technical scheme:
in order to achieve the aim, the preparation method of the lycium ruthenicum spice for the cigarettes comprises the following steps: (1) crushing: pulverizing dried fructus Lycii into coarse powder, and sieving with 60-80 mesh stainless steel screen;
(2) soxhlet extraction: accurately weighing Lycium ruthenicum Murr powder, placing in a Soxhlet extractor, adding sucrose 2-5 wt%, adding 50-100% ethanol 5-10 times of the weight of the powder, heating at 50-100 deg.C, and refluxing for 1-3 hr. Filtering to obtain filtrate A and filter residue.
(3) Ultrasonic extraction: and (4) carrying out ultrasonic extraction on the filter residue obtained in the step (3), adding 4-8 times of 40-80% ethanol water solution, and carrying out ultrasonic treatment at 50-70 ℃ for 30-70 min and 50-60 kHz ultrasonic frequency. Centrifuging to obtain filtrate B, and mixing the filtrate A and the filtrate B to obtain the Lycium ruthenicum Murr extract.
(4) Alcohol collection and concentration: and (4) carrying out reduced pressure distillation and concentration on the mixed extracting solution in the step (4) in a rotary evaporator to obtain an extractum, thus obtaining the lycium ruthenicum extract.
(5) And (3) separating with a microfiltration membrane: accurately weighing Lycium ruthenicum Murr extract, placing into a quantitative glass container, adding 40-50 times of 20-50% ethanol, and dissolving to obtain solution H1. After complete dissolution, filtering with 50-200nm ceramic microfiltration membrane, wherein the interception section is H2;
(6) and (3) ultrafiltration membrane separation, namely filtering the microfiltration membrane permeate by using an organic membrane with the concentration of 10-500kd, wherein the interception section is marked as H3, and the permeation section is marked as H4.
(7) Distilling H3 part under reduced pressure to relative density of 1.05-1.15 to obtain Lycium ruthenicum Murr essence.
Further, in the step (2), after sucrose with a mass ratio of preferably 3% is added, the amount of ethanol added is preferably 5 to 8 times, and more preferably 5 to 6 times; the concentration of the ethanol is preferably 70-95%, and more preferably 85-90%; the heating temperature is preferably 65-85 ℃, and more preferably 75-80 ℃;
further, in the step (3), ethanol is added preferably in an amount of 5 to 7 times, and more preferably in an amount of 5 to 6 times; the concentration of the ethanol is preferably 50% -70%, and is further preferably 55% -60%; the ultrasonic temperature is 60-70 ℃, and further preferably 60-65 ℃; the ultrasonic treatment time is preferably 40 to 60min, and more preferably 45 to 50 min.
Further, in the step (5), the pore diameter of the microfiltration membrane is preferably 50-100 nm;
further, in the step (6), the pore size of the ultrafiltration membrane is preferably 50-200KD, and more preferably 50-100 KD;
the lycium ruthenicum murr is one or more of Xinjiang, Qinghai and Gansu.
The invention discloses application of a lycium ruthenicum spice for cigarettes, which comprises the following steps: diluting the lycium ruthenicum spice for the cigarettes by using an organic solvent, wherein the dilution times are 10-100 times; before preparing cigarettes, the lycium ruthenicum spice for cigarettes is sprayed on tobacco shreds according to the mass ratio of 0.02-1%, and then the cigarettes are prepared.
Further, in the application of the lycium ruthenicum spice for the cigarettes, the dilution times of an organic solvent are optimized to be 20-70 times, and further optimized to be 40-50 times; the adding proportion of the tobacco shreds is optimized to be 0.05-0.5 percent, and is further optimized to be 0.1-0.3 percent.
Further, the organic solvent is ethanol, propylene glycol, sorbitol, xylitol or glycerol, or a mixture of any 2 or more thereof.
The application effect of the lycium ruthenicum spice for the cigarettes is characterized in that after the lycium ruthenicum spice is added into the cigarettes, the irritation and the miscellaneous gas can be obviously reduced, the sweet feeling is increased, and the aftertaste is comfortable.
The invention has the advantages that:
compared with the prior art, the membrane separation microfiltration method is utilized to remove a large amount of protein, pectin, starch, wax, cellulose and pigment substances contained in the lycium ruthenicum extract, and the problem of poor sensory comfort caused by burning and sucking the components added into tobacco shreds is avoided. In addition, the invention removes some small molecular substances which influence the aroma quality and the aroma quantity and have irritation in the lycium ruthenicum extract by using a membrane separation ultrafiltration method, reserves proper aroma components in the lycium ruthenicum extract as far as possible, reduces miscellaneous gas and irritation, and removes large molecular and small molecular impurities in the lycium ruthenicum extract, so that the application effect of the lycium ruthenicum extract is better.
The specific implementation mode is as follows:
the first embodiment is as follows:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 100g of lycium ruthenicum powder, adding 3% of cane sugar by mass ratio, wrapping with filter paper, loading into a Soxhlet extractor, adding 500mL of 90% ethanol, heating to 80 ℃, and heating and refluxing for 2 h. Filtering to obtain primary extract, placing the filter residue into a beaker, adding 5 times of 60% ethanol solution by mass, performing ultrasonic extraction at an ultrasonic frequency of 50kHz-60kHz and at an ultrasonic temperature of 60 ℃ for 50min, filtering to obtain secondary extract, mixing the two extracts, and performing reduced pressure distillation in a rotary evaporator until no ethanol flows out to obtain Lycium ruthenicum Murr extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with a 50nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 100kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.10 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with 50 times of ethanol, spraying onto tobacco shred at a ratio of 0.2%, rolling into cigarette, and collecting part H1, and performing the same method as control.
Example two:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 50g of lycium ruthenicum powder, adding 3% of sucrose by mass ratio, wrapping with filter paper, loading into a Soxhlet extractor, adding 500mL of 50% ethanol, heating to 50 ℃, and heating and refluxing for 2.5 h. Filtering to obtain primary extract, placing filter residue into a beaker, adding 55% ethanol solution with mass of 6 times, performing ultrasonic extraction at ultrasonic frequency of 50kHz-60kHz and ultrasonic temperature of 65 ℃ for 50min, filtering to obtain secondary extract, mixing the two extracts, and performing reduced pressure distillation in a rotary evaporator until no ethanol flows out to obtain Lycium ruthenicum Murr extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with a 200nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 500kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.15 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with propylene glycol 100 times, spraying onto tobacco shred at a ratio of 1%, and rolling into cigarette. Another portion H1 was taken and used in the same manner as a control.
Example three:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 150g of lycium ruthenicum powder, adding 3% of sucrose by mass ratio, wrapping with filter paper, loading into a Soxhlet extractor, adding 450mL of 100% ethanol (absolute ethanol), heating to 90 ℃, and heating and refluxing for 1 h. Filtering to obtain a primary extracting solution, putting filter residues into a beaker, adding 70% ethanol solution with the mass being 7 times of that of the filter residues, carrying out ultrasonic extraction at the ultrasonic frequency of 50kHz-60kHz and at the ultrasonic temperature of 70 ℃ for 40min, filtering to obtain a secondary extracting solution, combining the two extracting solutions, carrying out reduced pressure distillation in a rotary evaporator, and carrying out reduced pressure distillation on the filtrate until no ethanol flows out to obtain the lycium ruthenicum extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with 100nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 10kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.05 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with glycerol 10 times, spraying onto tobacco shred at a ratio of 0.02%, and making into cigarette. Another portion H1 was taken and used in the same manner as a control.
Example four:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 100g of lycium ruthenicum powder, wrapping the powder with filter paper, loading the wrapped powder into a Soxhlet extractor, adding sucrose with the mass ratio of 3%, adding 800mL of 70% ethanol, heating to 70 ℃, and heating and refluxing for 1.5 h. Filtering to obtain primary extract, placing the filter residue into a beaker, adding 5 times of 50% ethanol solution by mass, performing ultrasonic extraction at an ultrasonic frequency of 50kHz-60kHz and at an ultrasonic temperature of 70 ℃ for 60min, filtering to obtain secondary extract, mixing the two extracts, and performing reduced pressure distillation in a rotary evaporator until no ethanol flows out to obtain Lycium ruthenicum Murr extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with a 200nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 50kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.08, thus obtaining the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with sorbitol 30 times, spraying onto tobacco shred at a ratio of 0.5%, and making into cigarette. Another portion H1 was taken and used in the same manner as a control.
Example five:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 100g of lycium ruthenicum powder, wrapping the powder with filter paper, loading the wrapped powder into a Soxhlet extractor, adding sucrose with the mass ratio of 3%, adding 600mL of 60% ethanol, heating to 60 ℃, and heating and refluxing for 2 h. Filtering to obtain a primary extracting solution, putting filter residues into a beaker, adding 75% ethanol solution with the mass being 7 times of that of the filter residues, carrying out ultrasonic extraction at the ultrasonic frequency of 50kHz-60kHz and the ultrasonic temperature of 55 ℃ for 30min, filtering to obtain a secondary extracting solution, combining the two extracting solutions, carrying out reduced pressure distillation in a rotary evaporator, and carrying out reduced pressure distillation on the filtrate until no ethanol flows out to obtain the lycium ruthenicum extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with 100nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 200kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.13 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with xylitol 80 times, spraying onto tobacco shred at a ratio of 0.05%, and rolling into cigarette. Another portion H1 was taken and used in the same manner as a control.
Example six:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 100g of lycium ruthenicum powder, wrapping the powder with filter paper, loading the wrapped powder into a Soxhlet extractor, adding sucrose with the mass ratio of 3%, adding 400mL of 75% ethanol, heating to 55 ℃, and heating and refluxing for 1.5 h. Filtering to obtain primary extract, placing the filter residue into a beaker, adding 4 times of 50% ethanol solution by mass, performing ultrasonic extraction at an ultrasonic frequency of 50kHz-60kHz and an ultrasonic temperature of 35 ℃ for 50min, filtering to obtain secondary extract, combining the two extracts, and performing reduced pressure distillation in a rotary evaporator until no ethanol flows out to obtain Lycium ruthenicum Murr extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with a 50nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 30kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.07 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii spice for cigarette with ethanol/propylene glycol mixed solution (ethanol: propylene glycol 1:1) xylitol 40 times, spraying onto tobacco shred at a ratio of 0.1%, and rolling into cigarette. Another portion H1 was taken and used in the same manner as a control.
Example seven:
pulverizing dried fructus Lycii into coarse powder, and sieving with 60 mesh stainless steel screen. Accurately weighing 100g of lycium ruthenicum powder, wrapping the powder with filter paper, loading the wrapped powder into a Soxhlet extractor, adding sucrose with the mass ratio of 3%, adding 400mL of 75% ethanol, heating to 55 ℃, and heating and refluxing for 1.5 h. Filtering to obtain primary extract, placing the filter residue into a beaker, adding 4 times of 50% ethanol solution by mass, performing ultrasonic extraction at an ultrasonic frequency of 50kHz-60kHz and an ultrasonic temperature of 35 ℃ for 50min, filtering to obtain secondary extract, combining the two extracts, and performing reduced pressure distillation in a rotary evaporator until no ethanol flows out to obtain Lycium ruthenicum Murr extract. 10g of Lycium ruthenicum Murr extract is accurately weighed and placed in a 1000mL beaker, and 500mL of 20% ethanol is added for dissolution (H1). After complete dissolution, filtering with a 50nm ceramic microfiltration membrane, wherein the interception section is H2; and filtering the permeate of the microfiltration membrane by using a 30kd organic membrane, wherein the interception section is marked as H3, and the permeation section is marked as H4. And distilling part of H3 under reduced pressure until the relative density is 1.07 to obtain the black wolfberry spice for cigarettes. Diluting fructus Lycii aroma for cigarette with xylitol/sorbitol mixed solution (xylitol: sorbitol 1:1) 60 times, spraying onto tobacco shred at a ratio of 0.1%, and rolling into cigarette. Another part N1 was taken and the same procedure was followed as a control.
Example eight
1. Analysis of volatile components of lycium ruthenicum spice for cigarettes
Accurately weighing 1.0g of the lycium ruthenicum spice for the cigarettes prepared in the first example into a separating funnel, adding 20mL of 20% ethanol, shaking for dissolving, and adding 50mL of dichloromethane for extraction for 24 hours after complete dissolution. Taking down the clear liquid, adding a proper amount of anhydrous sodium sulfate, and standing overnight. Concentrate to 1mL for GC-MS analysis.
The GC-MS conditions were: a chromatographic column: HP-5MS capillary column (60m 0.32mm 0.25 μm); sample inlet temperature: 250 ℃; temperature programming: maintaining the initial temperature at 50 deg.C for 3min, then increasing to 260 deg.C at 4 deg.C, and maintaining for 5 min; vaporization temperature: 270 ℃; carrier gas: he, 1mL min-1; the split ratio is as follows: 5: 1; an ionization mode: an EI source; detector temperature: FID, 300 ℃; transmission line temperature: 280 ℃; ionization energy: 70 eV; ion source temperature: 230 ℃; mass scan range: 30-700 amu; searching a spectrum library: NIST11 library.
As can be seen from Table 1, 20 substances were co-detected from the Lycium ruthenicum Murr flavor for cigarettes. The furfural is characterized by bread aroma and butter aroma, so that the smoke has sweet taste; the methyl cyclopentenolone has coffee-like caramel-like pleasant aroma, has maple-like sweet aroma when diluted, and is a good flavoring agent and low-heat sweetener; phenylacetaldehyde is naturally found in essential oils such as rose oil and orange oil. The product has strong hyacinth fragrance similar to green leaf fragrance, and can be widely used in cigarette flavoring, meanwhile, phenylacetaldehyde is a widely used organic synthetic intermediate, and acetal perfume can be prepared in perfume aspect; the ethyl linoleate can increase the sweet and soft effects; the methyl stearate can soften smoke and increase sweet taste, so that the cigarette flavor shows certain burnt sweet flavor, thickness and long-lasting feeling. The refined and enriched flavor components can be the material basis of the lycium ruthenicum murr flavor for cigarettes for increasing the cigarette fragrance and improving the mouthfeel.
TABLE 1 volatile ingredients of Lycium ruthenicum Murr spice for tobacco
2. Sensory evaluation of application of lycium ruthenicum murr spice for cigarettes
The 7-style cigarette black wolfberry spice prepared in the first embodiment to the seventh embodiment and the cigarette prepared by rolling the H1 black wolfberry spice in the seven preparation processes are adopted. The cigarettes were compared with control cigarettes without any lycium ruthenicum perfume, which were submitted to a comprehensive test by 7 panelists and the results (table 2) showed that: compared with a control sample, after the lycium ruthenicum mill spice for cigarettes is added into cigarettes, the fragrance amount can be obviously increased, the fragrance is coordinated, the sweet feeling is increased, the irritation and the miscellaneous gas can be reduced, and the aftertaste is comfortable.
TABLE 2 influence of Lycium ruthenicum Murr spice for cigarette on sensory quality of cigarette
Claims (11)
1. The preparation method of the lycium ruthenicum for the cigarettes is characterized by comprising the following steps of:
(1) crushing: pulverizing dried fructus Lycii into coarse powder, and sieving with 60-80 mesh stainless steel screen;
(2) soxhlet extraction: weighing a certain amount of lycium ruthenicum raw material, placing the raw material into a Soxhlet extractor, adding sucrose with the mass ratio of 2-5%, adding 50% -100% ethanol with the mass ratio of 5-10 times, heating to 50-100 ℃, and heating and refluxing for 1-3 h; centrifuging to obtain filtrate A and filter residue;
(3) ultrasonic extraction: carrying out ultrasonic extraction on the filter residue obtained in the step (2), adding 4-8 times of 40% -80% ethanol water solution, and carrying out ultrasonic treatment at 50-70 ℃ for 30-70 min and 50-60 kHz ultrasonic frequency; centrifuging to obtain filtrate B, and mixing the filtrate A and the filtrate B to obtain Lycium ruthenicum Murr extract;
(4) alcohol collection and concentration: carrying out reduced pressure distillation and concentration on the mixed extracting solution in the step (3) in a rotary evaporator to obtain an extractum, and obtaining a lycium ruthenicum extract;
(5) and (3) separating with a microfiltration membrane: accurately weighing Lycium ruthenicum Murr extract, adding 40-50 times of 20-50% ethanol, and dissolving to obtain H1 solution; after complete dissolution, filtering with 50-200nm ceramic microfiltration membrane, wherein the interception section is H2;
(6) and (3) ultrafiltration membrane separation: filtering the microfiltration membrane permeate by using an organic membrane with the concentration of 10-500kd, wherein the interception section is marked as H3, and the permeation section is marked as H4;
(7) and (3) reduced pressure distillation: distilling H3 part under reduced pressure to relative density of 1.05-1.15 to obtain Lycium ruthenicum Murr essence.
2. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein 5-8 times of 70-95% ethanol is added in the step (2), the heating temperature is 65-85 ℃, and the heating reflux is carried out for 1-3 hours; filtering to obtain filtrate A and filter residue.
3. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (2), the mass ratio of the added cane sugar is 3%; adding 85-90% ethanol in an amount which is 5-6 times that of the raw materials, heating to 75-80 ℃, and heating and refluxing for 1-3 h; filtering to obtain filtrate A and filter residue.
4. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (3), 50% -70% of ethanol aqueous solution which is 5-7 times of the amount of the lycium ruthenicum spice is added, the ultrasonic temperature is 60-70 ℃, the ultrasonic time is 40-60min, and the ultrasonic frequency is 50kHz-60 kHz.
5. The preparation method of the lycium ruthenicum spice for the cigarettes according to claim 1, wherein in the step (3), 55% -60% of ethanol aqueous solution which is 5-6 times of the amount of the lycium ruthenicum spice is added, the ultrasonic temperature is 60-65 ℃, the ultrasonic time is 45-50min, and the ultrasonic frequency is 50kHz-60 kHz.
6. The preparation method of lycium ruthenicum mill flavor for cigarettes according to claim 1, wherein in the step (5), the pore diameter of the microfiltration membrane is 50-100 nm.
7. The preparation method of lycium ruthenicum murr spice for cigarettes according to claim 1, wherein in the step (6), the pore size of the ultrafiltration membrane is 50-200 KD.
8. The preparation method of lycium ruthenicum murr spice for cigarettes according to claim 1, wherein in the step (6), the pore size of the ultrafiltration membrane is 50-100 KD.
9. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 10-100; before preparing cigarettes, the lycium ruthenicum spice for cigarettes is sprayed on tobacco shreds according to the mass ratio of 0.02-1%, and then the cigarettes are prepared.
10. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 20-70; before preparing cigarettes, spraying the lycium ruthenicum spice for cigarettes on tobacco shreds according to the mass ratio of 0.05-0.5%, and rolling into cigarettes.
11. The application of the lycium ruthenicum spice for the cigarettes prepared by the method according to one of claims 1 to 8, wherein the lycium ruthenicum spice for the cigarettes is diluted by an organic solvent by a dilution factor of 40-50; before preparing cigarettes, spraying the lycium ruthenicum spice for cigarettes on tobacco shreds according to the mass ratio of 0.1-0.3%, and rolling into cigarettes; the organic solvent is ethanol, propylene glycol, sorbitol, xylitol or glycerol, or a mixed solution of more than 2 of the above.
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| CN112521524A (en) * | 2020-12-24 | 2021-03-19 | 中国科学院兰州化学物理研究所 | Composition for synergistically reducing blood sugar by using lycium barbarum polysaccharide and acaudina molpadioides functional peptide |
| CN112716028A (en) * | 2020-12-18 | 2021-04-30 | 云南天宏香精有限公司 | Additive for composite cigarette, preparation method and application |
| CN114082217A (en) * | 2021-11-12 | 2022-02-25 | 云南中烟新材料科技有限公司 | Preparation method and application of abelmoschus manihot flower extract |
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
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| CN112521524B (en) * | 2020-12-24 | 2022-05-24 | 中国科学院兰州化学物理研究所 | Composition for synergistically reducing blood sugar by using lycium barbarum polysaccharide and acaudina molpadioides functional peptide |
| CN114082217A (en) * | 2021-11-12 | 2022-02-25 | 云南中烟新材料科技有限公司 | Preparation method and application of abelmoschus manihot flower extract |
| CN115462552A (en) * | 2022-09-16 | 2022-12-13 | 湖南中烟工业有限责任公司 | Spice with fruit sweet fragrance, preparation method thereof and application thereof in cigarettes |
| CN115462552B (en) * | 2022-09-16 | 2023-09-05 | 湖南中烟工业有限责任公司 | Spice with fruit fragrance, preparation method thereof and application thereof in cigarettes |
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