CN114983003A - Preparation method and application of tobacco extract - Google Patents
Preparation method and application of tobacco extract Download PDFInfo
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- CN114983003A CN114983003A CN202210662106.2A CN202210662106A CN114983003A CN 114983003 A CN114983003 A CN 114983003A CN 202210662106 A CN202210662106 A CN 202210662106A CN 114983003 A CN114983003 A CN 114983003A
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- 241000208125 Nicotiana Species 0.000 title claims abstract description 138
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 138
- 239000000284 extract Substances 0.000 title claims abstract description 110
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 238000000605 extraction Methods 0.000 claims abstract description 69
- 238000000034 method Methods 0.000 claims abstract description 44
- 239000012043 crude product Substances 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 239000000047 product Substances 0.000 claims description 11
- 239000002245 particle Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 abstract description 33
- 239000000796 flavoring agent Substances 0.000 abstract description 27
- 235000019634 flavors Nutrition 0.000 abstract description 27
- 239000012530 fluid Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 description 30
- 230000009286 beneficial effect Effects 0.000 description 9
- 235000019504 cigarettes Nutrition 0.000 description 8
- 239000007788 liquid Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- SNICXCGAKADSCV-JTQLQIEISA-N (-)-Nicotine Chemical compound CN1CCC[C@H]1C1=CC=CN=C1 SNICXCGAKADSCV-JTQLQIEISA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229960002715 nicotine Drugs 0.000 description 5
- SNICXCGAKADSCV-UHFFFAOYSA-N nicotine Natural products CN1CCCC1C1=CC=CN=C1 SNICXCGAKADSCV-UHFFFAOYSA-N 0.000 description 5
- 230000000391 smoking effect Effects 0.000 description 5
- NIDGCIPAMWNKOA-WOJBJXKFSA-N Neophytadiene Natural products [C@H](CCC[C@@H](CCCC(C)C)C)(CCCC(C=C)=C)C NIDGCIPAMWNKOA-WOJBJXKFSA-N 0.000 description 4
- 238000007599 discharging Methods 0.000 description 4
- 239000003205 fragrance Substances 0.000 description 4
- 238000001819 mass spectrum Methods 0.000 description 4
- NIDGCIPAMWNKOA-UHFFFAOYSA-N neophytadiene Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(=C)C=C NIDGCIPAMWNKOA-UHFFFAOYSA-N 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- PQDRXUSSKFWCFA-CFNZNRNTSA-N solanone Chemical compound CC(=O)CC[C@@H](C(C)C)\C=C\C(C)=C PQDRXUSSKFWCFA-CFNZNRNTSA-N 0.000 description 4
- PQDRXUSSKFWCFA-UHFFFAOYSA-N solanone Natural products CC(=O)CCC(C(C)C)C=CC(C)=C PQDRXUSSKFWCFA-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 239000011344 liquid material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000001707 (E,7R,11R)-3,7,11,15-tetramethylhexadec-2-en-1-ol Substances 0.000 description 2
- YKVWPZJHENXDAJ-VOTSOKGWSA-N Megastigmatrienone Chemical compound CC1=CC(=O)CC(C)(C)C1\C=C\C=C YKVWPZJHENXDAJ-VOTSOKGWSA-N 0.000 description 2
- BLUHKGOSFDHHGX-UHFFFAOYSA-N Phytol Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C=CO BLUHKGOSFDHHGX-UHFFFAOYSA-N 0.000 description 2
- HNZBNQYXWOLKBA-UHFFFAOYSA-N Tetrahydrofarnesol Natural products CC(C)CCCC(C)CCCC(C)=CCO HNZBNQYXWOLKBA-UHFFFAOYSA-N 0.000 description 2
- BOTWFXYSPFMFNR-OALUTQOASA-N all-rac-phytol Natural products CC(C)CCC[C@H](C)CCC[C@H](C)CCCC(C)=CCO BOTWFXYSPFMFNR-OALUTQOASA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- BOTWFXYSPFMFNR-PYDDKJGSSA-N phytol Chemical compound CC(C)CCC[C@@H](C)CCC[C@@H](C)CCC\C(C)=C\CO BOTWFXYSPFMFNR-PYDDKJGSSA-N 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000003039 volatile agent Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000010812 external standard method Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
Images
Classifications
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a preparation method of a tobacco extract, which comprises the following steps: subjecting the tobacco extract crude product to supercritical CO 2 Extracting to obtain tobacco extract. The invention passes supercritical CO 2 The fluid extraction technology (SFE) modifies and improves the quality of the tobacco extract obtained by the thermochemical method, removes the foreign flavor substance components in the extract, avoids reducing the taste of the tobacco extract, and prepares the high-quality tobacco flavor extract. The invention also provides tobacco leaves.
Description
Technical Field
The invention belongs to the technical field of tobacco aroma extracts, and particularly relates to a preparation method and application of a tobacco extract.
Background
In the existing production technology of heating cigarettes, in order to improve the taste of cigarette cartridges, the content of aroma substances in reconstituted tobacco is increased by using tobacco taste compensation technologies such as natural spices, artificial spices or biotechnology spices, but the taste of the produced reconstituted tobacco still has the problem of insufficient taste, especially the original fragrance of tobacco is insufficient, so that the taste improvement is limited, and the development of the tobacco taste compensation technology with the original fragrance of tobacco is urgently needed.
During smoking of a cigarette, tobacco undergoes a devolatilization process to produce char and volatiles, and the volatiles and char subsequently combust to produce smoke. Most of the aroma components in the tobacco are released into the volatile matters, so the aroma components in the volatile matters obviously influence the smoking feeling.
The method is an effective way for making up the original fragrance of tobacco, but the conventional separation and purification method has the problems of low retention rate of effective fragrant components, more foreign flavor substances and non-uniform quality. Therefore, a separation and purification method capable of highly enriching the aroma components and removing the foreign flavor substances in the extract is urgently needed.
Disclosure of Invention
In view of this, the present invention aims to provide a preparation method of a tobacco extract and an application thereof, and the tobacco extract prepared by the method provided by the present invention has a good aroma effect.
The invention provides a preparation method of a tobacco extract, which comprises the following steps:
subjecting the tobacco extract crude product to supercritical CO 2 Extracting to obtain tobacco extract.
Preferably, the preparation method of the crude tobacco extract comprises the following steps:
extracting natural tobacco to obtain crude tobacco extract.
Preferably, the extraction method comprises:
the natural tobacco is sequentially crushed, heat treated, condensed and collected to obtain a crude tobacco extract product.
Preferably, the crushed particle size is 0.1-0.25 mm.
Preferably, the temperature of the heat treatment is 300-700 ℃.
Preferably, the supercritical CO 2 Compressing CO in an extraction process 2 The flow rate of the tobacco extract is nL/h which is 3-8 times of the mass of the crude tobacco extract;
the unit of the mass of the crude tobacco extract is g.
Preferably, the supercritical CO 2 Adding an entrainer in the extraction process;
the entrainer is selected from one or more of methanol, ethanol and acetic acid.
Preferably, the mass of the entrainer is 0.2-0.6 times of the mass of the crude tobacco extract product.
Preferably, the supercritical CO 2 The extraction time is 0.5-4 hours; the pressure is 23-26 MPa; the temperature is 40-55 ℃.
The invention provides a tobacco leaf, comprising: the tobacco extract is prepared by the method in the technical scheme.
The invention passes supercritical CO 2 The fluid extraction technology (SFE) modifies and improves the quality of the tobacco extract obtained by the thermochemical method, removes the foreign flavor substance components in the extract, avoids reducing the taste of the tobacco extract, and prepares the high-quality tobacco flavor extract.
The invention enriches the beneficial aroma components in the tobacco extract by using the supercritical extraction technology, ensures high yield and removes harmful foreign flavor substances influencing the smoking taste of the cigarette product. In the prior art, the tobacco extract obtained by the conventional thermochemical method such as the conventional separation means such as distillation has poor effect, and only crude extract with disordered components can be obtained. The invention further removes harmful foreign flavor substances from the tobacco extract by using a supercritical extraction technology, and re-enriches the aroma components in the tobacco extract, thereby being a high-efficiency separation method. The tobacco natural aroma component in the extracted enriched aroma component extract has high concentration, does not contain substances which can cause foreign flavor to influence the taste, can be used as a natural aroma component additive to be added into natural tobacco to prepare reconstituted tobacco, and is further processed into cigarette products. The method provided by the invention has high yield of aroma components, can obviously improve the smoke concentration of cigarettes, effectively increases the herbal aroma of the cigarettes, ensures the taste to be consistent with that of natural tobacco, greatly improves the taste of smoking, and is a method which has great development potential and can be applied to reconstituted tobacco.
Drawings
FIG. 1 is a flow chart of a process for preparing a tobacco extract according to an embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a preparation method of a tobacco extract, which comprises the following steps:
subjecting the tobacco extract crude product to supercritical CO 2 Extracting to obtain tobacco extract.
In the present invention, the preparation method of the crude tobacco extract preferably comprises:
extracting natural tobacco to obtain crude tobacco extract.
In the present invention, the method of extraction preferably comprises:
the natural tobacco is sequentially crushed, heat treated, condensed and collected to obtain a crude tobacco extract product.
In the present invention, the crushed particle size is preferably 0.1 to 0.25mm, and more preferably 0.15 to 0.2 mm.
In the invention, the crushing function is to increase the heating area of the natural tobacco, so that the natural tobacco is uniformly heated and the temperature is controllable in the heat treatment process, and more beneficial flavor substances can be released.
In the invention, the temperature of the heat treatment is preferably 300-700 ℃, more preferably 400-600 ℃, and most preferably 500 ℃. The heat treatment is preferably carried out at the heat treatment temperature, so that the tobacco can be fully cracked, the yield of beneficial flavor substances is improved, and the release of tar is obviously increased after the temperature is higher than 700 ℃.
According to the invention, the volatile components of the aroma substances after heat treatment are preferably fully condensed and collected to obtain the crude tobacco extract product, and the crude tobacco extract product contains a large amount of aroma substances and partial foreign flavor substances which can obviously influence the taste of the cigarette.
The invention utilizes supercritical CO 2 The extraction technology further separates and purifies the crude tobacco extract product to extract and separate out the tobacco aroma components. In order to realize the best separation and purification effect, improve the extraction rate of aroma components and reduce the water and foreign flavor substances in the extraction liquid, the invention preferably selects the extraction temperature and pressure, the separation pressure and the compressed CO 2 The flow rate and the amount of entrainer are controlled.
In the present invention, the supercritical CO 2 Compressing CO in an extraction process 2 The flow rate of the method is preferably nL/h which is 3-8 times of the mass of the crude tobacco extract, more preferably 4-7 times, and most preferably 5-6 times; the unit of the mass of the crude tobacco extract is g; if the mass of the crude tobacco extract is 1g, the CO is compressed within 1h of extraction time 2 The flow rate of (a) is 3-8 nL/h.
In the present invention, in order to enhance the effect of extracting the aroma component, supercritical CO is preferred 2 Adding entrainer in the extraction process; the entrainer is preferably one or more selected from methanol, ethanol and acetic acid, and is capable of improving aromaA solvent of different solubility. In the invention, the mass of the entrainer is preferably 0.2-0.6 times, more preferably 0.3-0.5 times and most preferably 0.4 times of the mass of the crude tobacco extract, and the entrainer is preferably used, so that the extraction rate of the aroma components can be effectively improved, and the increase range of the water content in the extraction liquid can be inhibited. In the invention, the entrainer is preferably added uniformly within 0.5-4 hours of extraction time.
In the present invention, the supercritical CO 2 The extraction time is preferably 0.5 to 4 hours, more preferably 1 to 3 hours, and most preferably 2 hours. In the present invention, the supercritical CO 2 The extraction pressure is preferably 23-26 MPa, and more preferably 24-25 MPa. In the present invention, the supercritical CO 2 The extraction temperature is preferably 40-55 ℃, and more preferably 45-50 ℃.
In the present invention, the above supercritical CO is preferably used 2 The pressure and temperature of the extraction can moderately increase CO 2 Increasing the selectivity towards the perfuming ingredients, decreasing the saturated vapour pressure of the compound so that the perfuming ingredients enter the gas phase.
In the present invention, the supercritical CO 2 The extraction process preferably further comprises the following steps:
and (4) reducing the pressure of the extracted product and separating.
In the invention, the pressure for reducing the pressure is preferably 6-10 MPa, more preferably 7-9 MPa, and most preferably 8 MPa; the time for the depressurization and separation is preferably 10-30 min, more preferably 15-25 min, and most preferably 20 min.
In the present invention, it is preferred that the addition of CO is stopped after the separation under reduced pressure is completed 2 Discharge of CO 2 Obtaining raffinate and extract liquor; the raffinate is mainly odorous substances and heavy oligomers, and the smell is more pungent; the extractive solution mainly contains aroma components, such as nicotine, solanone, phytol, neophytadiene, etc.
The method provided by the invention removes harmful components in the tobacco extract, and realizes the enrichment of beneficial flavor substances.
FIG. 1 is a flow chart of a process for preparing a tobacco extract according to an embodiment of the present invention. In the present invention, the preparation method of the tobacco extract preferably comprises:
obtaining a tobacco extract from natural tobacco:
firstly, natural tobacco is crushed, the particle size of the natural tobacco is controlled within the range of 0.1 mm-0.25 mm, the heating area is mainly increased, the natural tobacco is heated uniformly and the temperature of the natural tobacco is controllable in the heat treatment process, and further more beneficial flavor substances can be released.
Then, carrying out heat treatment, wherein the temperature of the heat treatment is 300-700 ℃, the tobacco can be fully cracked under the condition, the yield of beneficial flavor substances is improved, and the tar release can be obviously increased after the temperature exceeds 700 ℃; fully condensing and collecting the generated volatile matters of the flavor substances to obtain a tobacco extract; the tobacco extract contains a large amount of flavor substances which can obviously affect the mouthfeel and part of miscellaneous flavor substances.
Separating and purifying the tobacco extract:
by using supercritical CO 2 The extraction technology extracts and separates tobacco aroma components from tobacco extracts, and in order to realize the best separation and purification effect, improve the extraction rate of the aroma components and reduce the water content and other foreign flavor substances in the extraction liquid, the temperature and the pressure of an extraction kettle, the pressure of a separation kettle and compressed CO need to be strictly controlled 2 Flow rate, entrainer dosage and the like.
The specific extraction method comprises the following steps:
feeding the condensed extract into an extraction kettle via a liquid pump, and feeding compressed CO into the extraction kettle 2 The flow rate (nL/h, standard liter per hour) should be controlled to be 3-8 times of the mass (g, g) of the tobacco extract divided by the extraction time (h, h) (if the mass of the tobacco extract is 1g, in the extraction time of 1h, the CO is compressed 2 The flow rate of (a) should be 3-8 nL/h).
In order to enhance the extraction effect of the aroma components, an entrainer (such as methanol, ethanol, acetic acid, and other solvents capable of improving the solubility of the aroma components), an entrainer and compressed CO are added into the extraction kettle 2 Respectively fed by two pumps, fully mixed by a premixer and then delivered into an extraction kettleThe amount of the entrainer is 0.2-0.6 times of the amount of the tobacco extract (the increase of the moisture content in the extraction liquid is inhibited while the extraction rate of the aroma components is effectively improved), and the entrainer is injected at a constant speed within 0.5-4 h of extraction time.
The pressure of the extraction kettle is set to 23-26 MPa, and the temperature is set to 40-55 ℃ (moderately promoting CO) 2 Increasing selectivity towards the aroma component, decreasing the saturated vapour pressure of the compound so that the aroma component enters the vapour phase).
After the extraction time is reached, a valve from the extraction kettle to the separation kettle is opened to allow CO passing through the tobacco extract 2 Leaving the extraction kettle to reach a separation kettle, and reducing the pressure; setting the pressure of the separation kettle to be 8MPa, and stopping adding CO after 10-30 min 2 Then discharging CO in the extraction kettle and the separation kettle 2 Taking out raffinate (mainly foreign flavor substances) in the extractor and extract (aroma components) in the separation kettle; the treated extract mainly contains nicotine, solanone, phytol, neophytadiene and other beneficial fragrant substances, while the raffinate mainly contains heavy oligomers and has more pungent smell. The method provided by the invention removes harmful components in the tobacco extract, and realizes the enrichment of beneficial flavor substances.
The invention provides a tobacco leaf, comprising: the tobacco extract is prepared by the method of the technical method.
In the present invention, the preparation method of the tobacco leaf preferably comprises:
the tobacco extract prepared by the method in the technical scheme is added into tobacco to obtain the reconstituted tobacco with abundant tobacco fragrance.
The method provided by the invention can realize the collection of high-content tobacco aroma components and the removal of foreign flavor substances in the tobacco extract at the same time, and the reconstituted tobacco produced by utilizing the tobacco aroma components prepared by the method has enough herbal aroma and good smoking mouthfeel.
The natural tobacco used in the following examples of the present invention is commercially available.
Example 1
The preparation of tobacco extract was carried out according to the process flow diagram shown in fig. 1:
crushing 10kg of natural tobacco, and controlling the particle size of the natural tobacco within the range of 0.15 mm-0.2 mm.
And (3) carrying out heat treatment on the tobacco powder obtained after crushing, wherein the heat treatment temperature is 500 ℃, and fully condensing and collecting volatile components of the generated flavor substances to obtain the tobacco extract.
Inputting the condensed and collected extract into an extraction kettle by a liquid material pump, wherein the pressure of the extraction kettle is 24MPa, and the temperature is 45 ℃; using two pumps to input compressed CO into the extraction kettle through a premixer respectively 2 The flow rate is 25nL/h, the flow rate is 2kg/h, and the extraction time is 2 h.
After the extraction time is reached, the valve is opened to allow CO to pass through the tobacco extract 2 Leaving the extraction kettle to reach a separation kettle, and controlling the pressure of the separation kettle to be 8 MPa; stopping adding CO after 20min 2 And discharging CO in the extraction kettle and the separation kettle 2 (ii) a 1850g of the extract rich in aroma components was collected in the separation vessel, and the yield thereof was 18.50%.
Example 2
The preparation of tobacco extract was carried out according to the process flow shown in figure 1:
crushing 5kg of natural tobacco, and controlling the particle size of the natural tobacco within the range of 0.1 mm-0.15 mm.
And (3) carrying out heat treatment on the tobacco powder obtained after crushing, wherein the temperature of the heat treatment is 450 ℃, and fully condensing and collecting volatile components of the generated flavor substances to obtain the tobacco extract.
Inputting the condensed and collected extract into an extraction kettle by a liquid material pump, wherein the pressure of the extraction kettle is 24MPa, and the temperature is 45 ℃; using two pumps to input compressed CO into the extraction kettle through the premixer respectively 2 The flow rate is 20nL/h, the entrainer ethanol (the flow rate is 2.5kg/h) and the extraction time is 1 h.
After the extraction time is reached, the valve is opened to allow the CO to pass through the tobacco extract 2 Leaving the extraction kettle and reaching a separation kettle, wherein the pressure of the separation kettle is controlled to be 8 MPa; stopping adding CO after 15min 2 And discharging CO in the extraction kettle and the separation kettle 2 (ii) a Collecting the extract rich in aroma components in a separation kettle806g of liquid is taken, and the yield reaches 16.12%.
Example 3
The preparation of tobacco extract was carried out according to the process flow diagram shown in fig. 1:
crushing 12kg of natural tobacco, and controlling the particle size of the natural tobacco within the range of 0.1-0.2 mm.
And (3) carrying out heat treatment on the tobacco powder obtained after crushing, wherein the heat treatment temperature is 400 ℃, and fully condensing and collecting volatile components of the generated flavor substances to obtain the tobacco extract.
Inputting the condensed and collected extract into an extraction kettle by a liquid material pump, wherein the pressure of the extraction kettle is 25MPa, and the temperature is 40 ℃; using two pumps to input compressed CO into the extraction kettle through the premixer respectively 2 The flow rate is 16nL/h, the flow rate is 2kg/h, and the extraction time is 3 h.
After the extraction time is reached, the valve is opened to allow the CO to pass through the tobacco extract 2 Leaving the extraction kettle to reach a separation kettle, and controlling the pressure of the separation kettle to be 8 MPa; stopping adding CO after 25min 2 And discharging CO in the extraction kettle and the separation kettle 2 (ii) a 2150g of the extract enriched in the aroma components was collected in the separation vessel, and the yield thereof was 17.92%.
Comparative example 1
Tobacco extract preparation was carried out according to the method of example 1, except that the heat treatment temperature was increased to 650 ℃.
1526g of the extraction liquid enriched in the aroma components is collected in the separation kettle in the comparison document 1, and the yield reaches 15.26%.
Comparative example 2
The preparation of tobacco extract was carried out in the same manner as in example 1 except that the pressure in the extraction vessel was controlled to 26MPa and the temperature was controlled to 55 ℃ in the same manner as in example 1.
In comparative example 2, 1774g of the extract rich in aroma components was collected in the separation vessel, and the yield reached 17.74%.
Comparative example 3
Preparation of tobacco extract according to the method of example 1, in contrast to example 1, compressed CO 2 The flow rate of (b) is controlled to be 35nL/h,The flow rate of the entrainer ethanol was controlled at 2.5 kg/h.
In comparative example 3, 1796g of the extract rich in aroma components was collected in the separation vessel, and the yield reached 17.96%.
Product testing
The determination of nicotine is according to the method in GB/T23355-2009; and the other substances are measured by using a GC-MS external standard method, which specifically comprises the following steps: the capillary chromatographic column adopts HP-INNOWAx (length of 30m, inner diameter of 0.25mm, thickness of 0.25 mm); before testing, the sample solution was filtered through a 0.45 μm oily filter; the sample injection amount of the GC-MS is set to be 1 mu L/time, carrier gas is high-purity helium (the purity is more than 99.99 percent), the flow is 1.0ml/min, and the sample injection is carried out in a non-shunting mode; the source temperature of the mass spectrum is 230 ℃, and the quadrupole temperature of the mass spectrum is 150 ℃; the mass spectrum scanning range is 15-500 m/z; the mass spectrum delay time is set to 4.7 min; the injection port temperature was set to 250 ℃ and the column temperature program was: standing at 40 deg.C for 3min, heating to 250 deg.C at a heating rate of 5 deg.C/min, and standing for 10 min. The detection results are as follows:
note: in table 1, the extract yield refers to the mass/tobacco mass ratio of the extract collected during the extraction process, the extract nicotine concentration refers to the mass concentration of nicotine contained in the collected extract, the extract megastigmatrienone concentration refers to the mass concentration of megastigmatrienone contained in the collected extract, the extract solanone concentration refers to the mass concentration of solanone contained in the collected extract, and the extract neophytadiene concentration refers to the mass concentration of neophytadiene contained in the collected extract.
The method provided by the invention can effectively enrich beneficial fragrant substances in the tobacco extracting solution, and effectively remove foreign flavor substances which are unfavorable to the taste of the tobacco extract, and the extracting solution prepared by the invention can effectively realize the aroma enhancement of the reconstituted tobacco.
While the invention has been described and illustrated with reference to specific embodiments thereof, such description and illustration are not intended to limit the invention. It will be clearly understood by those skilled in the art that various changes may be made to adapt a particular situation, material, composition of matter, substance, method or process to the objective, spirit and scope of this application without departing from the true spirit and scope of the invention as defined by the appended claims. All such modifications are intended to be within the scope of the claims appended hereto. Although the methods disclosed herein have been described with reference to particular operations being performed in a particular order, it should be understood that these operations may be combined, sub-divided, or reordered to form equivalent methods without departing from the teachings of the present disclosure. Accordingly, unless specifically indicated herein, the order and grouping of the operations is not a limitation of the present application.
Claims (10)
1. A method for preparing a tobacco extract, comprising:
subjecting the tobacco extract crude product to supercritical CO 2 Extracting to obtain tobacco extract.
2. The method of claim 1, wherein the method of preparing the crude tobacco extract comprises:
extracting natural tobacco to obtain crude tobacco extract.
3. The method of claim 2, wherein the method of extracting comprises:
the natural tobacco is sequentially crushed, heat treated, condensed and collected to obtain a crude tobacco extract product.
4. The method according to claim 3, wherein the crushed particles have a size of 0.1 to 0.25 mm.
5. The method according to claim 3, wherein the temperature of the heat treatment is 300 to 700 ℃.
6. The method of claim 1, wherein the supercritical CO is 2 Compressing CO in an extraction process 2 The flow rate of the tobacco extract is 3 to cnL/h which is 8 times that of nL/h;
the unit of the mass of the crude tobacco extract is g.
7. The method of claim 1, wherein the supercritical CO is 2 Adding entrainer in the extraction process;
the entrainer is selected from one or more of methanol, ethanol and acetic acid.
8. The method of claim 7, wherein the entrainer has a mass of 0.2 to 0.6 times the mass of the crude tobacco extract.
9. The method of claim 1, wherein the supercritical CO is 2 The extraction time is 0.5-4 hours; the pressure is 23-26 MPa; the temperature is 40-55 ℃.
10. A tobacco leaf, comprising: a tobacco extract prepared by the method of claim 1.
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| CN1401751A (en) * | 2002-09-13 | 2003-03-12 | 云南瑞升科技有限公司 | Method for preparing pure tobacco oil |
| CN105199850A (en) * | 2015-10-16 | 2015-12-30 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of tobacco flavor |
| CN105852200A (en) * | 2016-04-28 | 2016-08-17 | 湖南中烟工业有限责任公司 | Preparation method of tobacco-sourced basic cigarette-smell raw material |
| CN114504119A (en) * | 2022-03-29 | 2022-05-17 | 南京林业大学 | Tobacco flavor extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1401751A (en) * | 2002-09-13 | 2003-03-12 | 云南瑞升科技有限公司 | Method for preparing pure tobacco oil |
| CN105199850A (en) * | 2015-10-16 | 2015-12-30 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of tobacco flavor |
| CN105852200A (en) * | 2016-04-28 | 2016-08-17 | 湖南中烟工业有限责任公司 | Preparation method of tobacco-sourced basic cigarette-smell raw material |
| CN114504119A (en) * | 2022-03-29 | 2022-05-17 | 南京林业大学 | Tobacco flavor extraction method |
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