CN111254013B - Perfume composition containing extract of lysimachia capillipes - Google Patents
Perfume composition containing extract of lysimachia capillipes Download PDFInfo
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- CN111254013B CN111254013B CN202010108129.XA CN202010108129A CN111254013B CN 111254013 B CN111254013 B CN 111254013B CN 202010108129 A CN202010108129 A CN 202010108129A CN 111254013 B CN111254013 B CN 111254013B
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- 239000000284 extract Substances 0.000 title claims abstract description 107
- 241000941637 Lysimachia capillipes Species 0.000 title claims abstract description 87
- 239000000203 mixture Substances 0.000 title claims abstract description 26
- 239000002304 perfume Substances 0.000 title claims description 9
- 239000002994 raw material Substances 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 23
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 239000003205 fragrance Substances 0.000 claims abstract description 14
- 239000007787 solid Substances 0.000 claims abstract description 14
- 150000001875 compounds Chemical class 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 238000001256 steam distillation Methods 0.000 claims abstract description 9
- 238000004821 distillation Methods 0.000 claims abstract description 6
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 235000020765 fenugreek extract Nutrition 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 235000019505 tobacco product Nutrition 0.000 claims description 28
- 239000000796 flavoring agent Substances 0.000 claims description 20
- 235000019634 flavors Nutrition 0.000 claims description 20
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 12
- 235000009499 Vanilla fragrans Nutrition 0.000 claims description 11
- 235000012036 Vanilla tahitensis Nutrition 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 10
- 238000002485 combustion reaction Methods 0.000 claims description 8
- 239000002798 polar solvent Substances 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 238000000638 solvent extraction Methods 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 229940098465 tincture Drugs 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000005057 refrigeration Methods 0.000 claims description 2
- 244000263375 Vanilla tahitensis Species 0.000 claims 5
- 241000220289 Pedunculata Species 0.000 claims 1
- 210000000582 semen Anatomy 0.000 abstract description 4
- 235000013599 spices Nutrition 0.000 abstract description 3
- 235000019504 cigarettes Nutrition 0.000 description 30
- 241000208125 Nicotiana Species 0.000 description 27
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 27
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 24
- 230000001953 sensory effect Effects 0.000 description 14
- 239000011259 mixed solution Substances 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 11
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 9
- 238000005507 spraying Methods 0.000 description 8
- 244000250129 Trigonella foenum graecum Species 0.000 description 7
- 235000001484 Trigonella foenum graecum Nutrition 0.000 description 7
- 238000007865 diluting Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 244000290333 Vanilla fragrans Species 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 235000001019 trigonella foenum-graecum Nutrition 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000002470 solid-phase micro-extraction Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OIPPWFOQEKKFEE-UHFFFAOYSA-N orcinol Chemical compound CC1=CC(O)=CC(O)=C1 OIPPWFOQEKKFEE-UHFFFAOYSA-N 0.000 description 4
- 238000011158 quantitative evaluation Methods 0.000 description 4
- 239000006228 supernatant Substances 0.000 description 4
- 235000019640 taste Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- 240000000377 Tussilago farfara Species 0.000 description 3
- 235000004869 Tussilago farfara Nutrition 0.000 description 3
- 230000000295 complement effect Effects 0.000 description 3
- 125000004494 ethyl ester group Chemical group 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- NOTCZLKDULMKBR-UHFFFAOYSA-N 3-Methoxy-5-methylphenol Chemical compound COC1=CC(C)=CC(O)=C1 NOTCZLKDULMKBR-UHFFFAOYSA-N 0.000 description 2
- GHVHDYYKJYXFGU-UHFFFAOYSA-N Beta-Orcinol Chemical compound CC1=CC(O)=C(C)C(O)=C1 GHVHDYYKJYXFGU-UHFFFAOYSA-N 0.000 description 2
- 206010013911 Dysgeusia Diseases 0.000 description 2
- 241000825107 Hierochloe Species 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- XIRNKXNNONJFQO-UHFFFAOYSA-N ethyl hexadecanoate Chemical compound CCCCCCCCCCCCCCCC(=O)OCC XIRNKXNNONJFQO-UHFFFAOYSA-N 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000007794 irritation Effects 0.000 description 2
- 230000008520 organization Effects 0.000 description 2
- MDHYEMXUFSJLGV-UHFFFAOYSA-N phenethyl acetate Chemical compound CC(=O)OCCC1=CC=CC=C1 MDHYEMXUFSJLGV-UHFFFAOYSA-N 0.000 description 2
- 239000008213 purified water Substances 0.000 description 2
- 238000013441 quality evaluation Methods 0.000 description 2
- 238000012764 semi-quantitative analysis Methods 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 244000061182 Coleus blumei Species 0.000 description 1
- 235000002659 Coleus scutellarioides Nutrition 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 description 1
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 description 1
- 241000220485 Fabaceae Species 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 229930191978 Gibberellin Natural products 0.000 description 1
- 241001430197 Mollicutes Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 241000208476 Primulaceae Species 0.000 description 1
- TVXBFESIOXBWNM-UHFFFAOYSA-N Xylitol Natural products OCCC(O)C(O)C(O)CCO TVXBFESIOXBWNM-UHFFFAOYSA-N 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- RDOXTESZEPMUJZ-UHFFFAOYSA-N anisole Chemical compound COC1=CC=CC=C1 RDOXTESZEPMUJZ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 239000002027 dichloromethane extract Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229940067592 ethyl palmitate Drugs 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 238000002546 full scan Methods 0.000 description 1
- IXORZMNAPKEEDV-UHFFFAOYSA-N gibberellic acid GA3 Natural products OC(=O)C1C2(C3)CC(=C)C3(O)CCC2C2(C=CC3O)C1C3(C)C(=O)O2 IXORZMNAPKEEDV-UHFFFAOYSA-N 0.000 description 1
- 239000003448 gibberellin Substances 0.000 description 1
- 150000004676 glycans Chemical class 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
- 230000006872 improvement Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- HEBKCHPVOIAQTA-UHFFFAOYSA-N meso ribitol Natural products OCC(O)C(O)C(O)CO HEBKCHPVOIAQTA-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- AMKYESDOVDKZKV-UHFFFAOYSA-N o-orsellinic acid Chemical compound CC1=CC(O)=CC(O)=C1C(O)=O AMKYESDOVDKZKV-UHFFFAOYSA-N 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 150000005856 steroid saponins Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000001917 trigonella foenum graecum l. absolute Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
- 239000000811 xylitol Substances 0.000 description 1
- HEBKCHPVOIAQTA-SCDXWVJYSA-N xylitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)CO HEBKCHPVOIAQTA-SCDXWVJYSA-N 0.000 description 1
- 229960002675 xylitol Drugs 0.000 description 1
- 235000010447 xylitol Nutrition 0.000 description 1
Classifications
-
- 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
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
- B01D11/0296—Condensation of solvent vapours
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
The present invention relates to a fragrance composition comprising an extract of lysimachia capillipes. The spice composition comprises a lysimachia capillipes extract and a compound extract; the preparation method of the lysimachia capillipes extract comprises the following steps: (1) Carrying out steam distillation on the lysimachia capillipes raw material to ensure that the flow rate of steam condensate is 3-10 times of the weight of the lysimachia capillipes raw material per hour, the distillation time is 3-6 hours, and collecting distilled lysimachia capillipes solid matters; (2) And (3) extracting the lysimachia capillipes solid obtained in the step (1) by using a solvent, performing solid-liquid separation after extraction, and collecting an extracting solution. The compound extract is semen Trigonellae extract and/or thallus Porphyrae extract.
Description
Technical Field
The invention belongs to the field of tobacco, and particularly relates to a spice composition containing a lysimachia capillipes extract.
Background
The herb of Hierochloes Adoratae (Lysimachia capillipes Hemsl.) is also called flos Rhododendri Dahurici, herba Phyllostachydis Henonis, herba Roxburghii, and Primuleach family (Primulaceae) genus plant, and is widely distributed in areas such as Guizhou, jiangxi, and Fujian in China, and the whole herb has strong fragrance after sun drying.
Fenugreek (Trigonella foenum-graecum L.) is also called herba Cymbopogonis, vanilla, herba Medicaginis, which is a plant of the subfamily Papilionaceae of Leguminosae, and has fragrance, and is distributed in the east-east, middle-east and Himalayan areas of Mediterranean, and mainly used for cultivation in China, such as Anhui, sichuan, henan, etc. The Chinese medicine has bitter taste and warm nature, has effects of warming kidney, dispelling cold, and relieving pain, and contains complex chemical components and wide pharmacological effects, and the main components are steroid saponin, flavonoid, alkaloids, polysaccharides, etc. The fenugreek extract extracted from fenugreek seeds is a tobacco flavor. It can inhibit pungency of tobacco leaf, cover miscellaneous gas, correct taste, and increase sweet and burnt flavor of tobacco.
The tree moss extract (Tree Moss Extract) is an extract of tree moss. The tree moss extract has clear fragrance and pine smell.
Disclosure of Invention
The present disclosure first provides a lysimachia capillipes extract. The lysimachia capillipes extract is prepared by a unique process, which weakens the strong style characteristics (herb taste) of the lysimachia capillipes in the lysimachia capillipes extract, but retains the functional components of the lysimachia capillipes. Further, the inventor finds that the lysimachia capillipes extract and the fenugreek extract (or the tree moss extract) are particularly coordinated through sensory analysis and component analysis, and are combined with each other to be used for tobacco products, and the lysimachia capillipes extract and the fenugreek extract complement each other and synergistically increase each other, so that the smoke is fine, soft and thoroughly emitted, and the aroma quality is obviously improved. Still further, the inventor also finds that the lysimachia capillipes extract, the fenugreek extract and the tree moss extract of the present disclosure can be combined for tobacco products, so as to further improve the fragrance quality.
In some aspects, a flavor composition is provided comprising a lysimachia capillipes extract and a compound extract;
wherein, the preparation method of the lysimachia capillipes extract comprises the following steps:
(1) Carrying out steam distillation on the lysimachia capillipes raw material, enabling the flow rate of steam condensate to be 3-10 times (for example, 4-5 times, 5-6 times, 6-7 times, 7-8 times or 8-9 times) of the weight of the lysimachia capillipes raw material per hour, enabling the distillation time to be 3-6 hours (for example, 3-4 hours, 4-5 hours or 5-6 hours), and collecting distilled lysimachia capillipes solid matters;
(2) Extracting the lysimachia capillipes solid obtained in the step 1 by a solvent, performing solid-liquid separation after extraction, and collecting an extracting solution;
the compound extract is a fenugreek extract and/or a tree moss extract.
In some embodiments, step 2 uses only the distilled vanilla solids obtained in step 1, and the water vapor condensate obtained in step 1 does not enter step 2. Thus, the characteristic components (herb flavor) of the lysimachia capillipes in the product of the step 2 are weakened, but the functional components of the lysimachia capillipes are reserved, and the obtained lysimachia capillipes extract is particularly suitable for being compounded with other spice components.
In some embodiments, in step 1, water is applied to the lysimachia capillipes raw material prior to steam distillation, the weight of water being 5-20% (e.g. 10-15%) of the weight of the lysimachia capillipes raw material.
In some embodiments, step 1 further comprises the operation of drying the distilled lysimachia capillipes solids.
In some embodiments, the solvent extraction is subcritical fluid solvent extraction.
In some embodiments, the solvent extraction is ultrasonic-assisted solvent extraction.
In some embodiments, the weight ratio of solvent to lysimachia capillipes raw material is 1-20:1-20, such as 1-20:1, such as 1-5:1, such as 6-10:1, such as 11-15:1, such as 16-20:1.
In some embodiments, the solvent comprises a polar solvent in a weight ratio of polar solvent to vanilla material of from 1 to 20:1 to 20, such as from 1 to 20:1, such as from 1 to 5:1, such as from 6 to 10:1, such as from 11 to 15:1, such as from 16 to 20:1, such as from 20:1 to 4.
In some embodiments, the solvent comprises a subcritical fluid and a polar solvent (e.g., ethanol). Optionally, the weight ratio of subcritical fluid to lysimachia capillipes raw material is 20-30:1. Optionally, the weight ratio of the polar solvent to the lysimachia capillipes raw material is 0.1-1:1.
In some embodiments, polar solvent refers to a solvent that is not less polar than ethanol.
In some embodiments, the polar solvent is selected from ethanol, water, or a combination thereof.
In some embodiments, the extraction temperature is 20-100 ℃ (e.g., 20-35 ℃, 40-55 ℃, 60-75 ℃, or 80-95 ℃).
In some embodiments, the time for each extraction is 20 to 200 minutes (e.g., 20 to 40 minutes, 50 to 70 minutes, 80 to 100 minutes, 110 to 130 minutes, 140 to 160 minutes, or 170 to 190 minutes).
In some embodiments, in step 2, the solvent comprises one or more of water and ethanol.
In some embodiments, in step 2, the solvent also contains a subcritical fluid, such as dimethyl ether.
In some embodiments, in step 2, the solvent comprises dimethyl ether and ethanol.
In some embodiments, the solvent is water, the extraction temperature is 80-100 ℃, and the single extraction time is 100-150 minutes. The weight ratio of the solvent to the lysimachia capillipes raw material is 10-30: 1. the extraction times can be selected to be 1-3 times.
In some embodiments, the solvent is an aqueous ethanol solution (ethanol concentration of 50-80 wt%), the extraction temperature is 80-100 ℃, and the single extraction time is 100-150 min. The weight ratio of the solvent to the lysimachia capillipes raw material is 15-25: 1. the extraction times can be selected to be 1-3 times.
In some embodiments, the solvent is a mixture of dimethyl ether and ethanol (the volume ratio of dimethyl ether to ethanol is 8-12:1), the extraction temperature is 20-35 ℃, and the single extraction time is 15-25 min. The weight ratio of the solvent to the lysimachia capillipes raw material is selected to be 20:1-4. The extraction times can be selected to be 1-3 times. After extraction, the extracts may be collected, combined and freeze dewaxed.
In some embodiments, wherein step 2 is repeated (e.g., 2, 3, 4, or 5 times), the extracts are combined. Repeating step (2) n times means that step (2) is performed n times altogether, n may be equal to 2, 3, 4, 5, or the like.
In some embodiments, the above preparation method further comprises the steps of:
(3) And (3) carrying out post-treatment on the extracting solution obtained in the step (2), wherein the post-treatment is one or more steps selected from refrigeration, freeze dewaxing, standing, centrifugation, concentration and dilution.
In some embodiments, the concentration is evaporative concentration.
In some embodiments, the evaporative concentration is single-effect evaporative concentration or multiple-effect evaporative concentration.
Preferably, the temperature of the evaporation concentration (temperature of the heating medium) is 40 to 70 ℃ (e.g., 45 to 65 ℃).
In some embodiments, the lysimachia capillipes extract has a relative density of 1.0 to 1.3 at 20 ℃.
In some embodiments, the lysimachia capillipes raw material is dried lysimachia capillipes whole herb, or a cut product of dried lysimachia capillipes whole herb, or a crushed product of dried lysimachia capillipes whole herb.
In some embodiments, the fenugreek extract is a powder, extract or tincture.
In some embodiments, the perfume composition further comprises a tree moss extract.
In some embodiments, the tree moss extract is a powder, extract or tincture.
In some embodiments, the weight ratio of the lysimachia capillipes extract to the fenugreek extract is 1-10 (e.g. 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10): 0.01 to 10 (e.g., 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10).
In some embodiments, the weight ratio of lysimachia capillipes extract to tree moss extract is 1-10 (e.g., 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10): 0.01 to 10 (e.g., 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10).
In some embodiments, the lysimachia capillipes extract: fenugreek extract: tree moss extract weight ratio = 1-10 (e.g. 1, 2, 3, 4, 5, 6, 7, 8, 9 or 10): 0.01 to 10 (e.g., 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10): 0.01 to 10 (e.g., 0.05, 0.1, 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10).
In some embodiments, the tree moss extract has one or more of the following characteristics:
-a relative density of 0.8 to 1, for example 0.8 to 0.9;
a refractive index of 1.3 to 1.5, for example 1.35 to 1.45;
-the content of the orcinol monomethyl ether is 0.0008-0.0012 mg/g;
the content of the beta-orcinol is 0.0104-0.0156 mg/g;
the content of the soft flat phenol monomethyl ether is 0.0952 to 0.1428mg/g;
the content of the orcinol is 0.0552 to 0.0828mg/g;
the content of the ethyl ester of the amygdalinate is 0.0064-0.0096 mg/g;
-methoxy olive alcohol content of 0.028-0.042 mg/g;
the content of the ethyl ester of the gibberellin is 0.128-0.192 mg/g;
the content of the beta-methyl ester of the orcinol is 1.26 to 1.89mg/g;
the content of the ethyl ester of the orcinol carboxylic acid is 1.9496 to 2.9244mg/g;
the content of the ethyl mollicutes is 0.2976 to 0.4464mg/g;
the content of the ethyl palmitate is 0.1088-0.1632 mg/g.
In some embodiments, the fenugreek extract is a fenugreek extract.
In some embodiments, the relative density of the fenugreek extract is 1.0 to 1.1, such as 1.0889.
In some embodiments, the fenugreek extract has a refractive index of 1.3 to 1.5, such as 1.4098.
In some aspects, there is provided the use of the above flavour composition for the preparation of a tobacco product.
In some embodiments, the tobacco product is a combustion tobacco product, a heated non-combustion tobacco product, or an atomized tobacco product.
In some aspects, there is provided a tobacco product comprising the above flavour composition;
in some embodiments, the tobacco product is a combustion tobacco product, a heated non-combustion tobacco product, or an atomized tobacco product.
In some embodiments, the common coleus extract, the fenugreek extract and the tree moss extract are compounded according to the weight ratio of 1-10:0.01-10, diluted by a polyhydroxy alcohol solvent with the volume of 1-200 times, and sprayed on tobacco shreds to be 0.01-2% of the mass of the tobacco shreds.
In some embodiments, the polyhydroxy alcohol solvent is a mixture of food grade alcohol, propylene glycol, sorbitol, and xylitol in any ratio.
Description of the terms
As used herein, the following terms may have the following meanings:
the term "steam distillation" may be direct steam distillation or water distillation, even if steam passes through the herb of Hierochloes Adoratae raw material, and then the steam is condensed, and the condensate is collected. During this time, the lysimachia capillipes raw material was not soaked in water.
The relative density refers to the density relative to water.
The semen Trigonellae extract refers to dried semen Trigonellae extract.
Advantageous effects
The extract preparation method/extract/composition/tobacco product of the present disclosure has one or more of the following beneficial effects:
(1) The lysimachia capillipes extract disclosed by the disclosure has weakened style characteristics (herb taste) of lysimachia capillipes, but retains functional components of lysimachia capillipes, is suitable for improving taste of tobacco products, and is particularly suitable for being compounded with other tobacco flavors;
(2) The common coltsfoot herb extract and the fenugreek extract are combined to be used for tobacco products, and the common coltsfoot herb extract and the fenugreek extract can be synergistic, so that the smoke is fine, soft and thoroughly emitted, and the fragrance quality is improved.
(3) The lysimachia capillipes extract, the fenugreek extract and the tree moss extract are combined to be used for tobacco products, and the three can be synergistic, so that the fragrance quality is further improved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. The following description of at least one exemplary embodiment is merely exemplary in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The raw materials used in the following examples are shown in the following table:
EXAMPLE 1.1-Lysimachia capillipes extract FC-1
Step (1) pretreatment of raw materials: cutting 10kg of dried herb of lysimachia capillipes into 10cm sections;
and (2) carrying out water dispersion treatment: spraying 1kg of pure water onto 10kg of cut lysimachia capillipes;
step (3) steam distillation: placing the product obtained in the step 2 on a porous plate, introducing water vapor from the lower part of the porous plate, controlling the opening of a water vapor valve to ensure that the flow rate of the water vapor condensate is 80kg/h and the time is 6h, and collecting the distilled lysimachia capillipes solid;
and (4) water extraction: adding purified water which is 10 times the mass of the raw materials in the step (1) into the lysimachia capillipes solid matters for soaking and extracting, wherein the extracting temperature is 100 ℃, the extracting time is 120min, filtering after extracting, the extracting times are 2 times, and combining the filtrates;
and (5) centrifuging: 9000rpm of the filtrate obtained in the step (4) at 20 ℃ for 30min to obtain a centrifugal clear liquid;
and (6) concentrating: concentrating the supernatant in the step (5) by adopting a double-effect concentration unit. The opening of a first-effect steam valve is 80%, the steam pressure is-0.070 Mpa, the steam temperature is 65 ℃, the liquid level of the first-effect separator is 3.0cm, the temperature of the first-effect separator is 55 ℃, the liquid level of the second-effect separator is 5.6cm, and the temperature of the second-effect separator is 45 ℃. The feed flow rate was 1.5m 3 Per hour, the feeding temperature is 54 ℃, the circulation temperature is 48 ℃, the condenser pressure is-0.090 Mpa, the condenser temperature is 25 ℃, and the evaporation capacity is 2.8m 3 And/h. 10kg of a lysimachia capillipes extract (accession number FC-1) having a relative density of 1.0 at 20℃was obtained.
EXAMPLE 1.2-Lysimachia capillipes extract FC-2
Step (1) pretreatment of raw materials: cutting 20kg of dried herb of lysimachia capillipes into 15cm sections;
and (2) carrying out water dispersion treatment: carrying out water dispersion treatment on the pretreated lysimachia capillipes segments, wherein the weight of pure water is 2kg;
step (3) steam distillation: placing the product obtained in the step 2 on a porous plate, introducing water vapor from the lower part of the porous plate, controlling the opening of a water vapor valve to ensure that the flow rate of the water vapor condensate is 100kg/h of the weight of the lysimachia capillipes and the time is 5h, and collecting distilled lysimachia capillipes solid;
and (4) alcohol extraction: adding 70% edible alcohol which is 20 times of the mass of the raw material in the step (1) into the lysimachia capillipes solid matter of the lysimachia capillipes, wherein the extraction temperature is 80 ℃, the time is 180min, and the extraction times are 1 time;
and (5) refrigerating and standing: standing the filtrate obtained in the step (4) at the temperature of between 10 ℃ below zero and 4 ℃ for 24 hours, and filtering to obtain supernatant;
and (6) concentrating: concentrating the supernatant in the step (5) by adopting a single-effect concentration unit, wherein the opening of a steam valve is 85%, the steam pressure is-0.008 Mpa, the steam temperature is 76 ℃, and the feeding flow is 0.26m 3 And/h, the feeding temperature is 30 ℃, the circulating temperature is 50 ℃, the pressure of a condenser is-0.008 Mpa, the temperature of the condenser is 12 ℃, and the evaporation capacity is 0.22m 3 And/h. 20kg of perfume FC-2 was obtained, having a relative density of 1.1 at 20 ℃.
EXAMPLE 1.3-Lysimachia capillipes extract FC-3
Step (1) pretreatment of raw materials: crushing 1kg of sun-dried herb of lysimachia capillipes into powder by using a 10-mesh screen, and subpackaging into 200 g/bag by using cotton bags;
and (2) carrying out water dispersion treatment: carrying out water dispersion treatment on the pretreated lysimachia capillipes powder, wherein the weight of pure water is 1.1kg;
step (3) steam distillation: placing the product obtained in the step 2 on a porous plate, introducing water vapor from the lower part of the porous plate, controlling the opening of a water vapor valve to ensure that the flow rate of the water vapor condensate is 100kg/h of the weight of the lysimachia capillipes, and the time is 3h, and airing the residual lysimachia capillipes solids after distillation for later use;
subcritical extraction in step (4): adding solvent (dimethyl ether 4L, entrainer ethanol 400 ml) into the herba Lysimachiae Foenumgraeci solid, extracting at room temperature for three times and 20min each time, freeze dewaxing for 2 times (in subcritical extraction process, extracting wax (i.e. higher fatty acid) in plant together, freezing, solidifying to form wax layer, floating on the surface of extract, scraping treatment), diluting the frozen dewaxed product with anhydrous ethanol; 1kg of perfume FC-3 was obtained, having a relative density of 1.1 at 20 ℃.
Application example 1-extract of Lysimachia capillipes+extract of Trigonella Foenum-Graecum
The mixed solution prepared by mixing the fenugreek extract and the propylene glycol according to the mass ratio of 10:100 is diluted by 10 times, and then added to cut tobacco in a feeding procedure in a spraying manner according to the addition amount of 0.01% of the weight of the cut tobacco, so as to prepare the cigarette with the number of 1A.
Diluting the mixed solution of the lysimachia capillipes extract FC-1 and propylene glycol according to the mass ratio of 10:100 by 10 times, and adding the mixed solution to cut tobacco in a feeding procedure in a spraying manner according to the adding amount of 0.01% of the weight of the cut tobacco to prepare the cigarette with the number of 2A.
Diluting the mixed solution prepared by mixing the fine stalk vanilla extract FC-1, the fenugreek extract and the propylene glycol according to the mass ratio of 4:6:100 by 10 times, and adding the mixed solution to cut tobacco in a feeding procedure according to the adding amount of 0.01% of the weight of the cut tobacco in a spraying manner to prepare the cigarette with the number of 3A.
Qualitative and quantitative evaluation
The cigarettes 1A to 3A were qualitatively and quantitatively evaluated by the organization professional cigarette evaluation staff. Scoring standard reference for quantitative evaluation sensory quality evaluation is carried out on cigarettes 1A-3A and cigarettes according to national standard (GB 5606.4-2005), scoring evaluation results are shown in table 1.1, and description evaluation results are shown in table 1.2.
Table 1.1 sensory quality scoring evaluation table for cigarettes 1A, 2A, 3A
| Project | Gloss 5 | Fragrance 32 | Harmony 6 | Miscellaneous gases 12 | Irritation 20 | Aftertaste 25 | Totalizing |
| Blank space | - | 29 | 5 | 10 | 18 | 22 | 84 |
| 1A | - | 31 | 5.5 | 11 | 18.5 | 23 | 89 |
| 2A | - | 31 | 5.5 | 11 | 19 | 22.5 | 89 |
| 3A | - | 31.5 | 5.5 | 11 | 19 | 23.5 | 90.5 |
Table 1.2 sensory quality description evaluation table for cigarettes 1A, 2A, 3A
As shown in the above table, cigarettes 1A, 2A, 3A all scored better than the blank.
As shown in examples 1A and 2A, the application of the herba Lysimachiae Foenumgraeci extract FC-1 and the fenugreek extract to tobacco shreds can improve the sensory quality of cigarettes to a substantially equivalent degree.
As shown in example 3A, the herba Lysimachiae Foenumgraeci extract FC-1 is mixed with semen Trigonellae extract and applied to tobacco shred to further improve the sensory quality of cigarette. This shows that the combination of FC-1 and Fenugreek extract has better effect than the FC-1 or Fenugreek extract alone. FC-1 and fenugreek extract are combined, so that the synergistic effect is achieved, the problem that smoke is rough and aroma quality is reduced by singly using the fenugreek extract can be solved, the FC-1 and the fenugreek extract complement each other, and the sensory quality of cigarettes is truly improved.
Application example 2-extract of lysimachia capillipes + extract of tree moss; herb of common coltsfoot extract, fenugreek extract and tree moss extract
Diluting the mixed solution prepared by mixing the tree moss extract and the propylene glycol in a mass ratio of 15:100 by 10 times, and adding the mixed solution to cut tobacco in a feeding procedure according to the adding amount of 0.01% of the weight of the cut tobacco in a spraying manner to prepare the cigarette with the number of 1B.
Diluting the mixed solution prepared by mixing the tree moss extract, the fenugreek extract and the propylene glycol in a mass ratio of 10:5:100 by 10 times, and adding the mixed solution to the cut tobacco in a feeding procedure according to the adding amount of 0.01% of the weight of the cut tobacco in a spraying manner to prepare the cigarette with the number of 2B.
Diluting the mixed solution prepared by mixing the tree moss extract, the lysimachia capillipes hance extract FC-1 and the propylene glycol according to the mass ratio of 10:5:100 by 10 times, and adding the mixed solution to cut tobacco in a feeding procedure in a spraying manner according to the adding amount of 0.01% of the weight of the cut tobacco to prepare cigarettes with the number of 3B.
Diluting the mixed solution prepared by mixing the tree moss extract, the lysimachia capillipes hance extract FC-1, the fenugreek extract and the propylene glycol according to the mass ratio of 10:2:3:100 by 10 times, and adding the mixed solution to cut tobacco in a feeding procedure in a spraying manner according to the adding amount of 0.01% of the weight of the cut tobacco to prepare cigarettes, wherein the number is 4B.
Qualitative and quantitative evaluation
The cigarettes 1B-4B are qualitatively and quantitatively evaluated by the organization professional cigarette evaluation personnel. Scoring criteria for quantitative evaluation reference sensory quality evaluation was performed on cigarettes 1B-4B according to national standard (GB 5606.4-2005), scoring evaluation is shown in table 2.1 below, and description evaluation is shown in table 2.2 below.
Table 2.1 sensory quality scoring evaluation table for cigarettes 1B, 2B, 3B, 4B
| Project | Gloss 5 | Fragrance 32 | Harmony 6 | Miscellaneous gases 12 | Irritation 20 | Aftertaste 25 | Totalizing |
| Blank space | - | 29 | 5 | 10 | 18 | 22 | 84 |
| 1B | - | 31 | 5.5 | 11 | 18.5 | 23 | 89 |
| 2B | - | 31 | 5.5 | 11 | 19 | 23 | 89.5 |
| 3B | - | 31 | 5.5 | 11 | 19 | 23.5 | 90 |
| 4B | - | 31.5 | 5.5 | 11.5 | 19 | 23.5 | 91 |
Table 2.2 sensory quality description evaluation table for cigarettes 1B, 2B, 3B, 4B
As shown in the above table, cigarettes 1B, 2B, 3B, 4B all had better scores than the blank.
The scoring of the cigarette 2B is superior to that of the cigarette 1B, the fact that the fenugreek extract and the tree moss extract are combined is verified, the fenugreek extract and the tree moss extract complement each other, and a coordinated moss fragrance style can be obtained.
The score of the cigarette 3B is superior to that of the cigarette 1B, the combination of the lysimachia capillipes extract and the tree moss extract is verified, the two are in the best of each other, and the coordinated moss flavor can be obtained.
The scoring and evaluation of the cigarette 4B are better than those of the cigarettes 1B, 2B and 3B, which shows that the combination of the detail herb extract FC-1, the fenugreek extract and the tree moss extract has better effect than the independent use of the tree moss extract, the combination of the tree moss extract and the FC-1, and the combination of the tree moss extract and the fenugreek extract, shows that the combination of the FC-1 and the fenugreek extract has a synergistic effect, can highlight the style of the tree moss extract, and truly improves the sensory quality of the cigarettes.
Analytical detection example 3-fragrance component analytical detection and analysis of FC1
Aroma components of the Lysimachia capillipes extract FC-1 were analyzed by SPME-GC-MS (solid phase microextraction-gas chromatography-mass spectrometry) and GC-MS (gas chromatography-mass spectrometry).
The analysis steps are as follows:
3.1 preparation of sample to be tested
(1) GC-MS sample preparation: taking 1-3 g of a sample, adding 10ml of dichloromethane extract according to the condition of the sample, mechanically oscillating for 20min, taking the supernatant, preparing the sample, and measuring.
(3) SPME sample preparation: taking 1.0g of sample in a headspace bottle, adding 5ml of purified water, sealing, and measuring.
3.2GC-MS combination
Chromatographic column: HP-INNOWAX (19091N-136, 260 ℃,60 m.times.0.25 mm.times.0.25 μm);
sample inlet temperature: 240 ℃, sample injection amount: 1 μl; carrier gas: helium, split ratio 10: l;
heating program: column temperature 60 ℃ (hold 2 min), raise temperature to 180 ℃ at 2 ℃/min, raise temperature to 230 ℃ (hold 40 min) at 5 ℃/min;
transmission line temperature: 240 ℃; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃;
EI voltage: 70eV;
TIC full-scan detection, scan range: 35-450amu.
Qualitative analysis: the NIST2014 spectral library, in principle qualitative >80, is partly combined with literature and empirical decisions.
Semi-quantitative analysis: and uniformly adopting an internal standard phenethyl acetate to perform internal standard-semi-quantitative analysis.
The analysis results are shown in Table 3.1 below.
3.3 solid phase microextraction (solid-phase microextraction, SPME)
(1) SPME extraction fiber (Supelco, 30/50 μm DVB/CAR/PDMS)
(2) Agilent DB-17ms quartz capillary column (60 m 0.25mm 0.25 μm); heating program: keeping the temperature at 60 ℃ for 2min, firstly heating to 240 ℃ at 2 ℃/min, keeping the temperature for 2min, then heating to 300 ℃ at 10 ℃/min, and keeping the temperature for 20min; the flow rate of carrier gas (He) is 1.0mL/min, the temperature of the sample inlet is 250 ℃, and the sample is not split.
Mass spectrometry conditions: ion source: EI; electron energy: 70eV; transmission line temperature: 250 ℃; ion source temperature: 250 ℃; the temperature of the four-stage rod is 150 ℃; solvent delay: 8min; scan scanning is adopted, and the mass scanning range is between 45 and 300.
The components were characterized using NIST2014 spectral library search and the relative content of each component was calculated by peak area percentage method.
The analysis results are shown in Table 3.1 below.
3.4 analysis of aroma components of perfume FC-1
Aroma components of the perfume FC-1 were analysed using SPME-GC-MS (solid phase microextraction-gas chromatography-Mass Spectrometry) and GC-MS (gas chromatography-Mass Spectrometry). Among them, SPME-GC-MS detected 47 compounds, GC-MS detected 12 compounds, and these two detection means detected 56 compounds in total, as shown in Table 3.1.
Through literature research, 15 of the 56 compounds are aroma components of tobacco leaves; of these 22 are the aroma components of the fenugreek flavor, the content of which is 63.7% of the tested compounds (calculated as SPME-GC-MS) and 91.6% of the tested compounds (calculated as GC-MS), which also explains the material basis of the synergistic effect of the tobacco flavor of the vanilla and the fenugreek flavor and the improvement of the sensory quality of tobacco from the side.
As can be seen from the above component analysis, the aroma components of the lysimachia capillipes extract and the aroma components of the fenugreek extract are overlapped in a large amount, so that the two components are particularly coordinated in compounding use. Based on the above, it can be reasonably deduced that the lysimachia capillipes extract can be compounded with fenugreek in any proportion for use.
The application of tree moss extract can impart moss aroma to tobacco products. The tree moss extract and the fenugreek extract can be compounded and used according to any proportion according to the required moss style.
The analysis conclusion of the aroma components and the analysis conclusion of the sensory analysis are mutually proved, so that the vanilla extract and the fenugreek extract/tree moss extract of the present disclosure have the advantages of synergistic effect and improved sensory quality of tobacco.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same; while the invention has been described in detail with reference to the preferred embodiments, those skilled in the art will appreciate that: modifications may be made to the specific embodiments of the present invention or equivalents may be substituted for part of the technical features thereof; without departing from the spirit of the invention, it is intended to cover the scope of the invention as claimed.
Claims (16)
1. A flavor composition comprising a lysimachia capillipes extract and a compound extract;
the preparation method of the lysimachia capillipes extract comprises the following steps of:
(1) Carrying out steam distillation on the lysimachia capillipes raw material to ensure that the flow rate of steam condensate is 3-10 times of the weight of the lysimachia capillipes raw material per hour, the distillation time is 3-6 hours, and collecting distilled lysimachia capillipes solid matters;
(2) Extracting the vanilla solids of the pedunculata obtained in the step (1) by a solvent, carrying out solid-liquid separation after extraction, and collecting an extracting solution; wherein the solvent contains a polar solvent, and the polar solvent is selected from one or more of water and ethanol;
wherein the compound extract is a fenugreek extract and/or a tree moss extract.
2. The flavor composition according to claim 1, wherein in step (1), water is applied to the lysimachia capillipes raw material before the water vapor distillation, the water being 5 to 20% by weight of the lysimachia capillipes raw material.
3. The fragrance composition of claim 1, step (2) having one or more of the following features:
-the solvent extraction is subcritical fluid solvent extraction or ultrasonic assisted solvent extraction;
-the weight ratio of solvent to lysimachia capillipes raw material is 1-20: 1-20;
-the extraction temperature is 20-100 ℃;
the extraction time is 20-200 min each time.
4. The perfume composition of claim 1, wherein in step (2), the solvent further comprises a subcritical fluid.
5. The flavor composition of claim 4, wherein the subcritical fluid is dimethyl ether.
6. The flavor composition of claim 1, wherein step (2) is repeated a plurality of times and the extracts are combined.
7. The flavor composition of claim 1, the method of preparing a lysimachia capillipes extract further comprising the steps of:
(3) And (3) carrying out post-treatment on the extracting solution obtained in the step (2), wherein the post-treatment is one or more steps selected from refrigeration, freeze dewaxing, standing, centrifugation, concentration and dilution.
8. The fragrance composition of claim 7, said concentrating being evaporative concentration.
9. The fragrance composition of claim 8, wherein the temperature of the evaporative concentration is from 40 to 70 ℃.
10. The flavor composition of claim 1, wherein the lysimachia capillipes extract has a relative density of 1.0 to 1.3 at 20 ℃.
11. The flavor composition of claim 1, wherein the vanilla material is dried vanilla whole herb, or a cut product of dried vanilla whole herb, or a crushed product of dried vanilla whole herb.
12. A perfume composition according to claim 1, characterized in that one or more of the following:
-the weight ratio of the lysimachia capillipes extract to the fenugreek extract is 1-10: 0.01 to 10;
-the weight ratio of the lysimachia capillipes extract to the tree moss extract is 1-10: 0.01 to 10;
-the weight ratio of the lysimachia capillipes extract, the fenugreek extract and the tree moss extract is 1-10: 0.01 to 10:0.01 to 10;
-said fenugreek extract is a powder, extract or tincture;
-the tree moss extract is a powder, extract or tincture.
13. Use of a flavour composition according to any of claims 1 to 12 for the preparation of tobacco products.
14. The use according to claim 13, wherein the tobacco product is a combustion tobacco product, a heating non-combustion tobacco product or an atomized tobacco product.
15. A tobacco product containing a flavour composition according to any one of claims 1 to 12.
16. The tobacco product of claim 15, wherein the tobacco product is a combustion tobacco product, a heating non-combustion tobacco product, or an atomized tobacco product.
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