CN106753791A - A kind of method for preparing cigarette extract of licorice root - Google Patents
A kind of method for preparing cigarette extract of licorice root Download PDFInfo
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- CN106753791A CN106753791A CN201611113935.6A CN201611113935A CN106753791A CN 106753791 A CN106753791 A CN 106753791A CN 201611113935 A CN201611113935 A CN 201611113935A CN 106753791 A CN106753791 A CN 106753791A
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- licorice root
- extract
- licorice
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- 235000006200 Glycyrrhiza glabra Nutrition 0.000 title claims abstract description 108
- 244000303040 Glycyrrhiza glabra Species 0.000 title claims abstract description 82
- 235000017443 Hedysarum boreale Nutrition 0.000 title claims abstract description 81
- 235000007858 Hedysarum occidentale Nutrition 0.000 title claims abstract description 81
- 239000001947 glycyrrhiza glabra rhizome/root Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 41
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 28
- 238000000605 extraction Methods 0.000 claims abstract description 39
- 238000000199 molecular distillation Methods 0.000 claims abstract description 29
- 230000008961 swelling Effects 0.000 claims abstract description 13
- 238000001704 evaporation Methods 0.000 claims description 39
- 241000202807 Glycyrrhiza Species 0.000 claims description 28
- 235000001453 Glycyrrhiza echinata Nutrition 0.000 claims description 27
- 235000017382 Glycyrrhiza lepidota Nutrition 0.000 claims description 27
- 229940010454 licorice Drugs 0.000 claims description 27
- 238000004821 distillation Methods 0.000 claims description 12
- 230000001007 puffing effect Effects 0.000 claims description 9
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000002304 perfume Substances 0.000 abstract description 9
- 235000009508 confectionery Nutrition 0.000 abstract description 7
- VTAJIXDZFCRWBR-UHFFFAOYSA-N Licoricesaponin B2 Natural products C1C(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2)C(O)=O)C)(C)CC2)(C)C2C(C)(C)CC1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O VTAJIXDZFCRWBR-UHFFFAOYSA-N 0.000 abstract description 4
- 239000004480 active ingredient Substances 0.000 abstract description 4
- LPLVUJXQOOQHMX-UHFFFAOYSA-N glycyrrhetinic acid glycoside Natural products C1CC(C2C(C3(CCC4(C)CCC(C)(CC4C3=CC2=O)C(O)=O)C)(C)CC2)(C)C2C(C)(C)C1OC1OC(C(O)=O)C(O)C(O)C1OC1OC(C(O)=O)C(O)C(O)C1O LPLVUJXQOOQHMX-UHFFFAOYSA-N 0.000 abstract description 4
- UYRUBYNTXSDKQT-UHFFFAOYSA-N glycyrrhizic acid Natural products CC1(C)C(CCC2(C)C1CCC3(C)C2C(=O)C=C4C5CC(C)(CCC5(C)CCC34C)C(=O)O)OC6OC(C(O)C(O)C6OC7OC(O)C(O)C(O)C7C(=O)O)C(=O)O UYRUBYNTXSDKQT-UHFFFAOYSA-N 0.000 abstract description 4
- 239000001685 glycyrrhizic acid Substances 0.000 abstract description 4
- 229960004949 glycyrrhizic acid Drugs 0.000 abstract description 4
- 235000019410 glycyrrhizin Nutrition 0.000 abstract description 4
- LPLVUJXQOOQHMX-QWBHMCJMSA-N glycyrrhizinic acid Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@H](O[C@@H]1O[C@@H]1C([C@H]2[C@]([C@@H]3[C@@]([C@@]4(CC[C@@]5(C)CC[C@@](C)(C[C@H]5C4=CC3=O)C(O)=O)C)(C)CC2)(C)CC1)(C)C)C(O)=O)[C@@H]1O[C@H](C(O)=O)[C@@H](O)[C@H](O)[C@H]1O LPLVUJXQOOQHMX-QWBHMCJMSA-N 0.000 abstract description 4
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 3
- 238000012937 correction Methods 0.000 abstract description 3
- 239000003546 flue gas Substances 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 241000208125 Nicotiana Species 0.000 description 7
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- 235000019441 ethanol Nutrition 0.000 description 6
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003205 fragrance Substances 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 235000013599 spices Nutrition 0.000 description 4
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 206010011224 Cough Diseases 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- 206010062717 Increased upper airway secretion Diseases 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 125000005909 ethyl alcohol group Chemical group 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 2
- 208000026435 phlegm Diseases 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 238000009738 saturating Methods 0.000 description 2
- 210000000952 spleen Anatomy 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 235000019505 tobacco product Nutrition 0.000 description 2
- -1 2- acetyl group furans Chemical class 0.000 description 1
- MOMFXATYAINJML-UHFFFAOYSA-N 2-Acetylthiazole Chemical group CC(=O)C1=NC=CS1 MOMFXATYAINJML-UHFFFAOYSA-N 0.000 description 1
- OUDFNZMQXZILJD-UHFFFAOYSA-N 5-methyl-2-furaldehyde Chemical compound CC1=CC=C(C=O)O1 OUDFNZMQXZILJD-UHFFFAOYSA-N 0.000 description 1
- 244000205574 Acorus calamus Species 0.000 description 1
- 235000006480 Acorus calamus Nutrition 0.000 description 1
- 206010007247 Carbuncle Diseases 0.000 description 1
- 208000030453 Drug-Related Side Effects and Adverse reaction Diseases 0.000 description 1
- 206010013911 Dysgeusia Diseases 0.000 description 1
- 240000008917 Glycyrrhiza uralensis Species 0.000 description 1
- 235000000554 Glycyrrhiza uralensis Nutrition 0.000 description 1
- 241000594394 Hedyotis Species 0.000 description 1
- STECJAGHUSJQJN-GAUPFVANSA-N Hyoscine Natural products C1([C@H](CO)C(=O)OC2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-GAUPFVANSA-N 0.000 description 1
- 208000006083 Hypokinesia Diseases 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- STECJAGHUSJQJN-UHFFFAOYSA-N N-Methyl-scopolamin Natural products C1C(C2C3O2)N(C)C3CC1OC(=O)C(CO)C1=CC=CC=C1 STECJAGHUSJQJN-UHFFFAOYSA-N 0.000 description 1
- 206010033557 Palpitations Diseases 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 206010070863 Toxicity to various agents Diseases 0.000 description 1
- DOOTYTYQINUNNV-UHFFFAOYSA-N Triethyl citrate Chemical compound CCOC(=O)CC(O)(C(=O)OCC)CC(=O)OCC DOOTYTYQINUNNV-UHFFFAOYSA-N 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 239000012190 activator Substances 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000003266 anti-allergic effect Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- HSUIVCLOAAJSRE-UHFFFAOYSA-N bis(2-methoxyethyl) benzene-1,2-dicarboxylate Chemical compound COCCOC(=O)C1=CC=CC=C1C(=O)OCCOC HSUIVCLOAAJSRE-UHFFFAOYSA-N 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005352 clarification Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 235000015114 espresso Nutrition 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 206010016256 fatigue Diseases 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- LTINPJMVDKPJJI-UHFFFAOYSA-N iodinated glycerol Chemical compound CC(I)C1OCC(CO)O1 LTINPJMVDKPJJI-UHFFFAOYSA-N 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 210000004877 mucosa Anatomy 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 239000012476 oxidizable substance Substances 0.000 description 1
- 229940100595 phenylacetaldehyde Drugs 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 231100000241 scar Toxicity 0.000 description 1
- STECJAGHUSJQJN-FWXGHANASA-N scopolamine Chemical compound C1([C@@H](CO)C(=O)O[C@H]2C[C@@H]3N([C@H](C2)[C@@H]2[C@H]3O2)C)=CC=CC=C1 STECJAGHUSJQJN-FWXGHANASA-N 0.000 description 1
- 229960002646 scopolamine Drugs 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 239000001069 triethyl citrate Substances 0.000 description 1
- VMYFZRTXGLUXMZ-UHFFFAOYSA-N triethyl citrate Natural products CCOC(=O)C(O)(C(=O)OCC)C(=O)OCC VMYFZRTXGLUXMZ-UHFFFAOYSA-N 0.000 description 1
- 235000013769 triethyl citrate Nutrition 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 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
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
-
- 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
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention provides a kind of method for preparing cigarette extract of licorice root, and Radix Glycyrrhizae is cut into slices after high pressure swelling, then by supercritical CO2Extraction and molecular distillation obtain cigarette extract of licorice root.The inventive method improves the extraction yield of active ingredient in Radix Glycyrrhizae, and glycyrrhizic acid content is higher in the extract of licorice root for obtaining, and extract of licorice root is applied in cigarette, can play a part of abundant cigarette perfume, sweet flue gas, correction suction taste.
Description
Technical field
The present invention relates to natural extraction and separation technology field, specifically a kind of method for preparing cigarette extract of licorice root.
Background technology
Radix Glycyrrhizae, Latin literary fame：Glycyrrhiza uralensis Fisch. alias：State is old, Herba Hedyotis cantonensis, sweet root, pulse family,
Glycyrrhiza perennial herb, happiness is dark moist, and the low dry climate of sunshine temperature long is grown in arid, semiarid desert more
Grassland, desert edge and loess hill area.Root and root-like stock hyoscine, root and the thick shape of root-like stock, are a kind of help Chinese herbal medicines.
In cylindrical, 25~l00cm, 0.6~3.5cm of diameter long, crust is elastic to differ Medicinal Materials Characters root, surface rufous or greyish brown
Color；In cylinder, there is bud scar on surface to rhizome, and there is marrow at section middle part.Gas is micro-, and taste is sweet and special.Radix Glycyrrhizae have invigorate the spleen and benefit qi, heat-clearing
Removing toxic substances, expelling phlegm and arresting coughing, relieving spasm to stop pain, effect of coordinating the drug actions of a prescription.For weakness of the spleen and the stomach, lassitude hypodynamia, palpitation, phlegm of coughing
Many, gastral cavity abdomen, four limbs contraction, carbuncle sore tumefacting virus alleviate drug toxicity, strong.Radix Glycyrrhizae also has anti-inflammatory, and anti-allergic effects can be protected
The throat and tunica mucosa tracheae of inflammation of taking care of hair.
The fragrance of extract of licorice root is fresh and sweet herbal, is given off a strong fragrance, and persistently, aftertaste is soft for lasting.Current extract of licorice root
Largely used in tobacco product, food, cosmetics, flavouring effect and flavoring effect are fairly obvious.It is especially mentioned that,
Extract of licorice root is applied on tobacco product, can play a part of abundant cigarette perfume, sweet flue gas, correction suction taste.
Obtained by after directly concentration using solvent extraction method more than the current preparation for extract of licorice root, in this way
The total extractives yield of licorice raw material is relatively low, and the different effective cause perfume component in Radix Glycyrrhizae can not be extracted fully, it is impossible to be filled
Divide and utilize raw material.
The content of the invention
For current licorice the deficiencies in the prior art, the present invention provides a kind of side for preparing cigarette extract of licorice root
Method, high pressure swelling, SCF-CO 2, molecular distillation technique are applied to the preparation of extract of licorice root, can improve extract of licorice root
Yield and effective aroma component content, gained extract of licorice root is applied on tobacco, can play abundant cigarette perfume, sweet flue gas,
The effect of taste is inhaled in correction, for the quality and the market competitiveness that lift extract of licorice root, promotes it to have weight in the application of flavouring essence for tobacco
The meaning wanted.
A kind of method for preparing cigarette extract of licorice root, comprises the following steps：
1) high pressure swelling:Licorice tablet is put into pressure cooker, high pressure swelling, obtains licorice tablet boride, bulking pressure is 2
~10MPa；
2) supercritical CO2Extraction：By step 1) the licorice tablet puff that obtains is put into supercritical CO2In extraction instrument, add
Entrainer is extracted, and obtains licorice, wherein CO2Flow is 1~5Kg/h, and extracting pressure is 20~40MPa；
3) molecular distillation：By step 2) licorice of extraction injects the evaporative flask of molecular distillation equipment, and controls
Preheating temperature processed be 35~50 DEG C, evaporating temperature be 45~80 DEG C, chilling temperature be -5~-30 DEG C, wriggling pump frequency be 5~
50Hz, blade applicator rotating speed is 100~300rpm, and evaporating pressure is 0.5~30mbar, collects light component standby；
4) quadratic component distillation：By step 3) gained light component injects the evaporative flask of molecular distillation equipment, and control preheating
Temperature is 40~55 DEG C, and evaporating temperature is 50~90 DEG C, and chilling temperature is -10~-35 DEG C, and wriggling pump frequency is 5~30Hz, is scraped
Membrane device rotating speed is 60~200rpm, and evaporating pressure is 0.1~20mbar.
Preferably, the step 1) in by the licorice tablet that licorice segment is 0.5~1cm, be conducive to licorice tablet
It is expanded.
Preferably, the step 1) in puffing time be 10~30 minutes, swelling temperature be 25~35 DEG C.
Preferably, the step 2) in extraction time be 1~5h, extraction temperature be 30~60 DEG C.
Preferably, the step 3) in molecular distillation to control preheating temperature be 35~50 DEG C, evaporating temperature
It it is 45~80 DEG C, chilling temperature is -5~-30 DEG C, wriggling pump frequency is 5~50Hz, blade applicator rotating speed is 100~300rpm, is steamed
Hair pressure is 0.5~30mbar.
Preferably, the step 4) in quadratic component distillation control preheating temperature be 40~55 DEG C, evaporating temperature
It it is 50~90 DEG C, chilling temperature is -10~-35 DEG C, wriggling pump frequency is 5~30Hz, blade applicator rotating speed is 60~200rpm, is steamed
Hair pressure is 0.1~20mbar.
Preferably, the step 1) in bulking pressure be 5Mpa, puffing time be 20 minutes, swelling temperature is 30
℃。
Preferably, the step 2) in CO2Flow is 3Kg/h, and extracting pressure is 25MPa, and extraction time is 3h,
Extraction temperature is 50 DEG C.
Preferably, the step 3) in molecular distillation control preheating temperature for 48 DEG C, evaporating temperature is 60
DEG C, chilling temperature is -10 DEG C, and wriggling pump frequency is 35Hz, and blade applicator rotating speed is 150rpm, and evaporating pressure is 10mbar.
Preferably, the step 4) in quadratic component distillation control preheating temperature be 45 DEG C, evaporating temperature is 70
DEG C, chilling temperature is -25 DEG C, and wriggling pump frequency is 20Hz, and blade applicator rotating speed is 100rpm, and evaporating pressure is 8mbar.
Preferably, the step 2) in entrainer be one kind in absolute ethyl alcohol or ethyl acetate.
Preferably, the step 2) in entrainer consumption for Radix Glycyrrhizae coupon weight 2~10%.
The advantage of the invention is that：
1st, high pressure swelling causes plant cell wall to crush, and increases the extraction efficiency of active ingredient, meanwhile, puffing technique is extracted
Thing is low because of its Extracting temperature, can be sufficiently reserved the fragrance component in raw material.
2nd, the CO under supercriticality2Effective cause perfume component in Radix Glycyrrhizae can be dissolved out, then by reducing pressure
Power makes CO2Gasify in non-critical state, the cause that is carried perfume component is just and CO2Separate, carried so as to reach the fragrant component of effectively cause
Take the purpose of separation.The method extraction time is short, and recovery rate is higher, can carry out at low temperature, keeps some temperature sensitive flavor matters
It is not subject to high temperature.
3rd, the pre-treatment of high pressure swelling technology, improves the extraction efficiency of Radix Glycyrrhizae, and glycyrrhizic acid contains in the extract of licorice root for obtaining
Amount is high, effective cause perfume component different in abundant extract and separate raw material.The application of molecular distillation technique, to adapting to cigarette in Radix Glycyrrhizae
Flavoring and casing composition realizes enrichment, improves its perfume quantity and product quality.
Brief description of the drawings
Fig. 1 is the GC-MS TICs of extract of licorice root prepared by alcohol extracting taking technique；
Fig. 2 is the GC-MS TICs of extract of licorice root prepared by the inventive method.
Specific embodiment
Below in conjunction with specific embodiment, the technical scheme in the present invention is clearly and completely described.
Embodiment one
1) Radix Glycyrrhizae section (1cm) 400g is weighed, is put into pressure vessel, at a temperature of 25 DEG C, pressure is risen into 8MPa, protected
After holding 8 minutes, abrupt release pressure makes licorice tablet in puffy to normal pressure, standby；
2) weigh step 1) in the expanded licorice tablets of 200g be put into supercritical CO2In abstraction instrument, 6g absolute ethyl alcohols, setting are added
CO2Flow is 1Kg/h, and extracting pressure is 25MPa, and extraction time is 2h, and extraction temperature is 50 DEG C, is clarified, transparent liquid
Body is extract of licorice root.
3) extract of licorice root will be tentatively prepared, the evaporative flask of molecular distillation equipment is injected, and controls preheating temperature for 35 DEG C, steamed
Hair temperature is 48 DEG C, and chilling temperature is -10 DEG C, and wriggling pump frequency is 35Hz, and blade applicator rotating speed is 150rpm, and evaporating pressure is
5mbar, collects extract of licorice root light component one, standby.
4) by a molecular distillation gained extract of licorice root light component one, the evaporative flask of molecular distillation equipment is injected, and control
Preheating temperature is 45 DEG C, and evaporating temperature is 55 DEG C, and chilling temperature is -15 DEG C, and wriggling pump frequency is 10Hz, and blade applicator rotating speed is
90rpm, evaporating pressure is 10mbar, obtains extract of licorice root light component two, as extract of licorice root product.
Embodiment two
1) Radix Glycyrrhizae section (0.8cm) 300g is weighed, is put into pressure vessel, at a temperature of 28 DEG C, pressure is risen into 7MPa,
After being kept for 10 minutes, abrupt release pressure makes licorice tablet in puffy to normal pressure, standby；
2) weigh step 1) in the expanded licorice tablets of 240g be put into supercritical CO2In abstraction instrument, 7g absolute ethyl alcohols, setting are added
CO2Flow is 2Kg/h, and extracting pressure is 30MPa, and extraction time is 2h, and extraction temperature is 40 DEG C, is clarified, transparent liquid
Body is extract of licorice root.
3) extract of licorice root will be tentatively prepared, the evaporative flask of molecular distillation equipment is injected, and controls preheating temperature for 38 DEG C, steamed
Hair temperature is 50 DEG C, and chilling temperature is -7 DEG C, and wriggling pump frequency is 30Hz, and blade applicator rotating speed is 120rpm, and evaporating pressure is
6mbar, collects extract of licorice root light component one, standby.
4) by a molecular distillation gained extract of licorice root light component one, the evaporative flask of molecular distillation equipment is re-injected, and
It is 45 DEG C to control preheating temperature, and evaporating temperature is 55 DEG C, and chilling temperature is -15 DEG C, and wriggling pump frequency is 15Hz, blade applicator rotating speed
It is 80rpm, evaporating pressure is 10mbar, obtains extract of licorice root light component two, as extract of licorice root product.
Embodiment three
1) Radix Glycyrrhizae section (0.8cm) 300g is weighed, is put into pressure vessel, at a temperature of 28 DEG C, pressure is risen into 6MPa,
After being kept for 12 minutes, abrupt release pressure makes licorice tablet in puffy to normal pressure, standby；
2) weigh step 1) in the expanded licorice tablets of 200g be put into supercritical CO2In abstraction instrument, 10g ethyl acetate is added, if
Determine CO2Flow is 3Kg/h, and extracting pressure is 40MPa, and extraction time is 1.5h, and extraction temperature is 50 DEG C, is clarified, transparent
Liquid be extract of licorice root.
3) extract of licorice root will be tentatively prepared, the evaporative flask of molecular distillation equipment is injected, and controls preheating temperature for 30 DEG C, steamed
Hair temperature is 45 DEG C, and chilling temperature is -15 DEG C, and wriggling pump frequency is 30Hz, and blade applicator rotating speed is 200rpm, and evaporating pressure is
7mbar, collects extract of licorice root light component one, standby.
4) by a molecular distillation gained extract of licorice root light component one, the evaporative flask of molecular distillation equipment is re-injected, and
It is 40 DEG C to control preheating temperature, and evaporating temperature is 55 DEG C, and chilling temperature is -20 DEG C, and wriggling pump frequency is 20Hz, blade applicator rotating speed
It is 120rpm, evaporating pressure is 10mbar, obtains extract of licorice root light component two, as extract of licorice root product.
Example IV
1) Radix Glycyrrhizae section (0.5cm) 200g is weighed, is put into pressure vessel, at a temperature of 25 DEG C, pressure is risen into 7MPa,
After being kept for 10 minutes, abrupt release pressure makes licorice tablet in puffy to normal pressure, standby；
2) weigh step 1) in the whole expanded licorice tablets of 200g be put into supercritical CO2In abstraction instrument, 12g acetic acid second is added
Ester, sets CO2Flow is 4Kg/h, and extracting pressure is 30MPa, and extraction time is 1h, and extraction temperature is 55 DEG C, clarify, saturating
Bright liquid is extract of licorice root.
3) extract of licorice root will be tentatively prepared, the evaporative flask of molecular distillation equipment is injected, and controls preheating temperature for 40 DEG C, steamed
Hair temperature is 55 DEG C, and chilling temperature is -10 DEG C, and wriggling pump frequency is 30Hz, and blade applicator rotating speed is 160rpm, and evaporating pressure is
7mbar, collects extract of licorice root light component one, standby.
4) by a molecular distillation gained extract of licorice root light component one, the evaporative flask of molecular distillation equipment is re-injected, and
It is 50 DEG C to control preheating temperature, and evaporating temperature is 60 DEG C, and chilling temperature is -15 DEG C, and wriggling pump frequency is 20Hz, blade applicator rotating speed
It is 100rpm, evaporating pressure is 8mbar, obtains extract of licorice root light component two, as extract of licorice root product.
Embodiment five
1) Radix Glycyrrhizae section (0.8cm) 200g is weighed, is put into pressure vessel, at a temperature of 25 DEG C, pressure is risen into 8MPa,
After being kept for 8 minutes, abrupt release pressure makes licorice tablet in puffy to normal pressure, standby；
2) weigh step 1) in the whole expanded licorice tablets of 200g be put into supercritical CO2In abstraction instrument, 15g acetic acid second is added
Ester, sets CO2Flow is 4Kg/h, and extracting pressure is 30MPa, and extraction time is 1h, and extraction temperature is 55 DEG C, clarify, saturating
Bright liquid is extract of licorice root.
3) extract of licorice root will be tentatively prepared, the evaporative flask of molecular distillation equipment is injected, and controls preheating temperature for 40 DEG C, steamed
Hair temperature is 55 DEG C, and chilling temperature is -15 DEG C, and wriggling pump frequency is 30Hz, and blade applicator rotating speed is 160rpm, and evaporating pressure is
7mbar, collects extract of licorice root light component one, standby.
4) by a molecular distillation gained extract of licorice root light component one, the evaporative flask of molecular distillation equipment is re-injected, and
It is 50 DEG C to control preheating temperature, and evaporating temperature is 60 DEG C, and chilling temperature is -10 DEG C, and wriggling pump frequency is 15Hz, blade applicator rotating speed
It is 100rpm, evaporating pressure is 8mbar, obtains extract of licorice root light component two, as extract of licorice root product.
1st, the physical index such as table 1 of extract of licorice root prepared by the inventive method：
The physical index of extract of licorice root prepared by the inventive method of table 1
| Title | Extract of licorice root |
| Outward appearance | Clarification brown liquid |
| Fragrance | Herbal that Radix Glycyrrhizae is fresh and sweet, cream are fragrant and sweet |
| Relative density (20/20 DEG C) | 1.1880 |
| Refraction index (20 DEG C) | 1.4530 |
| Miscible degree (25 DEG C) | 1ml samples are dissolved in 70% alcoholic solution of 20ml |
| Lead content (mg/Kg) in heavy metal | ≤4 |
| Arsenic content (mg/Kg) in heavy metal | ≤1 |
2nd, cigarette is tested with Contrast on effect：
The difference of cigarette extract of licorice root prepared by the cigarette extract of licorice root and common process prepared for clear and definite the inventive method,
Both are contrasted.
Control group is the extract of licorice root extracted using common process；Extraction process is：Weigh 200.0g Radix Glycyrrhizaes section (1cm
Left and right), it is put into 2000ml flasks, add the ethanol that 1000ml volume fractions are 70%, refluxing extraction 3 hours, low temperature concentration
It is about 1.2 to relative density, crosses 80 mesh miillpore filter 2 times, obtains final product extract of licorice root.
Experimental group is the extract of licorice root of the inventive method.
1) extract of licorice root prepared by two methods is added in cigarette shreds carries out sensory effects and smokes panel test evaluation：
The medicinal extract of 0.02g is weighed, (addition of the spices in pipe tobacco is 100ppm, solvent in being added to the pipe tobacco of 200g
It is the ethanol that volume fraction is 70%), after being sealed with sealed plastic bag, balanced 0.5 hour in 60 DEG C of baking oven, then roll
Into cigarette, in 25~28 DEG C of temperature, humidity is to balance more than 2 hours under conditions of 50~60%, asks 7 specialties to be smoked panel test people at random
Member carries out Turkish tobaccos effect assessment as evaluation group.Evaluation result such as table 2：
Extract of licorice root cigarette effect assessment prepared by 2 two kinds of techniques of table
2) volatile and semi-volatile compounds are analyzed in the extract of licorice root prepared to two methods：
Chromatographic condition GC/MS conditions are：
Chromatographic column HP-5MS (50m × 0.25mm × 0.25 μm) capillary column；Injector temperature：250℃；Splitless injecting samples；
Carrier gas：He；Volume flow：1mL/min；Heating schedule：It is raised to 250 DEG C (5min) with 5 DEG C/min from 50 DEG C (1min)；Transmission line
Temperature：250℃；Ion gun：EI sources；Electron energy：70eV；50~650amu of sweep limits；Composed using WILEY and MINILAB
Retrieved in storehouse.
Sample processing conditions：Simultaneous distillation treatment is carried out with dichloromethane, is concentrated into after 1-1.5ml and is taken filtrate and enter
Row GC-MS is analyzed.Analysis gained GC-MS TICs are as depicted in figs. 1 and 2.
In extract of licorice root major volatile constituents be dimethoxyethyl phthalate, phthalic acid two (2- ethyls) oneself
Ester, 5- (1- piperidines) -2 furan carboxyaldehyde, furfural, 5 methyl furfural, triethyl citrate, phenylacetaldehyde, furfuryl alcohol, 2- acetyl group furans
Mutter, 2- acetyl group-Isosorbide-5-Nitrae, 5,6- tetrahydropyridines etc., for main component glycyrrhizic acid, the glycyrrhizic acid prepared by the present invention is
10.34%, prepared by conventional alcohol extraction process is 8.62%, improves 19.95%.
Extract of licorice root is analyzed through GC-MS, is composed storehouse by WILEY and MINILAB and is retrieved, Radix Glycyrrhizae leaching prepared by the present invention
Cream identifies 37 kinds of compounds, and extract of licorice root prepared by common process identifies 29 kinds, the extract of licorice root prepared using the present invention
In increased 8 kinds of compounds.
The various chemical compositions and its peak area percent content of extract of licorice root prepared by two kinds of techniques are determined, be the results are shown in Table
3, as shown in Table 3, the volatile ingredient appearance time of extract of licorice root prepared by common process is concentrated mainly on 4.17-
35.15min, predominantly effumability composition and volatile ingredient；Volatile ingredient is main in extract of licorice root prepared by the present invention
4.17-43.48min, predominantly medium volatile composition and volatile ingredient are concentrated on, and chemical composition species is abundant.
Extract of licorice root volatile ingredient comparison sheet prepared by 3 two kinds of techniques of table
It is a kind of efficient method of comparing that the puffing technique raw material comparatively dense to institutional framework carries out extraction.Its principle
It is that after raw material is placed in puffing apparatus, with heating, the carrying out of pressurization, the hydrone in raw material is in superheat state, and raw material is in itself
Become soft, open that puffing apparatus lid is wet when reaching certain high pressure, high pressure rapidly goes to normal pressure, is at this moment superheat state in raw material
Moisture just there is violent explosion in instant vaporization quickly, inflatable about 2000 times of hydrone, the huge bulbs of pressure are broken
Bad plant cell wall, raw material becomes loose porous.Puffing technique extract is low because of its Extracting temperature, is sufficiently reserved the perfume (or spice) in raw material
Gas composition, increases the extraction efficiency of active ingredient, therefore it is suitable for the tobacco aromaticss of the fine and close raw material of the institutional frameworks such as Radix Glycyrrhizae
Extraction.
Supercritical CO2Extraction (SFE), can be close to room temperature condition used as a kind of extraction process of new type natural spices
Extracted under (30-40 DEG C) and CO2 gases, effectively prevented the oxidation and dissipation of heat-sensitive material, therefore be particularly suitable for heat
The separation of unstability natural products and physiological activator and refined, preparation and production tide in accordance with the natural spices of note
Stream.
Molecular distillation is a kind of special liquid -- liquid isolation technics, and it is different from Conventional espresso and separates original by boiling-point difference
Reason, but realize separating by the difference of different material molecular tools, it is more than weight molecule that its operation principle is
Free path and be less than at light molecular free path one cryosurface of setting, light molecule is constantly condensate on cryosurface, weight molecule by
Slipped out along evaporating surface in cryosurface is not reached, so as to separate weight molecule, molecular weight differences are bigger, and separating effect is more obvious.Point
The more conventional distillation of son distillation has significant advantage：Vapo(u)rizing temperature is low, and heated time is short, and material will not be damaged in itself, because
This is adapted to be effectively separated higher boiling, thermal sensitivity, oxidizable material；Distillation pressure is small, vacuum is high, it is to avoid readily oxidizable substance
The oxidation Decomposition of matter；Additionally, whole the evaporating also of molecule has that separation degree is high, product recovery rate is high, separate it is irreversible, it is existing without boiling
As, it is simple to operate, the characteristics of clean environment firendly.Molecular distillation equipment is expensive, but product power consumption is small, once configuration will be saved significantly
Save energy consumption.
The present invention is by high pressure swelling, supercritical CO2Extraction, molecular distillation technique are applied to the preparation of extract of licorice root, improve
The content of its active ingredient, for the quality and the market competitiveness that lift extract of licorice root, promotes it to have in the application of flavouring essence for tobacco
Important meaning.
The above, specific embodiment only of the invention, but protection scope of the present invention is not limited thereto, and it is any
Belong to those skilled in the art the invention discloses technical scope in, the change or replacement that can be readily occurred in, all should
It is included within the scope of the present invention.Therefore, protection scope of the present invention should be defined by scope of the claims.
Claims (10)
1. a kind of method for preparing cigarette extract of licorice root, it is characterised in that comprise the following steps：
1) high pressure swelling:Licorice tablet being put into pressure cooker, high pressure swelling, obtain licorice tablet boride, bulking pressure is 2~
10MPa；
2) supercritical CO2Extraction：By step 1) the licorice tablet puff that obtains is put into supercritical CO2In extraction instrument, entrainment is added
Agent is extracted, and obtains licorice, wherein CO2Flow is 1~5Kg/h, and extracting pressure is 20~40MPa；
3) molecular distillation：By step 2) licorice of extraction injects the evaporative flask of molecular distillation equipment, and control pre-
Hot temperature is 35~50 DEG C, and evaporating temperature is 45~80 DEG C, and chilling temperature is -5~-30 DEG C, and wriggling pump frequency is 5~50Hz,
Blade applicator rotating speed is 100~300rpm, and evaporating pressure is 0.5~30mbar, collects light component standby；
4) quadratic component distillation：By step 3) gained light component injects the evaporative flask of molecular distillation equipment, and control preheating temperature
It it is 40~55 DEG C, evaporating temperature is 50~90 DEG C, chilling temperature is -10~-35 DEG C, wriggling pump frequency is 5~30Hz, blade applicator
Rotating speed is 60~200rpm, and evaporating pressure is 0.1~20mbar.
2. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 1) in by licorice
Segment is the licorice tablet of 0.5~1cm.
3. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 1) in puffing time
It it is 10~30 minutes, swelling temperature is 25~35 DEG C.
4. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 2) in extraction time
It is 1~5h, extraction temperature is 30~60 DEG C.
5. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 3) in a molecule
It is 35~50 DEG C that distillation controls preheating temperature, and evaporating temperature is 45~80 DEG C, and chilling temperature is -5~-30 DEG C, wriggling pump frequency
It is 5~50Hz, blade applicator rotating speed is 100~300rpm, and evaporating pressure is 0.5~30mbar.
6. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 4) in quadratic component
It is 40~55 DEG C that distillation controls preheating temperature, and evaporating temperature is 50~90 DEG C, and chilling temperature is -10~-35 DEG C, wriggling pump frequency
It is 5~30Hz, blade applicator rotating speed is 60~200rpm, and evaporating pressure is 0.1~20mbar.
7. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 1) in bulking pressure
It is 5Mpa, puffing time is 20 minutes, and swelling temperature is 30 DEG C.
8. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 2) in CO2Flow is
3Kg/h, extracting pressure is 25MPa, and extraction time is 3h, and extraction temperature is 50 DEG C.
9. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 3) in a molecule
It is 48 DEG C that distillation controls preheating temperature, and evaporating temperature is 60 DEG C, and chilling temperature is -10 DEG C, and wriggling pump frequency is 35Hz, blade applicator
Rotating speed is 150rpm, and evaporating pressure is 10mbar.
10. the method for preparing cigarette extract of licorice root as claimed in claim 1, it is characterised in that：The step 4) in secondary point
It is 45 DEG C that son distillation controls preheating temperature, and evaporating temperature is 70 DEG C, and chilling temperature is -25 DEG C, and wriggling pump frequency is 20Hz, knifing
Device rotating speed is 100rpm, and evaporating pressure is 8mbar.
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| CN112190607A (en) * | 2020-10-21 | 2021-01-08 | 鹰潭华宝香精有限公司 | Method for preparing licorice concentrate |
| CN115211492A (en) * | 2022-06-07 | 2022-10-21 | 圣道生物技术(山东)有限公司 | Stress relieving medicine for resisting stress and promoting growth of livestock and poultry and preparation method and application thereof |
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| CN105861154A (en) * | 2016-03-30 | 2016-08-17 | 浙江中烟工业有限责任公司 | A method of directionally separating aroma substances from tobacco by utilizing supercritical extraction and molecule distillation and applications of the aroma substances |
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| CN104450190A (en) * | 2014-12-03 | 2015-03-25 | 湖北中烟工业有限责任公司 | Method for preparing chamomile extract for tobaccos |
| CN104946397A (en) * | 2015-06-19 | 2015-09-30 | 湖北中烟工业有限责任公司 | Method for extracting vanilla extract used for tobacco through high-pressure puffing of supercritical CO2 |
| CN105779128A (en) * | 2016-03-30 | 2016-07-20 | 浙江中烟工业有限责任公司 | Cigarette product with high sensorial comfort level |
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| CN112190607A (en) * | 2020-10-21 | 2021-01-08 | 鹰潭华宝香精有限公司 | Method for preparing licorice concentrate |
| CN115211492A (en) * | 2022-06-07 | 2022-10-21 | 圣道生物技术(山东)有限公司 | Stress relieving medicine for resisting stress and promoting growth of livestock and poultry and preparation method and application thereof |
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Application publication date: 20170531 |