CN106036992B - The method for extracting cigarette additive from faenum graecum with supercritical extraction - Google Patents
The method for extracting cigarette additive from faenum graecum with supercritical extraction Download PDFInfo
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- CN106036992B CN106036992B CN201610375408.6A CN201610375408A CN106036992B CN 106036992 B CN106036992 B CN 106036992B CN 201610375408 A CN201610375408 A CN 201610375408A CN 106036992 B CN106036992 B CN 106036992B
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- faenum graecum
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- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 41
- 239000000654 additive Substances 0.000 title claims abstract description 31
- 230000000996 additive effect Effects 0.000 title claims abstract description 31
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 24
- 239000000284 extract Substances 0.000 claims abstract description 20
- 238000000605 extraction Methods 0.000 claims description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- 238000000926 separation method Methods 0.000 claims description 13
- 239000012530 fluid Substances 0.000 claims description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 238000009288 screen filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 9
- 239000002304 perfume Substances 0.000 abstract description 9
- 239000000126 substance Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 abstract description 3
- 235000002637 Nicotiana tabacum Nutrition 0.000 description 7
- 239000003205 fragrance Substances 0.000 description 7
- 241000208125 Nicotiana Species 0.000 description 6
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- 235000005983 Crescentia cujete Nutrition 0.000 description 5
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- 230000001476 alcoholic effect Effects 0.000 description 3
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- 238000011156 evaluation Methods 0.000 description 3
- 230000001953 sensory effect Effects 0.000 description 3
- 230000000391 smoking effect Effects 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
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- 239000004480 active ingredient Substances 0.000 description 2
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- 231100000252 nontoxic Toxicity 0.000 description 2
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- ODBRNZZJSYPIDI-UHFFFAOYSA-N 3',4',5,7-tetrahydroxy-6-C-glucopyranosylflavone Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C=C(OC(=CC2=O)C=3C=C(O)C(O)=CC=3)C2=C1O ODBRNZZJSYPIDI-UHFFFAOYSA-N 0.000 description 1
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- 241000196324 Embryophyta Species 0.000 description 1
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- FWCXELAAYFYCSR-RYKNUXCGSA-N Gitogenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)C[C@@H](O)[C@H](O)C[C@@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 FWCXELAAYFYCSR-RYKNUXCGSA-N 0.000 description 1
- ZVWCWPUAQHAINU-UHFFFAOYSA-N Gitogenin Natural products CC1CCC2(CC3OC4C5CCC6CC(O)C(O)CC6(C)C5CCC4(C)C3C2C)OC1 ZVWCWPUAQHAINU-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
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- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- SHZGCJCMOBCMKK-JFNONXLTSA-N L-rhamnopyranose Chemical compound C[C@@H]1OC(O)[C@H](O)[C@H](O)[C@H]1O SHZGCJCMOBCMKK-JFNONXLTSA-N 0.000 description 1
- PNNNRSAQSRJVSB-UHFFFAOYSA-N L-rhamnose Natural products CC(O)C(O)C(O)C(O)C=O PNNNRSAQSRJVSB-UHFFFAOYSA-N 0.000 description 1
- 101710094902 Legumin Proteins 0.000 description 1
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- 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
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- RBVAFYCFAFADAG-UHFFFAOYSA-N Orientin Natural products OCC1OC(C(O)c2c(O)cc(O)c3C(=O)C=C(Oc23)c4ccc(O)c(O)c4)C(O)C1O RBVAFYCFAFADAG-UHFFFAOYSA-N 0.000 description 1
- -1 Pi Su Chemical class 0.000 description 1
- 241001480055 Quercus mongolica Species 0.000 description 1
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- GMBQZIIUCVWOCD-WWASVFFGSA-N Sarsapogenine Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)C[C@H]4CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@H](C)CO1 GMBQZIIUCVWOCD-WWASVFFGSA-N 0.000 description 1
- RTMWIZOXNKJHRE-UHFFFAOYSA-N Tigogenin Natural products CC1COC2CC(C)(OC12)C3CCC4C5CCC6CC(O)CCC6(C)C5CCC34C RTMWIZOXNKJHRE-UHFFFAOYSA-N 0.000 description 1
- DWCSNWXARWMZTG-UHFFFAOYSA-N Trigonegenin A Natural products CC1C(C2(CCC3C4(C)CCC(O)C=C4CCC3C2C2)C)C2OC11CCC(C)CO1 DWCSNWXARWMZTG-UHFFFAOYSA-N 0.000 description 1
- LQSNPVIQIPKOGP-UHFFFAOYSA-N UNPD159785 Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O LQSNPVIQIPKOGP-UHFFFAOYSA-N 0.000 description 1
- 244000029684 Vitex negundo var. negundo Species 0.000 description 1
- MOZJVOCOKZLBQB-UHFFFAOYSA-N Vitexin Natural products OCC1OC(Oc2c(O)c(O)cc3C(=O)C=C(Oc23)c4ccc(O)cc4)C(O)C(O)C1O MOZJVOCOKZLBQB-UHFFFAOYSA-N 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- AMSCMASJCYVAIF-QCVMBYIASA-N carpaine Chemical compound O([C@H]1CC[C@@H](CCCCCCCC(=O)O2)N[C@H]1C)C(=O)CCCCCCC[C@H]1N[C@@H](C)[C@@H]2CC1 AMSCMASJCYVAIF-QCVMBYIASA-N 0.000 description 1
- HXFUVYFNBRBBPM-UHFFFAOYSA-N carpaine Natural products CC1(CCCCCCCC(=O)O1)C2CCCN2 HXFUVYFNBRBBPM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 229960001231 choline Drugs 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
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- 230000007812 deficiency Effects 0.000 description 1
- WQLVFSAGQJTQCK-VKROHFNGSA-N diosgenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)CC[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 WQLVFSAGQJTQCK-VKROHFNGSA-N 0.000 description 1
- NEKNNCABDXGBEN-UHFFFAOYSA-L disodium;4-(4-chloro-2-methylphenoxy)butanoate;4-(2,4-dichlorophenoxy)butanoate Chemical compound [Na+].[Na+].CC1=CC(Cl)=CC=C1OCCCC([O-])=O.[O-]C(=O)CCCOC1=CC=C(Cl)C=C1Cl NEKNNCABDXGBEN-UHFFFAOYSA-L 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 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
- 235000013312 flour Nutrition 0.000 description 1
- DFNZYFAJQPLJFI-UHFFFAOYSA-N gentianine Chemical compound O=C1OCCC2=C1C=NC=C2C=C DFNZYFAJQPLJFI-UHFFFAOYSA-N 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 201000001881 impotence Diseases 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- ODBRNZZJSYPIDI-VJXVFPJBSA-N isoorientin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(OC(=CC2=O)C=3C=C(O)C(O)=CC=3)C2=C1O ODBRNZZJSYPIDI-VJXVFPJBSA-N 0.000 description 1
- UYJGIAWJIRZBNU-UHFFFAOYSA-N isoorientin Natural products OCC1OC(C(O)C(O)C1O)c2cc(O)c(O)c3C(=O)C=C(Oc23)c4ccc(O)c(O)c4 UYJGIAWJIRZBNU-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 235000021374 legumes Nutrition 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 230000001537 neural effect Effects 0.000 description 1
- PLAPMLGJVGLZOV-VPRICQMDSA-N orientin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O PLAPMLGJVGLZOV-VPRICQMDSA-N 0.000 description 1
- 244000045947 parasite Species 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 235000021251 pulses Nutrition 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- NWMIYTWHUDFRPL-UHFFFAOYSA-N sapogenin Natural products COC(=O)C1(CO)C(O)CCC2(C)C1CCC3(C)C2CC=C4C5C(C)(O)C(C)CCC5(CCC34C)C(=O)O NWMIYTWHUDFRPL-UHFFFAOYSA-N 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
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- 235000001366 vegetable intake Nutrition 0.000 description 1
- SGEWCQFRYRRZDC-VPRICQMDSA-N vitexin Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1C1=C(O)C=C(O)C2=C1OC(C=1C=CC(O)=CC=1)=CC2=O SGEWCQFRYRRZDC-VPRICQMDSA-N 0.000 description 1
- PZKISQRTNNHUGF-UHFFFAOYSA-N vitexine Natural products OC1C(O)C(O)C(CO)OC1OC1=C(O)C=C(O)C2=C1OC(C=1C=CC(O)=CC=1)=CC2=O PZKISQRTNNHUGF-UHFFFAOYSA-N 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Extraction Or Liquid Replacement (AREA)
- Manufacture Of Tobacco Products (AREA)
Abstract
The present invention provides a kind of method for extracting cigarette additive from faenum graecum with supercritical extraction.Methods described is specifically to crush faenum graecum seed to be filtrated to get faenum graecum coarse powder, then after 50%~70% ethanol for adding 0.5~2 times of its weight bakees 1~5 hour under conditions of being 50~60 DEG C in temperature, add in supercritical extraction reactor, it is filled with supercritical carbon dioxide extraction 5~10 hours, afterwards add entrainer extract 30~120min again, by the extract of reextraction in separating still isolated faenum graecum cigarette additive.The present invention makes the cell of faenum graecum raw material swell, by thermal fracture, aroma substance release is more prone to, product yield can be improved, and with abundant cigarette perfume, improve flavouring essence quality, and the effect of miscellaneous gas can be covered, whole technique is simple, is easily mastered, and production safety and is fully able to meet industrialized production.
Description
Technical field
It is specifically one kind supercritical extraction from calabash the present invention relates to the technical field of volume tobacco aromaticss extraction
The method that Lu Bazhong extracts cigarette additive.
Background technology
Faenum graecum, it is warm-natured, bitter, return kidney channel, be pulse family annual herb plant.Faenum graecum herb has strong lasting perfume (or spice)
It legumin smell, can be used as medicine, there is warming kidney and enhancing yang, eliminating cold to stop pain, moistening lung enriching yin, quiet brain is calmed the nerves, relax work(that is neural, removing obstruction in channels to relieve pain
Effect, it is mainly used in treating cold hernia, abdomen side of body turgor, the disturbance of lower legs due to pathogenic cold and dampness, the kidney deficiency soreness of waist, impotence etc..Faenum graecum is capable of using as feed；Tender stem, leaf
It can dry steamed wheaten foods in milling incorporation flour for vegetable consumption and make fumet；Seed hyoscine；Dry herb have anti-corrosion, expelling parasite,
The special efficiency such as delousing.Volatile oil contained by herb is used for daily chemical products, tobacco, hygienic articles perfuming, as commodity spices
Raw material, industrial essence.
The medicine elementary source of faenum graecum herein is the dry mature seed of legume fenugreek, has tonifying kidney and strengthening yang, dispels
The effect of phlegm dehumidifying, eliminating cold to stop pain.The seed of faenum graecum contains the alkaloids such as erythricine, carpaine, choline, trigonelline,
Sapogenin is mainly diosgenin, Yamogenin and a small amount of gitogenin, trace Tigogenin.Still separate five-leaved chaste tree
Element, the Arabic glucoside of Vitexin -7- glycosides, orientin or homo-orientin, the glucoside of glucose rhamnose two of flavones, Mongolian oak
The flavonoids such as Pi Su, cyanidenon.In addition to its Chinese medicine acts on, additive prepared by faenum graecum is mainly used in tobacco and food is fragrant
Essence.
Patent《The preparation method of cigarette fenugreek concrete》(publication number：CN102952636A) disclose a kind of cigarette and use cucurbit
The preparation method of bar medicinal extract, this method prepare cigarette additive using high temperature reflux extracting mode so that natural fragrance component
And the loss of small molecule flavor is more, flavouring essence quality is not high.
Supercritical fluid extraction refers to using supercritical fluid as solvent, and the separation of soluble constituent is extracted from solid or liquid
Operation.Supercritical fluid is the fluid between gas and liquid more than critical-temperature and critical pressure.To have and change
The third component for becoming solute solubility is referred to as entrainer.Supercritical CO2Critical-temperature close to room temperature, and with it is colourless, nontoxic,
It is tasteless, be not easy so, chemical inertness, it is inexpensive, high-pure gas is easily made, efficiently, not oxidizable, selective dissolution, pure natural, nothing
The features such as chemical contamination.Therefore supercritical CO2Extraction can effectively prevent the oxidation and loss of heat-sensitive substance, have extraction efficiency
It is high, energy consumption is less, improves production efficiency, reduce cost, technique is simple, the advantages that being easily mastered.Supercritical extract application
Wide, in medical industry, available for the extraction of effective component of Chinese herbal medicine, thermal sensitivity biological medicine refines, and lipid
The separation of class mixture；It is natural and synthetic perfume refined in perfume industry；Separation of mixture etc. in chemical industry.
The content of the invention
It is an object of the invention to the natural fragrance component for spices prepared by prior art and small molecule flavor
Lose the defects of more, flavouring essence quality is not high, there is provided a kind of to extract cigarette additive from faenum graecum with supercritical extraction
Method.This method can obtain the higher cigarette additive of flavouring essence quality, product yield at a lower temperature, and entirely produce
Process safety environmental protection, the extract of gained, which is added in cigarette, can obtain good effect.
The purpose of the present invention is achieved through the following technical solutions：
A kind of method for extracting cigarette additive from faenum graecum with supercritical extraction, it is characterised in that：Will be dry
Dry faenum graecum seed is crushed and filtered, and obtains faenum graecum coarse powder；0.5~2 times of its weight is added into gained faenum graecum coarse powder
50%~70% ethanol, stirs, and after being bakeed 1~5 hour under conditions of being 40~50 DEG C in temperature, adds overcritical extraction
Take in kettle；Supercritical carbon dioxide fluid is filled with supercritical extraction reactor as extractant and fully contacted with faenum graecum coarse powder,
And extract 5~10 hours；0.5~1.5 times of 95% ethanol of faenum graecum coarse powder weight is added into supercritical extraction reactor again,
30~120min of reextraction is carried out, the temperature of reextraction is 40~55 DEG C, and extracting pressure is 25~40MPa；Dividing afterwards
From isolated faenum graecum cigarette additive in kettle.
Preferably, it is described be filtered into faenum graecum is crushed after with the screen filtrations of 20 mesh.
Preferably, separation temperature in the separating still is 35~50 DEG C, separating pressure is 8~10MPa, main pump flow
For 60~120kg/hr, auxiliary pump flow is 30~90kg/hr.
Connected preferably, the separating still is single separating still or multiple separating stills, be generally separated kettle using two strings
Connection or three series connection, realize multi-stage separation, each separating still separation temperature is 35~50 DEG C, separating pressure is 8~
10MPa, the temperature and separating pressure of multiple separating stills can be with identical, can also be different, if the pressure and temp of each separating still
Different, it is different that thing out understands some.
There is no temperature and pressure requirement when being extracted for the first time in the present invention, it is only necessary to by carbon dioxide conversion into fluid, note
Enter to after extraction kettle, the intake valve in extraction kettle and air outlet valve are closed, carry out CO 2 fluid extraction.For the side of operation
Just, reextraction and is not influenceed, extraction temperature and extracting pressure can be directly adjusted to reextraction when extracting first time
Condition, extraction temperature be 40~55 DEG C, extracting pressure is 25~40MPa.
The beneficial effects of the invention are as follows：
1. the faenum graecum seed dried in the present invention is to harvest herb after faenum graecum autumn seed maturity, seed is laid, is removed
Net impurity, the seed of the faenum graecum dried, toasted after being then added into ethanol, by baked faenum graecum seed, fragrance tool
Change significantly, compared to not baked life faenum graecum seed, there is burnt odor, baking perfume, and it extracts yield and also increased, and increases
Tobacco aromaticss have been added to smoke panel test effect.
2. the present invention utilizes supercritical carbon dioxide extraction technology, ethanol infiltration, low temperature are carried out to faenum graecum raw material
The pretreatment of baking, the cell of faenum graecum raw material is swollen, be more prone to by thermal fracture, aroma substance release, production can be improved
Product yield, and there is preferable flavouring essence quality.Again by the associated clip such as supercritical carbon dioxide extraction or addition ethanol
Mode with agent, it is fully contacted with faenum graecum raw material, and then fully extract active ingredient, improve product yield, obtain calabash
Reed bar cigarette additive.The faenum graecum cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, and energy
Cover the effect of miscellaneous gas.
3. the present invention makees solvent with supercritical carbon dioxide fluid and extracted, have it is nontoxic, cheap, do not burn, operate
Mild condition, low-temperature extraction, inertia protection the features such as, the destruction to active ingredient is lacked, it is therefore prevented that the oxidation of heat-sensitive substance and
Loss, make extraction and separation be easy to be combined into one, be effectively improved production efficiency, save energy consumption, reduce cost.Producing
During can altogether dispense with any organic solvent, extract is free of organic solvent residual, maintains the All Pure Nature of extract.
The presence of harmful thing is not produced in extraction process, environment will not be polluted.Method production safety, the work of the present invention
Skill is simple, is easily mastered, and is fully able to meet industrialized production.
Embodiment
With reference to specific embodiment, the present invention is described in further detail.
Embodiment 1, a kind of method for extracting cigarette additive from faenum graecum with supercritical extraction, it is characterised in that tool
Body step is as follows：
With the screen filtration of 20 mesh after the faenum graecum seed crushing that 600g is dried, faenum graecum coarse powder is obtained；Afterwards with 0.5
The ethanol of the mass percent 50% of times faenum graecum coarse powder weight fully infiltrates faenum graecum coarse powder, stirs, is put into baking oven,
After being bakeed 1 hour under conditions of being 50 DEG C in temperature, it is put into 3L supercritical extraction reactor；Supercritical carbon dioxide fluid is made
It is filled with supercritical extraction reactor for extractant and is fully contacted with faenum graecum coarse powder, and extracts 5 hours, wherein supercritical carbon dioxide
The extraction temperature of fluid is 50 DEG C, extracting pressure 35MPa；After single extraction is completed, calabash is added into supercritical extraction reactor
0.5 times of mass percent of reed bar coarse powder weight is 95% edible ethanol, extracts 30min again；After extraction is completed, choosing
One 2L separating still, the separation temperature wherein in separating still is 40 DEG C, separating pressure 8MPa, and main pump flow is 80kg/hr,
Isolated burgundy grease is faenum graecum cigarette additive.
The faenum graecum cigarette additive is diluted to 1% alcoholic solution, is sprayed onto in pipe tobacco and cigarette is made, it is added
Measure as 5~20ppm.Sensory evaluation is carried out to faenum graecum cigarette additive according to national standard method, smoking result shows, the faenum graecum
Cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, and can cover the effect of miscellaneous gas.
Embodiment 2, a kind of method for extracting cigarette additive from faenum graecum with supercritical extraction, it is characterised in that tool
Body step is as follows：
With the screen filtration of 20 mesh after the faenum graecum seed crushing that 6000g is dried, faenum graecum coarse powder is obtained, uses calabash afterwards
The ethanol of the mass percent 60% of 0.6 times of reed bar coarse powder weight fully infiltrates faenum graecum coarse powder, stirs, and is put into baking
Case, bakee 5 hours, be put into 10L supercritical extraction reactor under conditions of being 50 DEG C in temperature；By supercritical carbon dioxide fluid
It is filled with supercritical extraction reactor as extractant and is fully contacted with faenum graecum coarse powder, and extract 10 hours, wherein overcritical dioxy
The extraction temperature for changing carbon flow body is 50 DEG C, extracting pressure 35MPa；After single extraction is completed, add into supercritical extraction reactor
The edible ethanol that 1 times of mass percent for adding faenum graecum coarse powder weight is 95%, extracts 120min again；Extract completion
Afterwards, connected from two separating stills, wherein the separation temperature of first separating still is 45 DEG C, separating pressure 8MPa；Second
The separation temperature of separating still is 40 DEG C, separating pressure 5MPa, and main pump flow is 80kg/hr.Isolated burgundy oily
Thing is faenum graecum cigarette additive.
The faenum graecum cigarette additive is diluted to 1% alcoholic solution, is sprayed onto in pipe tobacco and cigarette is made, it is added
Measure as 5~20ppm.Sensory evaluation is carried out to faenum graecum cigarette additive according to national standard method, smoking result shows, the faenum graecum
Cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, covers the effect of miscellaneous gas.
Embodiment 3, a kind of method for extracting cigarette additive from faenum graecum with supercritical extraction, it is characterised in that tool
Body step is as follows：
With the screen filtration of 20 mesh after the faenum graecum seed crushing that 600g is dried, faenum graecum coarse powder is obtained, uses calabash afterwards
The ethanol of the mass percent 70% of 0.7 times of reed bar coarse powder weight fully infiltrates faenum graecum coarse powder, stirs, and is put into baking
Case, after being bakeed 2 hours under conditions of being 45 DEG C in temperature, it is put into 3L supercritical extraction reactor；By stream of supercritical carbon dioxide
Body is filled with supercritical extraction reactor as extractant and fully contacted with faenum graecum coarse powder, and extracts 8 hours, wherein overcritical dioxy
The extraction temperature for changing carbon flow body is 50 DEG C, extracting pressure 35MPa；After single extraction is completed, add into supercritical extraction reactor
The edible ethanol that 0.75 times of mass percent for adding faenum graecum coarse powder weight is 95%, extracts 90min again；Extract completion
Afterwards, connected from two separating stills, wherein the separation temperature of first separating still is 40 DEG C, separating pressure 8MPa；Second
The separation temperature of separating still is 35 DEG C, separating pressure 5MPa, and main pump flow is 80kg/hr.Isolated burgundy oily
Thing is faenum graecum cigarette additive.
The faenum graecum cigarette additive is diluted to 1% alcoholic solution, is sprayed onto in pipe tobacco and cigarette is made, it is added
Measure as 5~20ppm.Sensory evaluation is carried out to faenum graecum cigarette additive according to national standard method, smoking result shows, the faenum graecum
Cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, covers the effect of miscellaneous gas.
Claims (2)
- A kind of 1. method for extracting cigarette additive from faenum graecum with supercritical extraction, it is characterised in that specific steps are such as Under：(1) dried faenum graecum seed is crushed and uses the screen filtration of 20 mesh, obtain faenum graecum coarse powder；(2) 50%~70% ethanol of 0.5~2 times of its weight is added in gained faenum graecum coarse powder into step (1), stirring is equal It is even, after being bakeed 1~5 hour under conditions of being 40~50 DEG C in temperature, add in supercritical extraction reactor；(3) supercritical carbon dioxide fluid is filled with supercritical extraction reactor as extractant and fully contacted with faenum graecum coarse powder, Extraction 5~10 hours；And the intake valve in extraction kettle and air outlet valve are closed in extraction process；(4) 0.5~1.5 times 95% of second of faenum graecum coarse powder weight is added in the backward supercritical extraction reactor of step (3) completion Alcohol, 30~120min of reextraction is carried out, the temperature of reextraction is 40~55 DEG C, and extracting pressure is 35~40MPa；(5) by the extract obtained in step (4), isolated faenum graecum cigarette additive, the separating still are in separating still It is in series by two separating stills, the separation temperature of separating still is 35~50 DEG C, and separating pressure is 8~10MPa.
- 2. the method according to claim 1 for extracting cigarette additive from faenum graecum with supercritical extraction, its feature It is：The extraction temperature of supercritical carbon dioxide fluid is 40~55 DEG C in the step (3), and extracting pressure is 25~40MPa, Main pump flow is 60~120kg/hr, and auxiliary pump flow is 30~90kg/hr.
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| CN107954956B (en) * | 2017-12-01 | 2021-09-07 | 广西中烟工业有限责任公司 | Method for separating and preparing fenugreek lactone based on column chromatography technology and application of fenugreek lactone in cigarettes |
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| CN101962598A (en) * | 2010-10-27 | 2011-02-02 | 江苏大学 | Essence composition for tobacco and preparation method thereof |
| CN102028734A (en) * | 2010-12-10 | 2011-04-27 | 湖北中烟工业有限责任公司 | Method for extracting flavone from fenugreek by microwave |
| CN103013665A (en) * | 2012-12-13 | 2013-04-03 | 湖北中烟工业有限责任公司 | Preparation method of fenugreek extract Maillard reaction product and application of reaction product in cigarette |
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