CN106036992A - Method for extracting tobacco additive from common fenugreek seeds by adopting supercritical extraction method - Google Patents
Method for extracting tobacco additive from common fenugreek seeds by adopting supercritical extraction method Download PDFInfo
- Publication number
- CN106036992A CN106036992A CN201610375408.6A CN201610375408A CN106036992A CN 106036992 A CN106036992 A CN 106036992A CN 201610375408 A CN201610375408 A CN 201610375408A CN 106036992 A CN106036992 A CN 106036992A
- Authority
- CN
- China
- Prior art keywords
- semen trigonellae
- supercritical extraction
- coarse powder
- supercritical
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000000654 additive Substances 0.000 title claims abstract description 33
- 230000000996 additive effect Effects 0.000 title claims abstract description 33
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 22
- 235000002637 Nicotiana tabacum Nutrition 0.000 title abstract description 11
- 244000250129 Trigonella foenum graecum Species 0.000 title abstract description 10
- 241000208125 Nicotiana Species 0.000 title abstract description 9
- 239000000284 extract Substances 0.000 claims abstract description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000843 powder Substances 0.000 claims abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 22
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012530 fluid Substances 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 12
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 10
- 210000000582 semen Anatomy 0.000 claims description 66
- 235000019504 cigarettes Nutrition 0.000 claims description 39
- 238000009288 screen filtration Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 10
- 239000003205 fragrance Substances 0.000 abstract description 10
- 239000000126 substance Substances 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000001917 trigonella foenum graecum l. absolute Substances 0.000 abstract 4
- 238000001914 filtration Methods 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 230000000873 masking effect Effects 0.000 abstract 1
- 240000009087 Crescentia cujete Species 0.000 description 6
- 235000005983 Crescentia cujete Nutrition 0.000 description 6
- 235000009797 Lagenaria vulgaris Nutrition 0.000 description 6
- 239000002304 perfume Substances 0.000 description 6
- 235000014676 Phragmites communis Nutrition 0.000 description 4
- 210000003734 kidney Anatomy 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 208000002193 Pain Diseases 0.000 description 3
- 230000001476 alcoholic effect Effects 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 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
- 241000790917 Dioxys <bee> Species 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 2
- WWNNZCOKKKDOPX-UHFFFAOYSA-N N-methylnicotinate Chemical compound C[N+]1=CC=CC(C([O-])=O)=C1 WWNNZCOKKKDOPX-UHFFFAOYSA-N 0.000 description 2
- 244000061176 Nicotiana tabacum Species 0.000 description 2
- WQLVFSAGQJTQCK-CAKNJAFZSA-N Yamogenin 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-CAKNJAFZSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- WQLVFSAGQJTQCK-UHFFFAOYSA-N diosgenin Natural products CC1C(C2(CCC3C4(C)CCC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 WQLVFSAGQJTQCK-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 150000008131 glucosides Chemical class 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 2
- 208000004998 Abdominal Pain Diseases 0.000 description 1
- 208000002881 Colic Diseases 0.000 description 1
- SHZGCJCMOBCMKK-UHFFFAOYSA-N D-mannomethylose Natural products CC1OC(O)C(O)C(O)C1O SHZGCJCMOBCMKK-UHFFFAOYSA-N 0.000 description 1
- PLAPMLGJVGLZOV-UHFFFAOYSA-N Epi-orientin Natural products OC1C(O)C(O)C(CO)OC1C1=C(O)C=C(O)C2=C1OC(C=1C=C(O)C(O)=CC=1)=CC2=O PLAPMLGJVGLZOV-UHFFFAOYSA-N 0.000 description 1
- FWCXELAAYFYCSR-UHFFFAOYSA-N Episamogenin Natural products CC1C(C2(CCC3C4(C)CC(O)C(O)CC4CCC3C2C2)C)C2OC11CCC(C)CO1 FWCXELAAYFYCSR-UHFFFAOYSA-N 0.000 description 1
- 208000010228 Erectile Dysfunction Diseases 0.000 description 1
- 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
- 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
- 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
- PTNJRKBWIYNFSY-UHFFFAOYSA-N Lirinin-O-methyl-ether Natural products COc1ccc-2c(CC3N(C)CCc4cc(OC)c(OC)c-2c34)c1 PTNJRKBWIYNFSY-UHFFFAOYSA-N 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
- 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
- QMQIQBOGXYYATH-IDABPMKMSA-N Ruscogenin Chemical compound O([C@@H]1[C@@H]([C@]2(CC[C@@H]3[C@@]4(C)[C@H](O)C[C@H](O)CC4=CC[C@H]3[C@@H]2C1)C)[C@@H]1C)[C@]11CC[C@@H](C)CO1 QMQIQBOGXYYATH-IDABPMKMSA-N 0.000 description 1
- BSUPFYRQXCQGLJ-UHFFFAOYSA-N Ruscogenin Natural products CC1CCC2(OC1)OC3C(O)C4C5CC=C6CC(O)CC(O)C6(C)C5CCC4(C)C3C2C BSUPFYRQXCQGLJ-UHFFFAOYSA-N 0.000 description 1
- 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
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-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
- 235000001484 Trigonella foenum graecum Nutrition 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
- 241001643642 Viticis Species 0.000 description 1
- 210000001015 abdomen Anatomy 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 230000000507 anthelmentic effect Effects 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
- 229960001231 choline Drugs 0.000 description 1
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 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
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- QMQIQBOGXYYATH-UHFFFAOYSA-N epiruscogenin Natural products CC1C(C2(CCC3C4(C)C(O)CC(O)CC4=CCC3C2C2)C)C2OC11CCC(C)CO1 QMQIQBOGXYYATH-UHFFFAOYSA-N 0.000 description 1
- 239000003172 expectorant agent Substances 0.000 description 1
- 230000003419 expectorant effect Effects 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives 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
- 239000004519 grease Substances 0.000 description 1
- 235000021384 green leafy vegetables Nutrition 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
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- LRDGATPGVJTWLJ-UHFFFAOYSA-N luteolin Natural products OC1=CC(O)=CC(C=2OC3=CC(O)=CC(O)=C3C(=O)C=2)=C1 LRDGATPGVJTWLJ-UHFFFAOYSA-N 0.000 description 1
- 235000009498 luteolin Nutrition 0.000 description 1
- IQPNAANSBPBGFQ-UHFFFAOYSA-N luteolin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C(O)=C1 IQPNAANSBPBGFQ-UHFFFAOYSA-N 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- PEFNSGRTCBGNAN-UHFFFAOYSA-N nephrocizin Natural products OC1C(O)C(O)C(CO)OC1OC1=CC(O)=C2C(=O)C=C(C=3C=C(O)C(O)=CC=3)OC2=C1 PEFNSGRTCBGNAN-UHFFFAOYSA-N 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
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229940109990 ruscogenin Drugs 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
- 230000035943 smell Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 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
- 235000001019 trigonella foenum-graecum Nutrition 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-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 invention provides a method for extracting a tobacco additive from common fenugreek seeds by adopting a supercritical extraction method. The method comprises the following steps: smashing common fenugreek seeds, filtering the smashed common fenugreek seeds to obtain common fenugreek seed coarse powder, adding 50-70% of alcohol with the weight being 0.5-2 times of that of the common fenugreek seed coarse powder into the common fenugreek seed coarse powder, carrying out baking at 50-60 DEG C for 1-5 h, adding the baked product into a supercritical extraction kettle, introducing supercritical carbon dioxide fluid into the supercritical extraction kettle, carrying out extraction for 5-10 h, adding an entrainer, carrying out extraction for 30-120 min, and separating the extract liquor obtained after the reextraction in a separation kettle, thus obtaining the common fenugreek seed tobacco additive. With the adoption of the method, the cells of the common fenugreek seeds swell, are heated and then crack, thus the aroma substances release easily, therefore, the yield of the product can be improved, in addition, the effects of enriching the tobacco fragrance, improving the quality of aroma, and masking the foreign smell are achieved, the whole process is simple and easy to master, the production is safe, and the industrial production can be completely satisfied.
Description
Technical field
The present invention relates to roll up the technical field that tobacco aromatics using extracts, be that one supercritical extraction is from calabash specifically
Lu Bazhong extracts the method for cigarette additive.
Background technology
Semen Trigonellae, warm in nature, bitter in the mouth, return kidney channel, for pulse family annual herb plant.Semen Trigonellae herb has strong lasting perfume (or spice)
Legumin abnormal smells from the patient, can be used as medicine, and has warming the kidney to activate YANG, and dispersing cold for relieving pain, lung moistening YIN nourishing, quiet brain are calmed the nerves, lax neural, the merit of removing obstruction in the collateral to relieve pain
Effect, is mainly used in treating colic of cold type, the abdomen side of body distension, the disturbance of lower legs due to pathogenic cold and dampness, the suffer from a deficiency of the kidney soreness of waist, sexual impotence etc..Semen Trigonellae is capable of using as feed；Tender stem, leaf
Vegetable can be made eat, steamed wheaten foods in pulverizing incorporation flour can be dried and make fumet；Seed hyoscine；Dry herb have anticorrosion, anthelmintic,
The special usefulness such as delousing.Volatile oil contained by herb is used for daily chemical products, Nicotiana tabacum L., and hygienic articles perfuming, as commodity spice
Raw material, industrial essence.
The dry mature seed that medical material Ji Yuan is leguminous plant Semen Trigonellae of Semen Trigonellae, has kidney invigorating and YANG supporting, dispels herein
Expectorant dehumidifying, effect of dispersing cold for relieving pain.The seed of Semen Trigonellae contains the alkaloids such as erythricine, carpaine, choline, trigonelline,
Ruscogenin is mainly diosgenin, Yamogenin and a small amount of gitogenin, trace Tigogenin.Still isolate Herba Viticis Cannabifoliae
Element, vitexin-7-glycoside, orientin or the Arabic glucoside of isorientin, glucose rhamnose two glucoside of flavone, Mongolian oak
The flavonoid such as Pi Su, luteolin.In addition to its Chinese medicine effect, additive prepared by Semen Trigonellae is mainly used in Nicotiana tabacum L. and food is fragrant
Essence.
Patent " preparation method of cigarette fenugreek concrete " (publication number: CN102952636A) discloses a kind of cigarette and uses calabash
The preparation method of bar extractum, the method uses high temperature reflux extracting mode to prepare cigarette additive so that natural fragrance component
And the loss of little molecule fragrance thing is more, flavouring essence quality is the highest.
Supercritical fluid extraction refers to supercritical fluid as solvent, extracts the separation of soluble constituent from solid or liquid
Operation.Supercritical fluid is in more than critical temperature and critical pressure, the fluid between gas and liquid.To have and change
The 3rd component becoming solute solubility is referred to as entrainer.Supercritical CO2Critical temperature close to room temperature, and have colourless, nontoxic,
Tasteless, be difficult to so, chemical inertness, inexpensive, easily make high-pure gas, efficiently, the most oxidizable, selective dissolution, pure natural, nothing
The features such as chemical contamination.Therefore supercritical CO2Extraction can effectively prevent oxidation and the loss of heat-sensitive substance, has extraction efficiency
The advantages such as high, energy consumption is less, raising production efficiency, reduction cost, technique is simple, be easily mastered.Supercritical extraction range of application
Wide, in medical industry, can be used for the extraction of effective component of Chinese herbal medicine, refining of thermal sensitivity biological medicine, and lipid
The separation of class mixture；In perfume industry, natural and synthetic perfume refined；The separation etc. of mixture in chemical industry.
Summary of the invention
Present invention aims to the natural fragrance component of spice prepared by prior art and little molecule fragrance thing
Lose more, the most high defect of flavouring essence quality, it is provided that a kind of supercritical extraction extracts cigarette additive from Semen Trigonellae
Method.The cigarette additive that the method can obtain flavouring essence quality at a lower temperature, product yield is the highest, and whole production
Process safety environmental protection, the extract of gained adds to can obtain good effect in Medicated cigarette.
It is an object of the invention to be achieved through the following technical solutions:
The method that described a kind of supercritical extraction extracts cigarette additive from Semen Trigonellae, it is characterised in that: will be dry
Dry Semen Trigonellae seed is pulverized and is filtered, and obtains Semen Trigonellae coarse powder；Its weight 0.5～2 times are added in gained Semen Trigonellae coarse powder
The ethanol of 50%～70%, stirs, and after bakeing 1～5 hour, adds supercritical extraction under conditions of temperature is 40～50 DEG C
Take in still；Supercritical carbon dioxide fluid is filled with in supercritical extraction reactor as extractant and is fully contacted with Semen Trigonellae coarse powder,
And extract 5～10 hours；The ethanol of the 95% of 0.5～1.5 times of interpolation Semen Trigonellae coarse powder weight in supercritical extraction reactor again,
Carrying out reextraction 30～120min, the temperature of reextraction is 40～55 DEG C, and extracting pressure is 25～40MPa；Dividing afterwards
Isolated Semen Trigonellae cigarette additive in still.
As preferably, described in be filtered into Semen Trigonellae is pulverized after with the screen filtration of 20 mesh.
As preferably, the separation temperature in described separating still is 35～50 DEG C, and separating pressure is 8～10MPa, main pump flow
Being 60～120kg/hr, auxiliary pump flow is 30～90kg/hr.
As preferably, described separating still is single separating still or the series connection of multiple separating still, is generally separated still and uses two strings
Connection, it is also possible to being three series connection, it is achieved multiple stage separation, each separating still separation temperature is 35～50 DEG C, separating pressure be 8～
10MPa, the temperature of multiple separating stills can be identical with separating pressure, it is also possible to different, if the pressure and temp of each separating still
Different, it is different that thing out understands some.
The present invention do not has temperature and pressure requirement during extraction for the first time, it is only necessary to carbon dioxide conversion is become fluid, note
Enter after extraction kettle, the intake valve in extraction kettle and air outlet valve are closed, carries out CO 2 fluid extraction.For the side of operation
Just, the most do not affect reextraction, when extraction for the first time, extraction temperature and extracting pressure can be directly adjusted to reextraction
Condition, extraction temperature is 40～55 DEG C, and extracting pressure is 25～40MPa.
The invention has the beneficial effects as follows:
1. the Semen Trigonellae seed being dried in the present invention is herb of gathering after Semen Trigonellae seed maturity in autumn, lays seed, removes
Clean impurity, the seed of the Semen Trigonellae dried, toast after being then added into ethanol, through baked Semen Trigonellae seed, fragrance has
Change significantly, compare the most baked raw Semen Trigonellae seed, there is burnt odor, baking perfume, and it extracts yield and also increases, and increases
Add tobacco aromatics using to smoke panel test effect.
2. the present invention utilizes supercritical carbon dioxide extraction technology, and Semen Trigonellae raw material is carried out ethanol infiltration, low temperature
The pretreatment bakeed, makes the cell of Semen Trigonellae raw material swell, by thermal fracture, and aroma substance release is more prone to, and can improve product
Product yield, and there is preferable flavouring essence quality.Again through associated clips such as supercritical carbon dioxide extraction or interpolation ethanol
The mode of band agent so that it is be fully contacted with Semen Trigonellae raw material, and then fully extract effective ingredient, carry high product yield, obtain calabash
Reed bar cigarette additive.This Semen Trigonellae cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, and energy
Cover the effect of miscellaneous QI.
3. the present invention makees solvent with supercritical carbon dioxide fluid and extracts, have nontoxic, inexpensively, do not burn, operate
The features such as mild condition, low-temperature extraction, inertia protection, few to the destruction of effective ingredient, it is therefore prevented that the oxidation of heat-sensitive substance and
Loss, makes extraction and separation be easy to unite two into one, and is effectively improved production efficiency, energy efficient, reduces cost.Producing
During can altogether dispense with any organic solvent, extract do not contain organic solvent residual, maintain the All Pure Nature of extract.
The existence of harmful thing is not produced in extraction process, will not be to environment.The method production safety of the present invention, work
Skill is simple, be easily mastered, and is fully able to meet industrialized production.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1, a kind of supercritical extraction extracts the method for cigarette additive from Semen Trigonellae, it is characterised in that tool
Body step is as follows:
With the screen filtration of 20 mesh after the Semen Trigonellae seed pulverizing being dried by 600g, obtain Semen Trigonellae coarse powder；Afterwards with 0.5
Semen Trigonellae coarse powder is fully infiltrated by the ethanol of the mass percent 50% of times Semen Trigonellae coarse powder weight, stirs, puts into baking oven,
After bakeing 1 hour under conditions of temperature is 50 DEG C, put in the supercritical extraction reactor of 3L；Supercritical carbon dioxide fluid is made
It is filled with in supercritical extraction reactor for extractant and is fully contacted with Semen Trigonellae coarse powder, and extract 5 hours, wherein supercritical carbon dioxide
The extraction temperature of fluid is 50 DEG C, and extracting pressure is 35MPa；After single extraction completes, in supercritical extraction reactor, add calabash
The edible ethanol that mass percent is 95% of 0.5 times of reed bar coarse powder weight, extracts 30min again；After having extracted, choosing
The separating still of one 2L, wherein the separation temperature in separating still is 40 DEG C, and separating pressure is 8MPa, and main pump flow is 80kg/hr,
The burgundy grease of isolated is Semen Trigonellae cigarette additive.
This Semen Trigonellae cigarette additive being diluted to the alcoholic solution of 1%, is sprayed onto in tobacco shred and makes Medicated cigarette, it adds
Amount is 5～20ppm.According to national standard method, Semen Trigonellae cigarette additive being carried out sensory evaluation, smoking result shows, this Semen Trigonellae
Cigarette additive has baking fragrance, has abundant cigarette perfume, improves flavouring essence quality, and can cover the effect of miscellaneous QI.
Embodiment 2, a kind of supercritical extraction extracts the method for cigarette additive from Semen Trigonellae, it is characterised in that tool
Body step is as follows:
With the screen filtration of 20 mesh after the Semen Trigonellae seed pulverizing that 6000g is dried, obtain Semen Trigonellae coarse powder, use calabash afterwards
Semen Trigonellae coarse powder is fully infiltrated by the ethanol of the mass percent 60% of reed bar coarse powder weight 0.6 times, stirs, puts into baking
Case, bakees 5 hours under conditions of temperature is 50 DEG C, puts in the supercritical extraction reactor of 10L；By supercritical carbon dioxide fluid
It is filled with in supercritical extraction reactor as extractant and is fully contacted with Semen Trigonellae coarse powder, and extract 10 hours, wherein supercritical dioxy
The extraction temperature changing carbon fluid is 50 DEG C, and extracting pressure is 35MPa；After single extraction completes, add in supercritical extraction reactor
Add the edible ethanol that mass percent is 95% of 1 times of Semen Trigonellae coarse powder weight, again extract 120min；Extract it
After, select two separating still series connection, wherein the separation temperature of first separating still is 45 DEG C, and separating pressure is 8MPa；Second
The separation temperature of separating still is 40 DEG C, and separating pressure is 5MPa, and main pump flow is 80kg/hr.The burgundy oily of isolated
Thing is Semen Trigonellae cigarette additive.
This Semen Trigonellae cigarette additive being diluted to the alcoholic solution of 1%, is sprayed onto in tobacco shred and makes Medicated cigarette, it adds
Amount is 5～20ppm.According to national standard method, Semen Trigonellae cigarette additive being carried out sensory evaluation, smoking result shows, this Semen Trigonellae
Cigarette additive has baking fragrance, has abundant cigarette fragrant, improves flavouring essence quality, covers the effect of miscellaneous QI.
Embodiment 3, a kind of supercritical extraction extracts the method for cigarette additive from Semen Trigonellae, it is characterised in that tool
Body step is as follows:
With the screen filtration of 20 mesh after the Semen Trigonellae seed pulverizing that 600g is dried, obtain Semen Trigonellae coarse powder, use calabash afterwards
Semen Trigonellae coarse powder is fully infiltrated by the ethanol of the mass percent 70% of reed bar coarse powder weight 0.7 times, stirs, puts into baking
Case, after bakeing 2 hours, puts in the supercritical extraction reactor of 3L under conditions of temperature is 45 DEG C；By stream of supercritical carbon dioxide
Body is filled with in supercritical extraction reactor as extractant and is fully contacted with Semen Trigonellae coarse powder, and extracts 8 hours, wherein supercritical dioxy
The extraction temperature changing carbon fluid is 50 DEG C, and extracting pressure is 35MPa；After single extraction completes, add in supercritical extraction reactor
Add the edible ethanol that mass percent is 95% of 0.75 times of Semen Trigonellae coarse powder weight, again extract 90min；Extract it
After, select two separating still series connection, wherein the separation temperature of first separating still is 40 DEG C, and separating pressure is 8MPa；Second
The separation temperature of separating still is 35 DEG C, and separating pressure is 5MPa, and main pump flow is 80kg/hr.The burgundy oily of isolated
Thing is Semen Trigonellae cigarette additive.
This Semen Trigonellae cigarette additive being diluted to the alcoholic solution of 1%, is sprayed onto in tobacco shred and makes Medicated cigarette, it adds
Amount is 5～20ppm.According to national standard method, Semen Trigonellae cigarette additive being carried out sensory evaluation, smoking result shows, this Semen Trigonellae
Cigarette additive has baking fragrance, has abundant cigarette fragrant, improves flavouring essence quality, covers the effect of miscellaneous QI.
Claims (4)
1. the method extracting cigarette additive from Semen Trigonellae with supercritical extraction, it is characterised in that concrete steps are such as
Under:
(1) dried Semen Trigonellae seed is pulverized and filtered, obtain Semen Trigonellae coarse powder；
(2) adding its weight 0.5～ethanol of the 50% of 2 times～70% in step (1) in gained Semen Trigonellae coarse powder, stirring is all
Even, after bakeing 1～5 hour under conditions of temperature is 50～60 DEG C, add in supercritical extraction reactor；
(3) supercritical carbon dioxide fluid is filled with in supercritical extraction reactor as extractant it is fully contacted with Semen Trigonellae coarse powder,
And extract 5～10 hours；
(4) second of 0.5～1.5 times 95% of interpolation Semen Trigonellae coarse powder weight in the backward supercritical extraction reactor that step (3) completes
Alcohol, carries out reextraction 30～120min, and the temperature of reextraction is 40～55 DEG C, and extracting pressure is 25～40MPa；
(5) the extract isolated Semen Trigonellae cigarette additive in separating still that will obtain in step (4), described separating still
Separation temperature is 35～50 DEG C, and separating pressure is 8～10MPa.
Supercritical extraction the most according to claim 1 extracts the method for cigarette additive from Semen Trigonellae, its feature
It is: be filtered into described in step (1) after Semen Trigonellae is pulverized with the screen filtration of 20 mesh.
Supercritical extraction the most according to claim 1 extracts the method for cigarette additive from Semen Trigonellae, its feature
Being: in described step (3), the extraction temperature of supercritical carbon dioxide fluid is 40～55 DEG C, extracting pressure is 25～40MPa,
Main pump flow is 60～120kg/hr, and auxiliary pump flow is 30～90kg/hr.
Supercritical extraction the most according to claim 1 extracts the method for cigarette additive from Semen Trigonellae, its feature
It is: described separating still is single separating still or multiple separating still is in series.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610375408.6A CN106036992B (en) | 2016-05-31 | 2016-05-31 | The method for extracting cigarette additive from faenum graecum with supercritical extraction |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610375408.6A CN106036992B (en) | 2016-05-31 | 2016-05-31 | The method for extracting cigarette additive from faenum graecum with supercritical extraction |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106036992A true CN106036992A (en) | 2016-10-26 |
| CN106036992B CN106036992B (en) | 2017-12-08 |
Family
ID=57172325
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610375408.6A Active CN106036992B (en) | 2016-05-31 | 2016-05-31 | The method for extracting cigarette additive from faenum graecum with supercritical extraction |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106036992B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967509A (en) * | 2017-05-19 | 2017-07-21 | 云南中烟工业有限责任公司 | A kind of supercritical extraction process of faenum graecum absolute oil |
| CN107954956A (en) * | 2017-12-01 | 2018-04-24 | 广西中烟工业有限责任公司 | It is a kind of that the method for fenugreck lactone is prepared based on column chromatography technology separation and is applied in cigarette |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050279373A1 (en) * | 2004-06-22 | 2005-12-22 | Rohit Prakash | Ayurvedic, herbal smoking composition |
| 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 |
| CN103952236A (en) * | 2014-05-22 | 2014-07-30 | 嘉兴市得百科新材料科技有限公司 | Perfume composition for fenugreek tobacco and preparation method thereof |
| CN105062678A (en) * | 2015-07-31 | 2015-11-18 | 湖北中烟工业有限责任公司 | Preparation method of cigarette fenugreek concrete |
-
2016
- 2016-05-31 CN CN201610375408.6A patent/CN106036992B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20050279373A1 (en) * | 2004-06-22 | 2005-12-22 | Rohit Prakash | Ayurvedic, herbal smoking composition |
| 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 |
| CN103952236A (en) * | 2014-05-22 | 2014-07-30 | 嘉兴市得百科新材料科技有限公司 | Perfume composition for fenugreek tobacco and preparation method thereof |
| CN105062678A (en) * | 2015-07-31 | 2015-11-18 | 湖北中烟工业有限责任公司 | Preparation method of cigarette fenugreek concrete |
Non-Patent Citations (1)
| Title |
|---|
| （印）安托卡托: "《天然食用香料与色素》", 30 September 2014, 中国轻工业出版社 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106967509A (en) * | 2017-05-19 | 2017-07-21 | 云南中烟工业有限责任公司 | A kind of supercritical extraction process of faenum graecum absolute oil |
| CN107954956A (en) * | 2017-12-01 | 2018-04-24 | 广西中烟工业有限责任公司 | It is a kind of that the method for fenugreck lactone is prepared based on column chromatography technology separation and is applied in cigarette |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106036992B (en) | 2017-12-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103013665B (en) | Preparation method of fenugreek extract Maillard reaction product and application of reaction product in cigarette | |
| CN101671600B (en) | Additives used in compound Chinese herbal medicine cigarette and use thereof | |
| KR100913243B1 (en) | A drink composition for eliminating hangover | |
| KR100910747B1 (en) | Herb medicine mixture extracts having antifungal, antiacne, skin calming, moisturizing and sebum controlling activities | |
| CN103450808B (en) | Method for extracting ginger oleoresin by adopting subcritical fluid butane | |
| CN104983066A (en) | Folium ginkgo and aloe tobacco substitute product and preparing method thereof | |
| CN101569438B (en) | Method for preparing mulberry cigarette flavor | |
| CN106221935A (en) | The preparation method of a kind of Pericarpium Citri Reticulatae absolute oil and the application in Medicated cigarette thereof | |
| CN103666761A (en) | Carrot extract and application thereof in tobacco flavoring and charging | |
| CN105410987A (en) | Nicotine liquid containing salvia miltiorrhiza extracts and preparing method of nicotine liquid | |
| CN106036992B (en) | The method for extracting cigarette additive from faenum graecum with supercritical extraction | |
| KR101281059B1 (en) | Shampoo composition and the manufacturing method thereof | |
| JP2006176436A (en) | Scf expression inhibitor | |
| CN106723276B (en) | A kind of tobacco aromaticss and preparation method thereof | |
| CN104086615B (en) | A kind of method preparing mogroside V from Grosvenor Momordica | |
| CN103710149B (en) | Wild chrysanthemum extract and taraxacum extract matched tobacco flavor, preparation method and application thereof | |
| CN105494814A (en) | Honeysuckle and cyclocarya paliurus substitutional tea and preparation method thereof | |
| CN105412613B (en) | A kind of formula and its processing method for senile dementia | |
| CN108567003A (en) | A kind of ultra micro composite mulberry leaf tea powder and preparation method thereof | |
| CN104957762B (en) | A kind of suspension type aerosol health care cigarette and preparation method thereof | |
| CN106119040A (en) | A kind of processing technology of dendrobium officinale health wine | |
| CN106263009A (en) | The preparation method of a kind of CHENPI DING and the application in Medicated cigarette thereof | |
| CN103271429B (en) | The application of moringa oleifera leaf extractive in cigarette and the cigarette containing moringa oleifera leaf extractive | |
| CN106139077A (en) | A kind of fragrant plant hair growth promoter and preparation method thereof | |
| KR102533237B1 (en) | Cosmetic composition containing complex medicinal herbs extract for improving condition of hair and preventing hair loss |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |