CN104560399A - Method for purifying jasmine flower extract for cigarettes - Google Patents
Method for purifying jasmine flower extract for cigarettes Download PDFInfo
- Publication number
- CN104560399A CN104560399A CN201410781153.4A CN201410781153A CN104560399A CN 104560399 A CN104560399 A CN 104560399A CN 201410781153 A CN201410781153 A CN 201410781153A CN 104560399 A CN104560399 A CN 104560399A
- Authority
- CN
- China
- Prior art keywords
- extract
- jasmine
- flower
- cigarettes
- extracting solution
- 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
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 36
- 239000000284 extract Substances 0.000 title claims abstract description 32
- 235000010254 Jasminum officinale Nutrition 0.000 title abstract description 20
- 238000000034 method Methods 0.000 title abstract description 6
- 240000005385 Jasminum sambac Species 0.000 title description 10
- 238000000746 purification Methods 0.000 claims abstract description 22
- 239000000287 crude extract Substances 0.000 claims abstract description 16
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000000926 separation method Methods 0.000 claims abstract description 11
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims abstract description 8
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims abstract description 8
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000005875 quercetin Nutrition 0.000 claims abstract description 8
- 229960001285 quercetin Drugs 0.000 claims abstract description 8
- 238000005238 degreasing Methods 0.000 claims abstract description 7
- 229930182486 flavonoid glycoside Natural products 0.000 claims abstract description 7
- 150000007955 flavonoid glycosides Chemical class 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 3
- 238000010992 reflux Methods 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 28
- 241000628997 Flos Species 0.000 claims description 17
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 239000000945 filler Substances 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 239000013049 sediment Substances 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 235000018958 Gardenia augusta Nutrition 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 238000000605 extraction Methods 0.000 abstract description 9
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 abstract description 8
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 8
- 239000000341 volatile oil Substances 0.000 abstract description 6
- 239000003208 petroleum Substances 0.000 abstract description 4
- 238000004062 sedimentation Methods 0.000 abstract description 4
- 230000000638 stimulation Effects 0.000 abstract description 2
- 241000207840 Jasminum Species 0.000 abstract 10
- 244000061176 Nicotiana tabacum Species 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000002791 soaking Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 239000003921 oil Substances 0.000 description 9
- 241000208125 Nicotiana Species 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 7
- 239000008868 Flower Essence Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 238000004587 chromatography analysis Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000005903 acid hydrolysis reaction Methods 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 244000269722 Thea sinensis Species 0.000 description 2
- -1 benzyl glycosides Chemical class 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 229930003944 flavone Natural products 0.000 description 2
- 150000002213 flavones Chemical class 0.000 description 2
- 235000011949 flavones Nutrition 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- ZUKLFFYDSALIQW-MSUKCBDUSA-N Iridoid glycoside Chemical compound [H][C@]12CC[C@H](C(O)=O)[C@@]1([H])[C@H](OC1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O)OC=C2 ZUKLFFYDSALIQW-MSUKCBDUSA-N 0.000 description 1
- 241000207834 Oleaceae Species 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000001088 anti-asthma Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 229930182489 iridoid glycoside Natural products 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 description 1
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000007920 subcutaneous administration Methods 0.000 description 1
- 231100000397 ulcer Toxicity 0.000 description 1
- 229940089401 xylon Drugs 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
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
- A24B15/26—Use of organic solvents for 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
- C11B9/025—Recovery by solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Seasonings (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention provides a method for purifying a jasmine flower extract for cigarettes. The method comprises the following steps: (1) degreasing jasmine flowers by soaking the jasmine flowers or jasmine flower residues obtained after jasmine essential oil extraction into petroleum ether; (2) performing reflux extraction of the degreased jasmine flowers, filtering and concentrating to obtain a crude extract; (3) adding an acid into the jasmine flower crude extract to make flavonoid glycosides totally hydrolyze, then adjusting the pH value to neutrality by adding an alkali, and then filtering to remove sedimentations to obtain an extract; (4) washing out and separating the extract obtained in the step (3) by using a high-performance liquid chromatography separation and purification column; and (5) collecting quercetin ingredients, concentrating the effluent product to obtain the jasmine flower extract for cigarettes. The method disclosed by the invention is simple and can purify the jasmine flower extract for the cigarettes with high purification degree under mild conditions, and the purification quality is stable; and the purified jasmine flower extract is used in cigarettes and can increase the aroma of the cigarettes and reduce the stimulation of the tobacco.
Description
Technical field
The present invention relates to the preparation method of cigarette flavors, especially relate to a kind of purification process of cigarette Flos Jasmini Sambac extract.
Background technology
At present, due to the progressively expansion of low burnt cigarette market, and the intrinsic flavor matter of adjoint many tobaccos loses along with the reduction of tar, so compensating aroma technology seems more and more important in perfuming cigarette is reinforced.Therefore, tobacco material is utilized to extract spices to prepare the research and apply attention of cigarette flavors.
Flower of Arabian Jasmine is the flower of Oleaceae plants jasmine, have regulate the flow of vital energy, open strongly fragrant, ward off dirty and in, clear fire of deficiency type cold removing disease, control sore, the effect such as the subcutaneous ulcer that disappears knurl, because of the fragrance of its uniqueness, make tea-drinking use, be the plant with extensive pharmaceutical use more.Flower of Arabian Jasmine is the common flowers of China, and Jasmine tea is conventional tea drink, very popular.Flower of Arabian Jasmine essential oil is also conventional tobacco aromatics using, and being used in cigarette to have increases cigarette perfume, reduces stimulation and waits effect.Research shows, Flower of Arabian Jasmine contains iridoid glycoside, flavonoid glycoside, benzyl glycosides etc.In Flower of Arabian Jasmine, Main Flavonoids composition is rutin and Quercetin glycosides, and both are flavones Quercetin through hydrolysis final product, and Quercetin has flavouring to fall the effect of thorn in tobacco aromatics using; As medicine, have eliminate the phlegm preferably, antitussive action, and have certain antiasthmatic effect.
At present, adopt the Flower of Arabian Jasmine essential oil of Petroleum ether extraction to be applied to cigarette more, extract application is less, after Petroleum ether extraction Flower of Arabian Jasmine essential oil, Flower of Arabian Jasmine raw material is rejected, and causes the wasting of resources, extracts in the Flower of Arabian Jasmine raw material of essential oil and also has the useful components such as Quercetin.But the Flos Jasmini Sambac extract that traditional extraction obtains lacks selectivity and specific aim, effective constituent cannot be trapped and purifying on the one hand, on the other hand some invalid components wherein or have the composition of disadvantageous effect still to exist to cigarette, cannot increase substantially aroma quality and the purity of product.
Summary of the invention
The object of the invention is the purification process that a kind of cigarette Flos Jasmini Sambac extract is provided according to the deficiencies in the prior art, the method can be purified into for the flavonoid flavor matter in Flower of Arabian Jasmine can the Flos Jasmini Sambac extract of cigarette, purification process is simple, mild condition, purification effect is good, and the jasmine residue extracting jasmin quintessence oil can be utilized to extract, and saves cost, the Flos Jasmini Sambac extract be purified into is for increasing cigarette flavor in cigarette, and reducing tobacco stimulates.
The present invention is achieved through the following technical solutions: a kind of purification process of cigarette Flos Jasmini Sambac extract, and its step comprises:
(1) Flower of Arabian Jasmine is soaked 1-8h with its weight 3-8 sherwood oil doubly and carry out degreasing, or adopt the Flower of Arabian Jasmine residue extracting jasmin quintessence oil;
(2) by the Flower of Arabian Jasmine after degreasing in step (1) with after alcohol reflux 1-3 time, filtering and concentrating obtains Flower of Arabian Jasmine crude extract;
(3) in Flower of Arabian Jasmine crude extract, add acid makes flavonoid glycoside be hydrolyzed completely, then adds alkali adjust ph for neutral, refilters removal sediment and obtains extracting solution;
(4) utilize high performance liquid chromatography separation and purification post, the extracting solution in step (3) is carried out wash-out separation; Described purification column adopts C18 filler, filler granularity 5 μm, and the system temperature that purification column is separated is 20-40 DEG C; Described moving phase is mass ratio is the methyl alcohol of 1:1-4 and the aqueous acetic acid of mass concentration 0.5%;
(5) collect quercetin component, after the product of outflow is concentrated, be described cigarette Flos Jasmini Sambac extract.
Preferably, after described step (3) completes, extracting solution nonpolar macroporous adsorption resin adsorbs, and uses water, ethanol elution successively, the ethanol eluate evaporation concentration obtained, and obtains Flower of Arabian Jasmine extracting solution after filtering, then carries out step (4).
Preferably, in described step (4), extracting solution first carries out ultrasonic degas before entering post.
Method of the present invention can be purified into for the flavonoid flavor matter in Flower of Arabian Jasmine can the Flos Jasmini Sambac extract of cigarette, and purification process is simple, and mild condition, purifying purity is high, steady quality.The Flower of Arabian Jasmine essential oil be purified into is for increasing cigarette flavor in cigarette, and reducing tobacco stimulates.
Accompanying drawing explanation
Fig. 1 is the liquid chromatogram of Flos Jasmini Sambac extract before embodiment 1 purifying;
Fig. 2 is the color atlas of Flos Jasmini Sambac extract after embodiment 1 purifying;
Fig. 3 is the first mass spectrometric figure of Flos Jasmini Sambac extract after embodiment 1 purifying;
Fig. 4 is the second order ms figure of Flos Jasmini Sambac extract after embodiment 1 purifying.
1#, 1.3-1.5min separated portion; 2#, 1.5-1.8min separated portion; 3#, 1.8-2.2min separated portion; 4#, 2.2-2.6min separated portion; 5#, 3.9-5min separated portion; 6#, 5.3-5.8min separated portion; 7#, 7.5-8.5min separated portion; 8#, 9.0-10.0min separated portion.
Embodiment
By the following specific examples further illustrate the invention:
Embodiment 1
(1) Flower of Arabian Jasmine taking 1kg is placed in extractor, soaks 5h carry out degreasing with 4kg sherwood oil.
(2), after sherwood oil having been volatilized, extract with the aqueous ethanolic solution that 5kg concentration is 40%, adopt supersound extraction 2 times; The Flower of Arabian Jasmine crude extract obtained by solvent extraction is filtered, and with Rotary Evaporators distillation removing ethanol, obtains crude extract for subsequent use;
(3) in crude extract, add the 0.5% aqueous sulfuric acid hydrolysis flavonoid glycoside of 1kg; After being hydrolyzed, adding sodium hydroxide neutralization and make extracting solution be neutral; By extract sample sedimentation 24h, filter, remove sediment;
(4) extracting solution AB-8 type absorption with macroporous adsorbent resin step (3) obtained, uses water, ethanol elution successively, and the ethanol eluate obtained utilizes rotary evaporation to concentrate, and with organic membrane filter, obtains extracting solution.
(5) ultrasonic degas is carried out to extracting solution;
(6) adopt Semipreparative chromatography sub-argument purification system, by above-mentioned degassed after extracting solution carry out wash-out separation; Separation condition adopts C18 filler, filler granularity 5 μm, system temperature 30 DEG C, and flow velocity is 3ml/min, and time segment carries out component collection;
Moving phase adopts the mixed solvent of methyl alcohol and mass concentration 0.5% aqueous acetic acid, and mass ratio is 50:50;
(7) by the solution concentration after time segment component collection.
As shown in Figure 1, to extracting solution according to 1.3-1.5min, 1.5-1.8min, 1.8-2.2min, 2.2-2.6min, 3.9-5min, 5.3-5.8min, 7.5-8.5min, 9.0-10.0min8 time period is divided into 1-8# group to carry out component collection respectively, and carries out cigarette effect assessment separately.
Specifically by above-mentioned each component with 75% ethanolic soln dilution after, add in cigarette, the adding proportion of each component is 3% of tobacco quality.Think after smokeing panel test, compared with contrast cigarette, 7# component Cigarette evaluation effect is better, and the flue gas Harmony of cigarette improves, and elegant fragrance is fine and smooth, and xylon gas reduces, and perfume quantity increases, pleasant impression Hui Tian.
As shown in Figure 2, by the jasmine flower essence after liquid-phase chromatographic analysis Flower of Arabian Jasmine crude extract and purifying.After purified, the content of 7# component brings up to 95.1% by original 32.6%.The jasmine flower essence of this component is carried out first mass spectrometric that mass spectroscopy obtains and second order ms spectrogram as shown in Figure 3,4.Can be judged by mass spectrum, be separated Quercetin (one of the flavones) composition that 7# component is Flower of Arabian Jasmine.The purity detecting of jasmine flower essence utilizes pump NewstyleNP7000 type, chromatographic column Venusi l MP C18250mm*4.6mm*5 μm, column temperature 35 DEG C, determined wavelength 510nm.
Embodiment 2
(1) take 1kg and cross the jasmine residue after jasmin quintessence oil through Petroleum ether extraction;
(2), after sherwood oil having been volatilized, extract with the aqueous ethanolic solution that 5kg concentration is 60%, adopt supersound extraction 1 time; The Flower of Arabian Jasmine crude extract obtained by solvent extraction is filtered, and with Rotary Evaporators distillation removing ethanol, obtains crude extract for subsequent use;
(3) in crude extract, add the 0.5% aqueous sulfuric acid hydrolysis flavonoid glycoside of 1kg; After being hydrolyzed, adding sodium hydroxide neutralization and make extracting solution be neutral; By extract sample sedimentation 24h, filter, remove sediment;
(4) extracting solution AB-8 type absorption with macroporous adsorbent resin step (3) obtained, uses water, ethanol elution successively, and the ethanol eluate obtained utilizes rotary evaporation to concentrate, and with organic membrane filter, obtains extracting solution.
(5) ultrasonic degas is carried out to extracting solution;
(6) adopt Semipreparative chromatography sub-argument purification system, by above-mentioned degassed after extracting solution carry out wash-out separation; Separation condition adopts C18 filler, filler granularity 5 μm, system temperature 20 DEG C, and flow velocity is 3ml/min, collect 7.5-8.5 minute go out peak component;
Moving phase adopts the mixed solvent of methyl alcohol and mass concentration 0.5% aqueous acetic acid, and mass ratio is 20:80;
(7) by 7.5-8.5 minute go out peak Fraction collection after solution concentration obtain described cigarette jasmine flower essence 2.
Embodiment 3
(1) Flower of Arabian Jasmine taking 1kg is placed in extractor, soaks 1h carry out degreasing with 8kg sherwood oil.
(2), after sherwood oil having been volatilized, extract with the aqueous ethanolic solution that 5kg concentration is 20%, adopt supersound extraction 3 times; The Flower of Arabian Jasmine crude extract obtained by solvent extraction is filtered, and with Rotary Evaporators distillation removing ethanol, obtains crude extract for subsequent use;
(3) in crude extract, add the 0.5% aqueous hydrochloric acid hydrolysis flavonoid glycoside of 1kg; After being hydrolyzed, adding sodium hydroxide neutralization and make extracting solution be neutral; By extract sample sedimentation 24h, filter, remove sediment;
(4) extracting solution AB-8 type absorption with macroporous adsorbent resin step (3) obtained, uses water, ethanol elution successively, and the ethanol eluate obtained utilizes rotary evaporation to concentrate, and with organic membrane filter, obtains extracting solution.
(5) ultrasonic degas is carried out to extracting solution;
(6) adopt Semipreparative chromatography sub-argument purification system, by above-mentioned degassed after extracting solution carry out wash-out separation; Separation condition adopts C18 filler, filler granularity 5 μm, system temperature 40 DEG C, and flow velocity is 3ml/min, collect 7.5-8.5 minute go out peak component;
Moving phase adopts the mixed solvent of methyl alcohol and mass concentration 0.5% aqueous acetic acid, and mass ratio is 40:60;
(7) by 7.5-8.5 minute go out peak Fraction collection after solution concentration obtain described cigarette jasmine flower essence 3.
Claims (3)
1. a purification process for cigarette Flos Jasmini Sambac extract, its step comprises:
(1) Flower of Arabian Jasmine is soaked 1-8h with its weight 3-8 sherwood oil doubly and carry out degreasing, or adopt the Flower of Arabian Jasmine residue extracting jasmin quintessence oil;
(2) by the Flower of Arabian Jasmine after degreasing in step (1) with after alcohol reflux 1-3 time, filtering and concentrating obtains Flower of Arabian Jasmine crude extract;
(3) in Flower of Arabian Jasmine crude extract, add acid makes flavonoid glycoside be hydrolyzed completely, then adds alkali adjust ph for neutral, refilters removal sediment and obtains extracting solution;
(4) utilize high performance liquid chromatography separation and purification post, the extracting solution in step (3) is carried out wash-out separation; Described purification column adopts C18 filler, filler granularity 5 μm, and the system temperature that purification column is separated is 20-40 DEG C; Described moving phase is mass ratio is the methyl alcohol of 1:1-4 and the aqueous acetic acid of mass concentration 0.5%;
(5) collect quercetin component, after the product of outflow is concentrated, be described cigarette Flos Jasmini Sambac extract.
2. the purification process of cigarette Flos Jasmini Sambac extract according to claim 1, it is characterized in that: after described step (3) completes, extracting solution nonpolar macroporous adsorption resin adsorbs, use water, ethanol elution successively, the ethanol eluate evaporation concentration obtained, and obtain Flower of Arabian Jasmine extracting solution after filtering, then carry out step (4).
3. the purification process of cigarette Flos Jasmini Sambac extract according to claim 1, it is characterized in that: in described step (4), extracting solution first carries out ultrasonic degas before entering post.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410781153.4A CN104560399B (en) | 2014-12-16 | 2014-12-16 | A kind of purification process of cigarette jasmine flower extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410781153.4A CN104560399B (en) | 2014-12-16 | 2014-12-16 | A kind of purification process of cigarette jasmine flower extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104560399A true CN104560399A (en) | 2015-04-29 |
| CN104560399B CN104560399B (en) | 2017-11-07 |
Family
ID=53077484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410781153.4A Active CN104560399B (en) | 2014-12-16 | 2014-12-16 | A kind of purification process of cigarette jasmine flower extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104560399B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105029681A (en) * | 2015-07-14 | 2015-11-11 | 中国烟草总公司郑州烟草研究院 | Natural perfume refining fluid suitable for cigarette fluid of electronic cigarettes and cigarette fluid and preparation method thereof |
| RU2594239C1 (en) * | 2015-05-20 | 2016-08-10 | Олег Иванович Квасенков | Method for production of hookah smoking composition |
| CN108395932A (en) * | 2018-03-29 | 2018-08-14 | 武汉黄鹤楼香精香料有限公司 | A kind of preparation method of cigarette jasmine oil |
| CN109105948A (en) * | 2018-07-05 | 2019-01-01 | 湖北中烟工业有限责任公司 | A kind of stage extraction preparation method and applications of jasmine flower extract |
| CN109401834A (en) * | 2017-08-16 | 2019-03-01 | 郎玉珍 | A kind of method of Jasmine petal low-temperature extraction Jasmine hydrosol |
| CN109609266A (en) * | 2018-12-29 | 2019-04-12 | 河南中烟工业有限责任公司 | A kind of quick-fried pearl cream jasmin france of cigarette, preparation method and application |
| CN113951534A (en) * | 2021-11-05 | 2022-01-21 | 云南中烟工业有限责任公司 | Jasmine extract, preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002437A (en) * | 2009-09-02 | 2011-04-06 | 湖北中烟工业有限责任公司 | Method for extracting cigarette additives from pre-degreased burdock by ethanol and application thereof |
| CN102090712A (en) * | 2010-12-29 | 2011-06-15 | 华宝食用香精香料（上海）有限公司 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
| CN102150948A (en) * | 2011-05-19 | 2011-08-17 | 湖北中烟工业有限责任公司 | Method for preparing jasmine extract for tobacco |
| CN102659740A (en) * | 2012-04-26 | 2012-09-12 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN103467425A (en) * | 2013-08-31 | 2013-12-25 | 塔里木大学 | Method for separating quercetin from oxytropis glabra |
| CN103695175A (en) * | 2013-12-13 | 2014-04-02 | 仙芝科技(福建)股份有限公司 | Method for extracting and separating components of osmanthus flower or arabian jasmine flower |
-
2014
- 2014-12-16 CN CN201410781153.4A patent/CN104560399B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002437A (en) * | 2009-09-02 | 2011-04-06 | 湖北中烟工业有限责任公司 | Method for extracting cigarette additives from pre-degreased burdock by ethanol and application thereof |
| CN102090712A (en) * | 2010-12-29 | 2011-06-15 | 华宝食用香精香料（上海）有限公司 | Method for preparing coarse extract of peanut shell total flavones and application thereof in cigarettes |
| CN102150948A (en) * | 2011-05-19 | 2011-08-17 | 湖北中烟工业有限责任公司 | Method for preparing jasmine extract for tobacco |
| CN102659740A (en) * | 2012-04-26 | 2012-09-12 | 西安医学院 | Method for extracting quercetin from eucommia leaves |
| CN103467425A (en) * | 2013-08-31 | 2013-12-25 | 塔里木大学 | Method for separating quercetin from oxytropis glabra |
| CN103695175A (en) * | 2013-12-13 | 2014-04-02 | 仙芝科技(福建)股份有限公司 | Method for extracting and separating components of osmanthus flower or arabian jasmine flower |
Non-Patent Citations (1)
| Title |
|---|
| 张新发!生物与化学工程系 武汉430023等: "茉莉花香料的提取及其应用的研究", 《武汉工业学院学报》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2594239C1 (en) * | 2015-05-20 | 2016-08-10 | Олег Иванович Квасенков | Method for production of hookah smoking composition |
| CN105029681A (en) * | 2015-07-14 | 2015-11-11 | 中国烟草总公司郑州烟草研究院 | Natural perfume refining fluid suitable for cigarette fluid of electronic cigarettes and cigarette fluid and preparation method thereof |
| CN109401834A (en) * | 2017-08-16 | 2019-03-01 | 郎玉珍 | A kind of method of Jasmine petal low-temperature extraction Jasmine hydrosol |
| CN108395932A (en) * | 2018-03-29 | 2018-08-14 | 武汉黄鹤楼香精香料有限公司 | A kind of preparation method of cigarette jasmine oil |
| CN109105948A (en) * | 2018-07-05 | 2019-01-01 | 湖北中烟工业有限责任公司 | A kind of stage extraction preparation method and applications of jasmine flower extract |
| CN109609266A (en) * | 2018-12-29 | 2019-04-12 | 河南中烟工业有限责任公司 | A kind of quick-fried pearl cream jasmin france of cigarette, preparation method and application |
| CN113951534A (en) * | 2021-11-05 | 2022-01-21 | 云南中烟工业有限责任公司 | Jasmine extract, preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104560399B (en) | 2017-11-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104560399A (en) | Method for purifying jasmine flower extract for cigarettes | |
| CN101570717B (en) | Method for preparing tobacco extract and application thereof | |
| CN103467540B (en) | A kind of method extracting rhodioside from Root of Kirilow Rhodiola | |
| CN106220698A (en) | A kind of method of separating high-purity Hesperidin, neohesperidin, naringin and Neosynephrine from Fructus Aurantii Immaturus | |
| CN101336949B (en) | Method for extracting polysaccharide and flavone from Gynura divaricata | |
| CN103436363B (en) | Preparation method of aroma substance in Zimbabwe tobacco extractive as well as products and application of aroma substance | |
| CN103923152A (en) | Method for extracting mogroside V | |
| CN104327948A (en) | Preparation method and application of chamomile spices for cigarettes | |
| CN102675398B (en) | A kind of method extracting momordica grosvenori glycoside V and farnesol from Grosvenor Momordica | |
| CN102532217B (en) | Method for purifying and separating high-content oleuropein from olive leaves | |
| CN103709014B (en) | High and the Hydroxytyrosol extracting method that the rate of recovery is high of a kind of transformation efficiency | |
| CN104926897A (en) | Method and system for extracting and separating novel Schaftoside in Desmodium styracifolium | |
| CN104825523A (en) | Wild chrysanthemum flower general flavone extraction method | |
| CN109123754B (en) | Efficient preparation method and application of red date absolute | |
| CN102648965A (en) | Industrialization preparation method of lophatherum gracile general flavone | |
| CN104725449A (en) | Paeoniflorin extracting method | |
| CN109181875B (en) | Method for extracting and refining green tea absolute oil for flavoring tobacco | |
| CN107595908A (en) | A kind of extracting method that notoginsenoside is extracted from fresh pseudo-ginseng | |
| CN104435015A (en) | High-quality ginkgetin extraction process | |
| CN109280582B (en) | Efficient preparation method of dried orange peel absolute oil for flavoring tobacco | |
| CN106256353A (en) | A kind of method of isolated and purified chlorogenic acid in mulberry leaves constituents | |
| CN109181877B (en) | Efficient extraction and refining method and application of tree moss absolute | |
| CN106336440A (en) | Method for extracting and separating out oleanolic acid from olive leaves | |
| CN101869605B (en) | Method for extracting and separating mulberry leaf flavone and alkaloid composite | |
| CN102603768A (en) | Method of using macroporous resin to separate and purify artemisinin |
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 |