CN104560399B - A kind of purification process of cigarette jasmine flower extract - Google Patents
A kind of purification process of cigarette jasmine flower extract Download PDFInfo
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- CN104560399B CN104560399B CN201410781153.4A CN201410781153A CN104560399B CN 104560399 B CN104560399 B CN 104560399B CN 201410781153 A CN201410781153 A CN 201410781153A CN 104560399 B CN104560399 B CN 104560399B
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- jasmine
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- flower extract
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- 235000010254 Jasminum officinale Nutrition 0.000 title claims abstract description 67
- 239000000284 extract Substances 0.000 title claims abstract description 48
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 35
- 238000000746 purification Methods 0.000 title claims abstract description 23
- 240000005385 Jasminum sambac Species 0.000 title 1
- 241000207840 Jasminum Species 0.000 claims abstract description 66
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000926 separation method Methods 0.000 claims abstract description 21
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 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 11
- 239000003208 petroleum Substances 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 9
- 238000005238 degreasing Methods 0.000 claims abstract description 8
- 238000010828 elution Methods 0.000 claims abstract description 8
- 229930182486 flavonoid glycoside Natural products 0.000 claims abstract description 7
- 150000007955 flavonoid glycosides Chemical class 0.000 claims abstract description 7
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 7
- 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 6
- 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 6
- 238000004128 high performance liquid chromatography Methods 0.000 claims abstract description 6
- 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 6
- 235000005875 quercetin Nutrition 0.000 claims abstract description 6
- 229960001285 quercetin Drugs 0.000 claims abstract description 6
- 239000010656 jasmine oil Substances 0.000 claims abstract description 5
- 239000002253 acid Substances 0.000 claims abstract description 3
- 239000003513 alkali Substances 0.000 claims abstract description 3
- 238000010992 reflux Methods 0.000 claims abstract description 3
- 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
- 238000007872 degassing Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000007654 immersion Methods 0.000 claims description 4
- 238000001704 evaporation Methods 0.000 claims description 2
- 230000008020 evaporation Effects 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 235000002637 Nicotiana tabacum Nutrition 0.000 abstract description 8
- 239000000796 flavoring agent Substances 0.000 abstract description 8
- 235000019634 flavors Nutrition 0.000 abstract description 8
- 230000009467 reduction Effects 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 244000061176 Nicotiana tabacum Species 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 241000208125 Nicotiana Species 0.000 description 7
- 239000008868 Flower Essence Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000002250 absorbent Substances 0.000 description 3
- 230000002745 absorbent Effects 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 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
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- 238000002390 rotary evaporation Methods 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000000638 solvent extraction Methods 0.000 description 3
- 238000002137 ultrasound extraction Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LUJAXSNNYBCFEE-UHFFFAOYSA-N Quercetin 3,7-dimethyl ether Natural products C=1C(OC)=CC(O)=C(C(C=2OC)=O)C=1OC=2C1=CC=C(O)C(O)=C1 LUJAXSNNYBCFEE-UHFFFAOYSA-N 0.000 description 2
- PUTDIROJWHRSJW-UHFFFAOYSA-N Quercitrin Natural products CC1OC(Oc2cc(cc(O)c2O)C3=CC(=O)c4c(O)cc(O)cc4O3)C(O)C(O)C1O PUTDIROJWHRSJW-UHFFFAOYSA-N 0.000 description 2
- OXGUCUVFOIWWQJ-XIMSSLRFSA-N acanthophorin B Natural products O[C@H]1[C@H](O)[C@H](O)[C@H](C)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OXGUCUVFOIWWQJ-XIMSSLRFSA-N 0.000 description 2
- 238000005903 acid hydrolysis reaction Methods 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002170 ethers Chemical class 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
- OEKUVLQNKPXSOY-UHFFFAOYSA-N quercetin 3-O-beta-D-glucopyranosyl(1->3)-alpha-L-rhamnopyranosyl(1->6)-beta-d-galactopyranoside Natural products OC1C(O)C(C(O)C)OC1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OEKUVLQNKPXSOY-UHFFFAOYSA-N 0.000 description 2
- QPHXPNUXTNHJOF-UHFFFAOYSA-N quercetin-7-O-beta-L-rhamnopyranoside Natural products OC1C(O)C(O)C(C)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 QPHXPNUXTNHJOF-UHFFFAOYSA-N 0.000 description 2
- OXGUCUVFOIWWQJ-HQBVPOQASA-N quercitrin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OXGUCUVFOIWWQJ-HQBVPOQASA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000005303 weighing Methods 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
- -1 Quercetin glycosides Chemical class 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 208000025865 Ulcer Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000954 anitussive effect Effects 0.000 description 1
- 230000001088 anti-asthma Effects 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000001514 detection method Methods 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
- 238000000605 extraction 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
- 150000002338 glycosides Chemical class 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 229930182489 iridoid glycoside Natural products 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 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
- 238000010183 spectrum analysis Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000000638 stimulation Effects 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
Abstract
The invention provides a kind of purification process of cigarette jasmine flower extract, its step includes：(1) by Jasmine with petroleum ether soak degreasing or using the Jasmine residue for extracting refined jasmine oil；(2) after the Jasmine after degreasing is extracted with alcohol reflux, filtering and concentrating obtains crude extract；(3) acid is added into Jasmine crude extract to be made after flavonoid glycoside hydrolysis completely, and it is neutrality to add alkali regulation pH value, is refiltered removal precipitum and is obtained extract solution；(4) high performance liquid chromatography separation purification column is utilized, the extract solution in step (3) is subjected to elution separation；(5) quercetin component is collected, is the cigarette jasmine flower extract after the product concentration of outflow.The method of the present invention can be purified into can be with the jasmine flower extract of cigarette, and purification process is simple, mild condition, and purifying purity is high, steady quality.The jasmine flower extract being purified into is used in cigarette that cigarette flavor can be increased, and reduction tobacco stimulates.
Description
Technical field
The present invention relates to the preparation method of cigarette flavors, more particularly, to a kind of purifying of cigarette jasmine flower extract
Method.
Background technology
At present, due to the progressively expansion of low burnt cigarette market, and the intrinsic flavor matter of adjoint many tobaccos is with Jiao
Oil reduction and lose, so compensating aroma technology perfuming cigarette charging in seem more and more important.Therefore, it is former using tobacco
Material extracts spices to prepare the research of cigarette flavors and apply attention.
Jasmine is the flower of Oleaceae plants jasmine, with qi-regulating, open it is strongly fragrant, ward off it is dirty and in, clear fire of deficiency type cold removing disease, control sore
The effects such as poison, subcutaneous ulcer knurl that disappears, because of its unique fragrance, it is used as tea-drinking more, is the plant with extensive medical value.Jasmine is for I
The common flowers of state, jasmine tea is traditional teabag drink, very popular.Jasmine essential oil is also conventional tobacco aromaticss,
There is increase cigarette perfume in cigarette, reduction stimulation etc. is acted on.Research shows that Jasmine contains iridoid glycoside, flavonoid glycoside, benzyl
Base glycosides etc..Main Flavonoids composition is rutin and Quercetin glycosides in Jasmine, and both are flavones Quercetin through hydrolyzing final product,
Quercetin has the effect of flavouring drop thorn in tobacco aromaticss；As medicine, with preferable eliminating the phlegm, antitussive action, and have certain
Antiasthmatic effect.
At present, the jasmine essential oil extracted using petroleum ether is more applied to cigarette, and extract applies less, and petroleum ether is carried
Take after jasmine essential oil, Jasmine raw material is rejected, and causes the wasting of resources, extracted and also have quercitrin in the Jasmine raw material of essential oil
The useful components such as element.But the jasmine flower extract that traditional extraction is obtained lacks selectivity and specific aim, one side active ingredient
Trapping and purifying can not be obtained, another aspect some of which invalid components or the composition adversely affected to cigarette are still deposited
, it is impossible to increase substantially the aroma quality and purity of product.
The content of the invention
The purpose of the present invention is to provide a kind of purification process of cigarette jasmine flower extract according to the deficiencies in the prior art, should
The flavonoids flavor matter that method can be directed in Jasmine is purified into can be with the jasmine flower extract of cigarette, purification process letter
Single, mild condition, purification effect is good, and can be extracted using the jasmine residue for extracting refined jasmine oil, saves cost,
The jasmine flower extract being purified into is used in cigarette that cigarette flavor can be increased, and reduction tobacco stimulates.
The present invention is achieved through the following technical solutions：A kind of purification process of cigarette jasmine flower extract, its step
Including：
(1) Jasmine is subjected to degreasing with the petroleum ether immersion 1-8h of 3-8 times of its weight, or refined jasmine oil was extracted in use
Jasmine residue；
(2) after the Jasmine after degreasing in step (1) is extracted 1-3 times with alcohol reflux, filtering and concentrating obtains Jasmine
Crude extract；
(3) acid is added into Jasmine crude extract to be made after flavonoid glycoside hydrolysis completely, and it is neutrality to add alkali regulation pH value, then
Filtering removes precipitum and obtains extract solution；
(4) high performance liquid chromatography separation purification column is utilized, the extract solution in step (3) is subjected to elution separation；It is described pure
Change post and use C18 fillers, 5 μm of filler particle size, the system temperature for purifying post separation is 20-40 DEG C；The mobile phase is mass ratio
For 1:1-4 methanol and the aqueous acetic acid of mass concentration 0.5%；
(5) quercetin component is collected, is the cigarette jasmine flower extract after the product concentration of outflow.
It is preferred that, after the completion of the step (3), extract solution is adsorbed with nonpolar macroporous adsorption resin, successively with water, ethanol
Elution, obtained ethanol eluate is concentrated by evaporation, and obtains Jasmine extract solution after filtering, then carries out step (4).
It is preferred that, in the step (4), extract solution, which enters, first carries out ultrasonic degassing before post.
The flavonoids flavor matter that the method for the present invention can be directed in Jasmine is purified into and can carried with the Jasmine of cigarette
Thing is taken, and purification process is simple, mild condition, and purifying purity is high, steady quality.The jasmine essential oil being purified into is used for cigarette
In can increase cigarette flavor, reduction tobacco stimulates.
Brief description of the drawings
Fig. 1 is the liquid chromatogram of the jasmine flower extract before purification of embodiment 1；
Fig. 2 is the chromatogram of the jasmine flower extract after purification of embodiment 1；
Fig. 3 is the first mass spectrometric figure of the jasmine flower extract after purification of embodiment 1；
Fig. 4 is the second order mses figure of the jasmine flower extract after purification of embodiment 1.
1#, 1.3-1.5min separation component；2#, 1.5-1.8min separation component；3#, 1.8-2.2min separation component；4#、
2.2-2.6min separation component；5#, 3.9-5min separation component；6#, 5.3-5.8min separation component；7#, 7.5-8.5min points
From component；8#, 9.0-10.0min separation component.
Embodiment
By the following specific examples further illustrate the invention：
Embodiment 1
(1) Jasmine for weighing 1kg is placed in extractor, and degreasing is carried out with 4kg petroleum ethers immersion 5h.
(2) after the completion of petroleum ether is volatilized, extracted with 5kg concentration for 40% ethanol water, using ultrasonic extraction 2
It is secondary；The Jasmine crude extract obtained by solvent extraction is filtered, and ethanol is distilled off with Rotary Evaporators, crude extract is obtained
It is standby；
(3) 1kg 0.5% aqueous sulfuric acid hydrolysis flavonoid glycoside is added into crude extract；After the completion of hydrolysis, hydroxide is added
Sodium, which is neutralized, makes extract solution in neutrality；Extract sample is settled into 24h, precipitum is removed in filtering；
(4) extract solution for obtaining step (3) AB-8 types macroporous absorbent resin is adsorbed, and successively with water, ethanol elution, is obtained
The ethanol eluate arrived is concentrated using rotary evaporation, and uses organic membrane filter, obtains extract solution.
(5) ultrasonic degassing is carried out to extract solution；
(6) semipreparative high performance liquid chromatography sub-argument purification system is used, the extract solution after above-mentioned degassing is eluted
Separation；Separation condition uses C18 fillers, 5 μm of filler particle size, 30 DEG C of system temperature, and flow velocity is 3ml/min, and time segment is carried out
Component collection；
Mobile phase is using the mixed solvent of methanol and the aqueous acetic acid of mass concentration 0.5%, and mass ratio is 50:50；
(7) by the solution concentration after time segment component collection.
As shown in figure 1, to extract 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 periods are divided into 1-8# groups and carry out composition receipts respectively
Collection, and each carry out cigarette effect assessment.
Specifically above-mentioned each component is added in cigarette, the adding proportion of each component with after 75% ethanol solution dilution
For the 3% of tobacco quality.Think after smokeing panel test, compared with compareing cigarette, 7# component Cigarette evaluations effect is preferable, the flue gas of cigarette
Harmony improves, and elegant fragrance is fine and smooth, and xylon gas are reduced, perfume quantity increase, pleasant impression Hui Tian.
As shown in Fig. 2 passing through liquid-phase chromatographic analysis Jasmine crude extract and jasmine flower essence after purification.After purified,
The content of 7# components brings up to 95.1% by original 32.6%.The jasmine flower essence of the component is carried out what mass spectral analysis was obtained
First mass spectrometric and second order mses spectrogram are as shown in Figure 3,4.It may determine that by mass spectrogram, separated 7# components are the quercitrin of Jasmine
Plain (one kind of flavones) composition.The purity detecting of jasmine flower essence is to utilize pump NewstyleNP7000 types, chromatographic column Venusi
L MP C18250mm*4.6mm*5 μm, 35 DEG C of column temperature, Detection wavelength 510nm.
Embodiment 2
(1) the jasmine residue after 1kg extracted refined jasmine oil through petroleum ether is weighed；
(2) after the completion of petroleum ether is volatilized, extracted with 5kg concentration for 60% ethanol water, using ultrasonic extraction 1
It is secondary；The Jasmine crude extract obtained by solvent extraction is filtered, and ethanol is distilled off with Rotary Evaporators, crude extract is obtained
It is standby；
(3) 1kg 0.5% aqueous sulfuric acid hydrolysis flavonoid glycoside is added into crude extract；After the completion of hydrolysis, hydroxide is added
Sodium, which is neutralized, makes extract solution in neutrality；Extract sample is settled into 24h, precipitum is removed in filtering；
(4) extract solution for obtaining step (3) AB-8 types macroporous absorbent resin is adsorbed, and successively with water, ethanol elution, is obtained
The ethanol eluate arrived is concentrated using rotary evaporation, and uses organic membrane filter, obtains extract solution.
(5) ultrasonic degassing is carried out to extract solution；
(6) semipreparative high performance liquid chromatography sub-argument purification system is used, the extract solution after above-mentioned degassing is eluted
Separation；Separation condition uses C18 fillers, 5 μm of filler particle size, 20 DEG C of system temperature, and flow velocity is 3ml/min, collects 7.5-8.5 point
The appearance component of clock；
Mobile phase is using the mixed solvent of methanol and the aqueous acetic acid of mass concentration 0.5%, and mass ratio is 20:80；
(7) the solution concentration after the appearance Fraction collection of 7.5-8.5 minutes is obtained into the cigarette jasmine flower essence
2。
Embodiment 3
(1) Jasmine for weighing 1kg is placed in extractor, and degreasing is carried out with 8kg petroleum ethers immersion 1h.
(2) after the completion of petroleum ether is volatilized, extracted with 5kg concentration for 20% ethanol water, using ultrasonic extraction 3
It is secondary；The Jasmine crude extract obtained by solvent extraction is filtered, and ethanol is distilled off with Rotary Evaporators, crude extract is obtained
It is standby；
(3) 1kg 0.5% aqueous hydrochloric acid solution hydrolysis flavonoid glycoside is added into crude extract；After the completion of hydrolysis, hydroxide is added
Sodium, which is neutralized, makes extract solution in neutrality；Extract sample is settled into 24h, precipitum is removed in filtering；
(4) extract solution for obtaining step (3) AB-8 types macroporous absorbent resin is adsorbed, and successively with water, ethanol elution, is obtained
The ethanol eluate arrived is concentrated using rotary evaporation, and uses organic membrane filter, obtains extract solution.
(5) ultrasonic degassing is carried out to extract solution；
(6) semipreparative high performance liquid chromatography sub-argument purification system is used, the extract solution after above-mentioned degassing is eluted
Separation；Separation condition uses C18 fillers, 5 μm of filler particle size, 40 DEG C of system temperature, and flow velocity is 3ml/min, collects 7.5-8.5 point
The appearance component of clock；
Mobile phase is using the mixed solvent of methanol and the aqueous acetic acid of mass concentration 0.5%, and mass ratio is 40:60；
(7) the solution concentration after the appearance Fraction collection of 7.5-8.5 minutes is obtained into the cigarette jasmine flower essence
3。
Claims (2)
1. a kind of purification process of cigarette jasmine flower extract, its step includes：
(1) Jasmine is subjected to degreasing with the petroleum ether immersion 1-8h of 3-8 times of its weight, or the jasmine of refined jasmine oil was extracted in use
Jasmine residue；
(2) after extracting the Jasmine after degreasing in step (1) or Jasmine residue 1-3 times with alcohol reflux, filtering and concentrating is obtained
To Jasmine crude extract；
(3) acid is added into Jasmine crude extract to be made after flavonoid glycoside hydrolysis completely, and it is neutrality to add alkali regulation pH value, is refiltered
Remove precipitum and obtain extract solution；After the completion of, extract solution is adsorbed with nonpolar macroporous adsorption resin, successively with water, ethanol elution,
Obtained ethanol eluate is concentrated by evaporation, and obtains Jasmine extract solution after filtering；
(4) high performance liquid chromatography separation purification column is utilized, the Jasmine extract solution in step (3) is subjected to elution separation；It is described
Purification column uses C18 fillers, and 5 μm of filler particle size, the system temperature for purifying post separation is 20-40 DEG C；The mobile phase is quality
Than for 1:1-4 methanol and the aqueous acetic acid of mass concentration 0.5%；
(5) quercetin component is collected, is the cigarette jasmine flower extract after the product concentration of outflow.
2. the purification process of cigarette jasmine flower extract according to claim 1, it is characterised in that：In the step (4), carry
Take liquid to enter and ultrasonic degassing is first carried out before post.
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| RU2594239C1 (en) * | 2015-05-20 | 2016-08-10 | Олег Иванович Квасенков | Method for production of hookah smoking composition |
| CN105029681B (en) * | 2015-07-14 | 2017-10-31 | 中国烟草总公司郑州烟草研究院 | Natural perfume material refined liquid, tobacco juice suitable for tobacco juice for electronic smoke 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 |
| CN113951534B (en) * | 2021-11-05 | 2023-02-10 | 云南中烟工业有限责任公司 | Jasmine extract, preparation method and application thereof |
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