CN107974349A - 一种生物发酵当归油的制备方法及其应用 - Google Patents
一种生物发酵当归油的制备方法及其应用 Download PDFInfo
- Publication number
- CN107974349A CN107974349A CN201711225703.4A CN201711225703A CN107974349A CN 107974349 A CN107974349 A CN 107974349A CN 201711225703 A CN201711225703 A CN 201711225703A CN 107974349 A CN107974349 A CN 107974349A
- Authority
- CN
- China
- Prior art keywords
- angelica
- oil
- fermentation
- biofermentation
- cigarette
- 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.)
- Pending
Links
- 235000001287 Guettarda speciosa Nutrition 0.000 title claims abstract description 84
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 244000061520 Angelica archangelica Species 0.000 title 1
- 241000125175 Angelica Species 0.000 claims abstract description 83
- 239000003921 oil Substances 0.000 claims abstract description 69
- 238000000855 fermentation Methods 0.000 claims abstract description 44
- 230000004151 fermentation Effects 0.000 claims abstract description 44
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 39
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 38
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000000341 volatile oil Substances 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 239000003124 biologic agent Substances 0.000 claims abstract description 16
- 150000001875 compounds Chemical class 0.000 claims abstract description 13
- 238000001256 steam distillation Methods 0.000 claims abstract description 9
- 230000004087 circulation Effects 0.000 claims abstract description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 33
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 12
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 11
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 102000004190 Enzymes Human genes 0.000 claims description 9
- 108090000790 Enzymes Proteins 0.000 claims description 9
- 241000186660 Lactobacillus Species 0.000 claims description 7
- 229940039696 lactobacillus Drugs 0.000 claims description 7
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 239000000284 extract Substances 0.000 claims description 6
- 239000000706 filtrate Substances 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 230000002779 inactivation Effects 0.000 claims description 2
- 241000213006 Angelica dahurica Species 0.000 claims 4
- 244000061176 Nicotiana tabacum Species 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 241000382455 Angelica sinensis Species 0.000 abstract description 50
- 239000003205 fragrance Substances 0.000 abstract description 19
- 239000003814 drug Substances 0.000 abstract description 14
- 239000002304 perfume Substances 0.000 abstract description 12
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 11
- 239000003546 flue gas Substances 0.000 abstract description 11
- 239000007789 gas Substances 0.000 abstract description 7
- 230000007062 hydrolysis Effects 0.000 abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 7
- 238000013329 compounding Methods 0.000 abstract description 6
- 208000006673 asthma Diseases 0.000 abstract description 5
- 230000000146 antalgic effect Effects 0.000 abstract description 4
- 230000003110 anti-inflammatory effect Effects 0.000 abstract description 4
- 230000007794 irritation Effects 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007254 oxidation reaction Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 150000003254 radicals Chemical class 0.000 abstract description 3
- 230000000638 stimulation Effects 0.000 abstract 1
- 238000000034 method Methods 0.000 description 12
- 241000208125 Nicotiana Species 0.000 description 11
- 230000000694 effects Effects 0.000 description 11
- 229940088598 enzyme Drugs 0.000 description 8
- 239000000796 flavoring agent Substances 0.000 description 8
- 238000010790 dilution Methods 0.000 description 7
- 239000012895 dilution Substances 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 150000004676 glycans Chemical class 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 5
- 239000005017 polysaccharide Substances 0.000 description 5
- 230000002000 scavenging effect Effects 0.000 description 5
- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical group C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 description 4
- BGLUXFNVVSVEET-UHFFFAOYSA-N beta-angelica lactone Chemical compound CC1OC(=O)C=C1 BGLUXFNVVSVEET-UHFFFAOYSA-N 0.000 description 4
- 235000009508 confectionery Nutrition 0.000 description 4
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 235000013355 food flavoring agent Nutrition 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229920005610 lignin Polymers 0.000 description 4
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 230000001351 cycling effect Effects 0.000 description 3
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 241000193830 Bacillus <bacterium> Species 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- 239000004365 Protease Substances 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 230000017531 blood circulation Effects 0.000 description 2
- 210000004027 cell Anatomy 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- 210000000697 sensory organ Anatomy 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 238000002604 ultrasonography Methods 0.000 description 2
- 241000208173 Apiaceae Species 0.000 description 1
- 208000024172 Cardiovascular disease Diseases 0.000 description 1
- 108010059892 Cellulase Proteins 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 206010013935 Dysmenorrhoea Diseases 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
- 208000037093 Menstruation Disturbances Diseases 0.000 description 1
- 206010027339 Menstruation irregular Diseases 0.000 description 1
- 108090000526 Papain Proteins 0.000 description 1
- 108091005804 Peptidases Proteins 0.000 description 1
- 102100037486 Reverse transcriptase/ribonuclease H Human genes 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000003213 activating effect Effects 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 229940106157 cellulase Drugs 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 208000026106 cerebrovascular disease Diseases 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002279 cholagogic effect Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000000502 dialysis Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 230000003694 hair properties Effects 0.000 description 1
- 235000013402 health food Nutrition 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- 241000411851 herbal medicine Species 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 201000010260 leiomyoma Diseases 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 239000013642 negative control Substances 0.000 description 1
- 229940055729 papain Drugs 0.000 description 1
- 235000019834 papain Nutrition 0.000 description 1
- 230000035790 physiological processes and functions Effects 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- ULWHHBHJGPPBCO-UHFFFAOYSA-N propane-1,1-diol Chemical class CCC(O)O ULWHHBHJGPPBCO-UHFFFAOYSA-N 0.000 description 1
- 235000019419 proteases Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000005406 washing Methods 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
-
- 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
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Medicines Containing Plant Substances (AREA)
- Fats And Perfumes (AREA)
Abstract
本发明的目的是提供一种生物发酵当归油的制备方法及其应用,将当归根低温超微粉碎,加压破壁,加入复合生物制剂复合水解发酵,水蒸气蒸馏提取发酵当归挥发油A,抽滤,滤渣加入乙酸乙酯加热加压循环提取当归油,抽滤浓缩除溶剂后得到当归油B,两者复配得到生物发酵当归油,具有自然复合当归药香和清果香等天然气息,刺激性降低,香气品质提高,具有较强清除自由基抗氧化能力;在卷烟中应用,香气丰富自然,带有药香与清香、果香的发酵香气,与烟气协调,烟香清晰、具有抗炎镇痛平喘、增强喉部舒适性的作用,克服了当归特征药香气过于强烈、刺激较大、有杂气的缺陷。
Description
技术领域
本发明涉及烟用添加剂技术领域,具体涉及一种生物发酵当归油的制备方法及其应用。
背景技术
香精香料在中式卷烟香气和吃味特征的形成方面起到了关键作用。但就目前的生产实践而言,作为卷烟制造核心技术的香精香料的基础理论研究还较薄弱,尤其是对于卷烟企业,更多的是基于现有香精香料产品的调配和组合,表现为加香加料技术的针对性和可控性不高。目前香精香料产品在与卷烟原料、工艺、产品内在质量的有机结合方面还有较大欠缺,相应地体现在针对卷烟品牌量身定做的特色天然香原料的开发应用尤显不足。而且,在卷烟工业上广泛应用的烟用天然香料大多为初级加工产品,通常采用传统的提取方法简单加工获得。由此导致加香加料的效果不能较好满足卷烟设计要求。
当归(Radix AngelicaeSinensis),别名秦归、云归等。目前药材当归指伞形科植物当归的根。当归的成分相当复杂,大体上分为两部分:一部分为脂溶性物质(当归油),另一部分为水溶性物质(当归多糖类物质)。当归油具有补血活血、促进血液循环、缓解血管平滑肌痉挛、抗炎镇痛、平喘、保肝利胆等作用,可治疗月经不调、痛经、子宫肌瘤及哮喘治疗等病症,也被用于治疗心脑血管疾病,是目前市场上较为畅销的医药中间体和保健食品原料,同时当归油也还广泛应用于化妆品及香料工业。当归油中已鉴定出52种成份,其中最主要成份为藁本内酯,含量45~65%,是评价当归油质量的重要指标,值得重视的是藁本内酯长时间受热易引起异构化,失去药理作用。
目前对于中草药当归提取物及其在卷烟中应用的专利包括:(1)授权专利“一种食甲醇芽孢杆菌及其烟用当归浸膏制备方法和应用”(ZL201210113762.3),利用微生物食甲醇芽孢杆菌生物转化当归制备烟用当归浸膏,用于卷烟中与烟气协调、增加甜香、回甜感、减小刺激、杂气减少、透发性增强、烟气细腻柔和、顺畅、干燥程度降低、余味变好、改善吸味;(2)一种新型当归烟用香料及其制备方法(ZL200810197140.7),将当归破碎,加入乙醇溶液回流提取,浓缩为粗提取物,进行大孔吸附树脂吸附,将乙醇洗脱液浓缩为烟用香料,与烟香协调性好、无残留、能明显提调烟香,改善吃味;(3)一种当归三醋酸甘油酯提取物及其在卷烟中的应用(申请号201610156100.2),以晾晒干燥当归粉碎过筛后的当归粉末为原料,三醋酸甘油酯为提取剂,采用超声波、微波依次提取,再加热回流提取制备得到,喷洒到滤棒丝束上,制成卷烟滤棒,通过常规的卷烟接装程序制成含有当归有效成分滤棒的卷烟,使卷烟香气丰富性增加、提升甜润感、明显提升抽吸品质;(4)一种含有当归成分的雾化液及其制备方法(申请号201410855364.8),公开了一种含有当归成分的雾化液及其制备方法,雾化液由丙二醇、甘油、当归成分、蒸馏水组成,对女性吸烟者特别有效,并且具有补血活血、调经止痛、润肠通便的保健功效,能使使用者在逐渐戒除烟瘾的同时,吸收当归药用成分,改善生理机能,加强身体素质;(5)微波超声技术制备当归提取物的方法(申请号201510435421.1),公开一种微波超声技术制备当归提取物的方法,将当归清洗除杂,冷冻、干燥、粉碎处理,超声-微波提取器中进行提取过滤,对滤液低压浓缩,然后对滤渣进行二次提取、过滤;合并浓缩液及二次提取液,离心分离并浓缩;(6)当归多糖、提取纯化方法及其作为烟草保润剂的应用(ZL201410217669.6),将粉碎过的干燥当归用乙醚索氏提取后,残渣挥干再用沸水进行提取,浓缩、离心,取上清液醇沉静置,再次离心收集沉淀物,洗涤后用蒸馏水溶解,再加入1-2‰的木瓜蛋白酶于50±5℃水浴中放置2-4h,采用Sevage法脱除蛋白,活性炭脱色后减压浓缩、冷却、流水透析、再次醇沉静置,干燥得粗多糖,对卷烟具有很好的物理和感官保润作用,并且可以降低卷烟的刺激性和杂气,提高卷烟烟气的圆润感和舒适性。
还未见将当归根低温超微粉碎,加压破壁,加入复合生物制剂复合水解发酵,水蒸气蒸馏提取当归挥发油A,抽滤得到的滤渣加入乙酸乙酯加热加压循环提取当归油,抽滤浓缩除溶剂后得到当归油B,两者复配得到生物发酵当归油卷烟中应用的报道。
发明内容
本发明的目的是提供一种生物发酵当归油的制备方法及其应用,将当归根低温超微粉碎,加压破壁,加入复合生物制剂复合水解发酵,水蒸气蒸馏提取当归挥发油A,抽滤,滤渣加入乙酸乙酯加热加压循环提取当归油,抽滤浓缩除溶剂后得到当归油B,两者复配得到生物发酵当归油,具有自然复合当归药香和清果香等天然气息,刺激性降低,香气品质提高,具有较强清除自由基抗氧化能力;在卷烟中应用,香气丰富自然,带有药香与清香、果香的发酵香气,与烟气协调,烟香清晰、具有抗炎镇痛平喘、增强喉部舒适性的作用。克服了当归特征药香气过于强烈、刺激较大、有杂气的缺陷。
本发明通过以下技术方案实现:
一种生物发酵当归油的制备方法,包括如下步骤:
(1)低温超微粉碎和加压破壁:将当归根放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度-4~4℃,目数为200~280目,将当归超微粉末和水按质量比1:10~40加入加压提取罐中,搅拌均匀,加压5MPa~30MPa、5~20min,促进细胞破壁;
(2)水解发酵:加入占归超微粉质量0.3~1.2%的乙酸和占归超微粉质量0.01~0.3%的复合生物制剂混合搅拌均匀,加热至30~45℃,温育发酵4h~72h,所述复合生物制剂包括菊糖芽孢乳杆菌、β-葡萄糖苷酶、木质素酶,均为食品级,β-葡萄糖苷酶和木质素酶的酶活分别为100~5000u/g、2万-10万u/g,三者配比按质量比为1:0.5~2:0.5~2;
(3)水蒸气蒸馏制备发酵当归挥发油A:将加压提取罐温度提升至98±2℃,水蒸气蒸馏3-6h,生物制剂灭活,得到发酵当归挥发油A,常温避光保存;
(4)制备当归油B:将加压提取罐的发酵提取液减压抽滤,滤渣常温风干,加入3~20倍质量的乙酸乙酯,50℃~80℃、按照5MPa~30MPa程序加压循环萃取3h~6h,抽滤取滤液,所得为当归油B;
(5)复配:将步骤3)和4)制备的发酵当归挥发油A和当归油B按一定比例复配得到生物发酵当归油,常温避光储存待用。
进一步的,所述步骤5)中发酵当归挥发油A和当归油B复配比例为:由75%乙醇溶液稀释当归挥发油A至0.1~1%,当归油B至1~10%,然后按质量比1:1混配。
进一步的,所述的乙酸、乙酸乙酯为食品级。
进一步的,本发明还提供一种上述方法制备的生物发酵当归油复配稀释液在卷烟中的应用,添加量为烟丝质量的1~5ppm。
本发明的有益效果是:
(1)-4~4℃低温下超微粉碎当归根至200~280目,然后加压5MPa~30MPa,可使当归根原料在较低温度下保持致香成分等生物活性成分活力的同时,提高细胞破壁程度,破坏细胞壁大分子物质,有利于后期的复合生物制剂水解发酵,也有利于释放细胞壁内的化学物质;
(2)加入乙酸调节pH值为弱酸性,加大多糖键易断裂程度,弱酸、复合生物制剂(菊糖芽孢乳杆菌、β-葡萄糖苷酶、木质素酶)联合水解当归超微粉末多糖等大分子物质,使之发生转化、分解、氧化等反应,将糖类发酵产乳酸,将木质素分解为葡萄糖,将葡萄糖苷键断裂产生风味物质或香味前体物,且活性菊糖芽孢乳杆菌中的蛋白酶、纤维素酶等活性酶体系,还能分解蛋白质、纤维素等,在这些协同增效作用下,提高了多糖、蛋白质、纤维素、木质素等分解效率,使产物中大分子刺激性成分减少,致香成分种类和含量增多,香气量提高,且富含乳酸,中和烟气碱性,烟香柔和醇厚;
(3)制备发酵当归挥发油A后,其滤渣中仍含有丰富的藁本内酯等当归油脂成分,遂采用乙酸乙酯较低温度下加压循环提取当归渣中的当归油致香成分与有效成分,保留其藁本内酯药理活性,得到当归油B,然后与发酵当归挥发油A复配后,香气丰富自然,为药香与清香、果香的发酵香气,且具有较强的清除自由基抗氧化能力;在卷烟中应用,能与烟气协调,具有抗炎镇痛平喘、增强喉部舒适性的作用。
该方法所制备的天然香料产物香气丰富自然,致香成分纯度高,杂质少,致香作用效果好;所用原料来源广泛,绿色环保,工艺条件简单易操作,成本低,具有产业化前景。
具体实施方式
以下结合具体实施例对本发明进行详细地说明。
实施例1
一种生物发酵当归油的制备方法,包括如下步骤:
(1)低温超微粉碎和加压破壁:将当归根放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度-4℃,目数为200目,当归超微粉末和水按质量比1:15加入到加压提取罐中,搅拌均匀,加压5Mpa20min;
(2)水解发酵:加入乙酸(按当归超微粉质量的0.3%),复合生物制剂(按当归超微粉末质量的0.27%,菊糖芽孢乳杆菌粉、β-葡萄糖苷酶粉、木质素酶粉各占0.15%、0.06%、0.06%,食品级,β-葡萄糖苷酶、木质素酶的酶活分别为2000u/g、10万u/g)混合搅拌均匀,加热至35℃,温育发酵12h;
(3)水蒸气蒸馏制备发酵当归挥发油A:将加压提取罐温度提升至98+2℃,水蒸气蒸馏3h,制备发酵当归挥发油A,常温避光保存;
(4)当归油B的制备:将加压提取罐的发酵提取液减压抽滤,滤渣常温风干,加入5倍质量的乙酸乙酯,55℃、程序加压(20MPa2h,降至10MPa 1h)循环萃取3h,抽滤取滤液,所得为当归油B;
(5)复配:将步骤3)和4)的发酵当归挥发油A和当归油B分别由75%乙醇水溶液稀释至0.1%和5%,再按质量比1:1混配,得到生物发酵当归油稀释液,常温避光储存待用。
所述的乙酸、乙酸乙酯为食品级。
本发明制备的生物发酵当归油复配稀释液在卷烟中应用,添加量为烟丝质量的1ppm,与烟气协调,香气更丰富,带有淡药香与清果香的发酵气息,具有增强喉部舒适性的作用。
实施例2
一种生物发酵当归油的制备方法,包括如下步骤:
(1)低温超微粉碎和加压破壁:将当归根放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度0℃,目数为250目,粉末和水按质量比1:20,加入到加压提取罐中,搅拌均匀,加压10MPa 15min;
(2)水解发酵:加入乙酸(按当归超微粉质量的0.6%),复合生物制剂(按当归超微粉末质量的0.24%,菊糖芽孢乳杆菌粉、β-葡萄糖苷酶粉、木质素酶粉各占0.08%、0.08%、0.08%,食品级,β-葡萄糖苷酶、木质素酶的酶活分别为1000u/g、15万u/g)混合搅拌均匀,加热至40℃,温育发酵36h;
(3)水蒸气蒸馏制备发酵当归挥发油A:将加压提取罐温度提升至98+2℃,水蒸气蒸馏4h,制备发酵当归挥发油A,常温避光保存;
(4)当归油B的制备:将加压提取罐的发酵提取液减压抽滤,滤渣常温风干,加入8倍质量的乙酸乙酯,60℃、程序加压(30MPa、20MPa、10MPa各1h)循环萃取3h,抽滤取滤液,所得为当归油B;
(5)复配:将步骤3)和4)的发酵当归挥发油A和当归油B分别由75%乙醇水溶液稀释至0.5%和1%,再按1:1混配,得到生物发酵当归油稀释液,常温避光储存待用。
所述的乙酸、乙酸乙酯为食品级。
本发明制备的生物发酵当归油复配稀释液在卷烟中应用,添加量为烟丝质量的2ppm,与烟气协调,香气丰富,带有药香与清果香气,余味干净,口感改善。
实施例3
一种生物发酵当归油的制备方法,包括如下步骤:
(1)低温超微粉碎和加压破壁:将当归根放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度2℃,目数为280目,粉末和水按质量比1:30,加入到加压提取罐中,搅拌均匀,加压20MPa 10min;
(2)水解发酵:加入乙酸(按当归超微粉质量的1.0%),复合生物制剂(按当归超微粉末质量的0.18%,菊糖芽孢乳杆菌粉、β-葡萄糖苷酶粉、木质素酶粉各占0.06%、0.06%、0.06%,食品级,β-葡萄糖苷酶、木质素酶的酶活分别为5000u/g、20万u/g)混合搅拌均匀,加热至42℃,温育发酵60h;
(3)水蒸气蒸馏制备发酵当归挥发油A:将加压提取罐温度提升至98+2℃,水蒸气蒸馏5h,制备发酵当归挥发油A,常温避光保存;
(4)当归油B的制备:将加压提取罐的发酵提取液减压抽滤,滤渣常温风干,加入15倍质量的乙酸乙酯,60℃、程序加压(25MPa2.5h,降至10MPa1.5h)循环萃取5h,抽滤取滤液,所得为当归油B;
(5)复配:将步骤3)和4)的发酵当归挥发油A和当归油B分别由75%乙醇水溶液稀释至0.8%和10%,再按1:1混配,得到生物发酵当归油稀释液,常温避光储存待用。
所述的乙酸、乙酸乙酯为食品级。
本发明制备的生物发酵当归油复配稀释液在卷烟中应用,添加量为烟丝质量的3ppm,与烟气协调,香气丰富,带有药香与清果香气,烟气浓度增加,口感舒适。
试验例1.提取效率
称取1Kg发酵当归挥发油A和当归油B浓缩除溶剂产物及其对照,称重,计算提取率,如表1。
表1.发酵及对照当归油的提取率
发酵当归挥发油A | 对照1 | 当归油B | 对照2 | |
质量 | 5.8g | 3.2g | 5.4g | 2.4g |
提取率 | 0.58% | 0.32% | 0.54% | 0.24% |
由表1可知,经超微粉碎、加压破壁联合生物制剂复合水解发酵处理的发酵当归挥发油A、当归油B,对比经普通粉碎、未经加压破壁及生物发酵预处理的当归挥发油对照1及当归油对照2,提取率明显提高,分别提高了81.25%、1.25倍。
试验例2.应用的感官效果评价
将实施例1-3制备及复配的生物发酵当归油在卷烟配方烟丝中加香,进行感官评价,对照组为施加未经低温超微粉碎、加压破壁及生物制剂复合水解发酵的相应复配当归油对照,在卷烟配方烟丝中加香,结果见表2。
表2.提高香气品质的罗马春黄菊油在配方烟丝中的感官评价
表2表明:本发明方法提高了当归油的香气品质,杂质减少、纯度变高、刺激性降低,发酵香气复合自然;在卷烟配方烟丝中应用,与烟气协调,香气更丰富,带有淡药香与清果香的发酵气息,具有增强喉部舒适性的作用,克服了当归特征药香气过于明显、具有刺激性和带有杂气、余味不净的缺陷。
试验例3.当归内酯对DPPH·的清除作用
取2.5mL 6.5×10-5mol·L-1DPPH·的DMSO溶液,与0.5mL不同浓度的当归油B或其对照(未经超微粉碎、加压破壁、生物制剂复合水解发酵的当归油对照)混合均匀,室温下静置30min,于517nm测定吸光度(Ai);以DMSO代替药品,测定阴性对照组吸光度(A0)。清除率=(1-Ai/A0)×100%。结果显示:当归内酯对DPPH·具很强的清除作用,且随当归内酯浓度的增加,其清除能力增强,且当归油B的清除能力明显强于其阳性对照(表3)。
表3当归内酯对DPPH·的清除作用
Claims (4)
1.一种生物发酵当归油的制备方法,其特征在于包括如下步骤:
(1)低温超微粉碎和加压破壁:将当归根放入液氮冷冻超微粉碎机中粉碎成超微粉末,温度-4~4℃,目数为200~280目,将当归超微粉末和水按质量比1:10~40加入加压提取罐中,搅拌均匀,加压5MPa~30MPa、5~20min,促进细胞破壁;
(2)水解发酵:加入占归超微粉质量0.3~1.2%的乙酸和占归超微粉质量0.01~0.3%的复合生物制剂混合搅拌均匀,加热至30~45℃,温育发酵4h~72h,所述复合生物制剂包括菊糖芽孢乳杆菌、β-葡萄糖苷酶、木质素酶,均为食品级,β-葡萄糖苷酶和木质素酶的酶活分别为100~5000u/g、2万-10万u/g,三者配比按质量比为1:0.5~2:0.5~2;
(3)水蒸气蒸馏制备发酵当归挥发油A:将加压提取罐温度提升至98±2℃,水蒸气蒸馏3-6h,生物制剂灭活,得到发酵当归挥发油A,常温避光保存;
(4)制备当归油B:将加压提取罐的发酵提取液减压抽滤,滤渣常温风干,加入3~20倍质量的乙酸乙酯,50℃~80℃、按照5MPa~30MPa程序加压循环萃取3h~6h,抽滤取滤液,所得为当归油B;
(5)复配:将步骤3)和4)制备的发酵当归挥发油A和当归油B按一定比例复配得到生物发酵当归油,常温避光储存待用。
2.如权利要求1所述的生物发酵当归油的制备方法,其特征在于:所述步骤5)中发酵当归挥发油A和当归油B复配比例为:由75%乙醇溶液稀释当归挥发油A至0.1~1%,当归油B至1~10%,然后按质量比1:1混配。
3.如权利要求1所述的生物发酵当归油的制备方法,其特征在于:所述的乙酸、乙酸乙酯为食品级。
4.一种如权利要求1-3中任一项所述制备的生物发酵当归油在卷烟中的应用,添加量为烟丝质量的1~5ppm。
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711225703.4A CN107974349A (zh) | 2017-11-29 | 2017-11-29 | 一种生物发酵当归油的制备方法及其应用 |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201711225703.4A CN107974349A (zh) | 2017-11-29 | 2017-11-29 | 一种生物发酵当归油的制备方法及其应用 |
Publications (1)
Publication Number | Publication Date |
---|---|
CN107974349A true CN107974349A (zh) | 2018-05-01 |
Family
ID=62008525
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201711225703.4A Pending CN107974349A (zh) | 2017-11-29 | 2017-11-29 | 一种生物发酵当归油的制备方法及其应用 |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN107974349A (zh) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109536283A (zh) * | 2018-11-09 | 2019-03-29 | 湖北中烟工业有限责任公司 | 一种提高品质的苏合香油的制备方法及其应用 |
CN111154548A (zh) * | 2020-01-13 | 2020-05-15 | 合肥学院 | 一种肉桂精油的提取方法 |
CN112273709A (zh) * | 2020-10-23 | 2021-01-29 | 湖北中烟工业有限责任公司 | 一种用于烟草加香的石窑当归提取物的制备方法 |
IT202000019075A1 (it) * | 2020-08-04 | 2022-02-04 | Andrea Darecchio | Metodo termofisico, rapido e ad elevata efficienza, e relativo apparato, per ottenere prodotti alimentari, bevande, prodotti dietetici, erboristici, medicinali, farmaceutici, cosmetici, detergenti, profumi, e simili, o loro ingredienti, crudi oppure cotti, cucinati, pastorizzati o sterilizzati, pronti per il consumo oppure a breve, media o lunga conservazione a temperatura ambiente oppure di refrigeratore o di surgelatore, aventi la fragranza e i pigmenti di prodotti aromatici naturali freschi o trasformati |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5099862A (en) * | 1990-04-05 | 1992-03-31 | R. J. Reynolds Tobacco Company | Tobacco extraction process |
CN1608639A (zh) * | 2003-10-23 | 2005-04-27 | 苏少宁 | 当归油滴丸及其制备方法 |
CN102851229A (zh) * | 2012-04-18 | 2013-01-02 | 湖北中烟工业有限责任公司 | 一种食甲醇芽孢杆菌及其烟用当归浸膏制备方法和应用 |
CN105861563A (zh) * | 2016-06-03 | 2016-08-17 | 湖北中烟工业有限责任公司 | 一种综合技术制备广陵香复合香料的方法及其应用 |
CN105998112A (zh) * | 2016-06-27 | 2016-10-12 | 四川省中医药科学院 | 由废弃药渣制备植物药材挥发油的方法 |
CN107232638A (zh) * | 2017-07-05 | 2017-10-10 | 湖北中烟工业有限责任公司 | 一种葡萄干提取物的提质纯化方法及其应用 |
-
2017
- 2017-11-29 CN CN201711225703.4A patent/CN107974349A/zh active Pending
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5099862A (en) * | 1990-04-05 | 1992-03-31 | R. J. Reynolds Tobacco Company | Tobacco extraction process |
CN1608639A (zh) * | 2003-10-23 | 2005-04-27 | 苏少宁 | 当归油滴丸及其制备方法 |
CN102851229A (zh) * | 2012-04-18 | 2013-01-02 | 湖北中烟工业有限责任公司 | 一种食甲醇芽孢杆菌及其烟用当归浸膏制备方法和应用 |
CN105861563A (zh) * | 2016-06-03 | 2016-08-17 | 湖北中烟工业有限责任公司 | 一种综合技术制备广陵香复合香料的方法及其应用 |
CN105998112A (zh) * | 2016-06-27 | 2016-10-12 | 四川省中医药科学院 | 由废弃药渣制备植物药材挥发油的方法 |
CN107232638A (zh) * | 2017-07-05 | 2017-10-10 | 湖北中烟工业有限责任公司 | 一种葡萄干提取物的提质纯化方法及其应用 |
Non-Patent Citations (2)
Title |
---|
张晓鸣: "《食品风味化学》", 31 March 2009, 中国轻工业出版社 * |
王沛: "《中药制药工程原理与设备》", 31 August 2016, 北京:中国中医药出版社 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109536283A (zh) * | 2018-11-09 | 2019-03-29 | 湖北中烟工业有限责任公司 | 一种提高品质的苏合香油的制备方法及其应用 |
CN111154548A (zh) * | 2020-01-13 | 2020-05-15 | 合肥学院 | 一种肉桂精油的提取方法 |
IT202000019075A1 (it) * | 2020-08-04 | 2022-02-04 | Andrea Darecchio | Metodo termofisico, rapido e ad elevata efficienza, e relativo apparato, per ottenere prodotti alimentari, bevande, prodotti dietetici, erboristici, medicinali, farmaceutici, cosmetici, detergenti, profumi, e simili, o loro ingredienti, crudi oppure cotti, cucinati, pastorizzati o sterilizzati, pronti per il consumo oppure a breve, media o lunga conservazione a temperatura ambiente oppure di refrigeratore o di surgelatore, aventi la fragranza e i pigmenti di prodotti aromatici naturali freschi o trasformati |
CN112273709A (zh) * | 2020-10-23 | 2021-01-29 | 湖北中烟工业有限责任公司 | 一种用于烟草加香的石窑当归提取物的制备方法 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN106418663B (zh) | 一种玫瑰花净油的生物化学联合制备方法及其应用 | |
CN107974349A (zh) | 一种生物发酵当归油的制备方法及其应用 | |
CN101928729B (zh) | 一种红枣发酵提取物和制备方法及其在卷烟中的应用 | |
CN104957298A (zh) | 养生茉莉花茶 | |
CN103690469B (zh) | 一种含有银杏酵素的护肤液及其制备方法和应用 | |
CN106912982A (zh) | 一种电子烟烟油及其制备方法 | |
CN106136303B (zh) | 一种栀子烟用提取物的制备方法及其应用 | |
CN101942362B (zh) | 一种中草药水果混合香基及其制备方法与应用 | |
CN101666062A (zh) | 一种添加中草药添加剂的水松纸及其制备方法 | |
CN106723301A (zh) | 电子烟烟液 | |
CN105368688A (zh) | 一种葡萄醋 | |
KR20120133799A (ko) | 기능성 비누 및 이의 제조방법 | |
CN106190558A (zh) | 一种烟用发酵型五味子香料的制备方法及其应用 | |
CN101569438B (zh) | 制备桑椹烟用香料的方法 | |
CN102031194A (zh) | 银杏叶挥发油提取方法及利用该挥发油对卷烟加香的方法 | |
CN106360213A (zh) | 一种黄精植物饮料及其制备方法 | |
CN109156895A (zh) | 一种降低卷烟抽吸干燥感和刺激性的滤棒添加剂、其制备方法及用途 | |
CN107043788A (zh) | 一种基于生物产香制备无花果香料的方法及其应用 | |
CN108771757A (zh) | 一种保健足贴组合物及保健足贴 | |
CN107997228A (zh) | 一种带烘烤香的当归提取物的制备方法及其应用 | |
CN108949347A (zh) | 增加加热不燃烧新型卷烟烟气湿润感的香精及其制备方法和应用 | |
CN106753790A (zh) | 香气均匀、稳定的烟用香料及其制备方法 | |
CN104694254B (zh) | 红参提取物及其制备方法和应用 | |
CN109536283A (zh) | 一种提高品质的苏合香油的制备方法及其应用 | |
CN110122921A (zh) | 一种红茶爆珠的制备方法 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180501 |