CN108451008A - A kind of biofermentation prepares the method and its application of lavender absolute oil - Google Patents
A kind of biofermentation prepares the method and its application of lavender absolute oil Download PDFInfo
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- CN108451008A CN108451008A CN201810201161.5A CN201810201161A CN108451008A CN 108451008 A CN108451008 A CN 108451008A CN 201810201161 A CN201810201161 A CN 201810201161A CN 108451008 A CN108451008 A CN 108451008A
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- lavender
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- absolute oil
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- 244000178870 Lavandula angustifolia Species 0.000 title claims abstract description 114
- 235000010663 Lavandula angustifolia Nutrition 0.000 title claims abstract description 113
- 239000001102 lavandula vera Substances 0.000 title claims abstract description 112
- 235000018219 lavender Nutrition 0.000 title claims abstract description 112
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000000855 fermentation Methods 0.000 claims abstract description 35
- 230000004151 fermentation Effects 0.000 claims abstract description 35
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000605 extraction Methods 0.000 claims abstract description 27
- 235000019441 ethanol Nutrition 0.000 claims abstract description 24
- 239000003124 biologic agent Substances 0.000 claims abstract description 20
- 239000002131 composite material Substances 0.000 claims abstract description 17
- 238000005119 centrifugation Methods 0.000 claims abstract description 12
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000009288 screen filtration Methods 0.000 claims abstract description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 33
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 33
- 239000000463 material Substances 0.000 claims description 16
- 241000208125 Nicotiana Species 0.000 claims description 15
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 15
- 241000218588 Lactobacillus rhamnosus Species 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 12
- 235000006408 oxalic acid Nutrition 0.000 claims description 11
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 9
- 108090000790 Enzymes Proteins 0.000 claims description 9
- 102000004190 Enzymes Human genes 0.000 claims description 9
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 9
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 9
- 235000015165 citric acid Nutrition 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 9
- 229940088598 enzyme Drugs 0.000 claims description 9
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 9
- 239000011976 maleic acid Substances 0.000 claims description 9
- 239000001630 malic acid Substances 0.000 claims description 9
- 235000011090 malic acid Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 7
- 108010059892 Cellulase Proteins 0.000 claims description 6
- 108010029541 Laccase Proteins 0.000 claims description 6
- 239000000654 additive Substances 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- 108010047754 beta-Glucosidase Proteins 0.000 claims description 6
- 102000006995 beta-Glucosidase Human genes 0.000 claims description 6
- 229940106157 cellulase Drugs 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 238000000874 microwave-assisted extraction Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 abstract description 41
- 239000003205 fragrance Substances 0.000 abstract description 21
- 239000002304 perfume Substances 0.000 abstract description 8
- 244000299461 Theobroma cacao Species 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 7
- 230000007794 irritation Effects 0.000 abstract description 7
- 235000019219 chocolate Nutrition 0.000 abstract description 6
- 239000012535 impurity Substances 0.000 abstract description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 abstract description 5
- 241000628997 Flos Species 0.000 abstract description 5
- 244000272264 Saussurea lappa Species 0.000 abstract description 5
- 235000006784 Saussurea lappa Nutrition 0.000 abstract description 5
- 235000013399 edible fruits Nutrition 0.000 abstract description 5
- 239000003546 flue gas Substances 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 4
- 239000000171 lavandula angustifolia l. flower oil Substances 0.000 abstract description 4
- 235000019658 bitter taste Nutrition 0.000 abstract description 3
- 235000009508 confectionery Nutrition 0.000 abstract description 3
- 239000007789 gas Substances 0.000 abstract description 2
- 238000011534 incubation Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 description 10
- 238000002360 preparation method Methods 0.000 description 10
- 239000000306 component Substances 0.000 description 5
- 239000000796 flavoring agent Substances 0.000 description 5
- 235000019634 flavors Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- 239000000945 filler Substances 0.000 description 4
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000005520 cutting process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000686 essence Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- BYGQBDHUGHBGMD-UHFFFAOYSA-N 2-methylbutanal Chemical compound CCC(C)C=O BYGQBDHUGHBGMD-UHFFFAOYSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 150000001336 alkenes Chemical class 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 150000004676 glycans Chemical class 0.000 description 2
- 238000001785 headspace extraction Methods 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- -1 nonyl ester Chemical class 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- NDTYTMIUWGWIMO-UHFFFAOYSA-N perillyl alcohol Chemical compound CC(=C)C1CCC(CO)=CC1 NDTYTMIUWGWIMO-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920001282 polysaccharide Polymers 0.000 description 2
- 239000005017 polysaccharide Substances 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
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- 239000000779 smoke Substances 0.000 description 2
- 230000000391 smoking effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000010792 warming Methods 0.000 description 2
- 239000001893 (2R)-2-methylbutanal Substances 0.000 description 1
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000196324 Embryophyta Species 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
- 241001579180 Matthiola longipetala Species 0.000 description 1
- 241000337007 Oceania Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 241000220324 Pyrus Species 0.000 description 1
- 235000009470 Theobroma cacao Nutrition 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000001857 anti-mycotic effect Effects 0.000 description 1
- 239000002543 antimycotic Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000015173 baked goods and baking mixes Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000011285 coke tar Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000000147 hypnotic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- CAWHJQAVHZEVTJ-UHFFFAOYSA-N methylpyrazine Chemical class CC1=CN=CC=N1 CAWHJQAVHZEVTJ-UHFFFAOYSA-N 0.000 description 1
- DUNCVNHORHNONW-UHFFFAOYSA-N myrcenol Chemical compound CC(C)(O)CCCC(=C)C=C DUNCVNHORHNONW-UHFFFAOYSA-N 0.000 description 1
- 229930008383 myrcenol Natural products 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 235000014571 nuts Nutrition 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 235000019645 odor Nutrition 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 235000021017 pears Nutrition 0.000 description 1
- 239000005426 pharmaceutical component Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 230000001766 physiological effect Effects 0.000 description 1
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 210000003296 saliva Anatomy 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/28—Treatment of tobacco products or tobacco substitutes by chemical substances
- A24B15/30—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances
- A24B15/302—Treatment of tobacco products or tobacco substitutes by chemical substances by organic substances by natural substances obtained from animals or plants
- A24B15/303—Plant extracts other than tobacco
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Fats And Perfumes (AREA)
Abstract
The object of the present invention is to provide the method and its application that a kind of biofermentation prepares lavender absolute oil, a certain proportion of water is added in lavender dried flower fringe, Microwave Pretreatment is carried out, sour water solution, composite biological agent incubation fermentation, then alcohol reflux extraction is then added, screen filtration, lavender fermentation extraction filtrate is obtained, after reduced pressure, absolute ethyl alcohol precipitation is stood overnight, centrifugation removal precipitation, obtains lavender absolute oil prepared by biofermentation of the present invention.The present invention also provides the biofermentation prepare lavender oil in cigarette perfumed applications, coordinate very much with flue gas, cigarette perfume clear and natural, fragrance is naturally abundant, in addition to fragrance specific to fresh lavandulae flos and root of Aucklandia lappa Decne note, also carrying compound baking, chocolate, fruit, fragrant and sweet gas etc., compared with the control, irritation reduces, and impurity is reduced, not bitter.Overcome that the lavender absolute oil characteristic perfume prepared without biofermentation is excessively single, strong, irritation is larger, pleasant impression carries the defect of bitter taste.
Description
Technical field
The present invention relates to cigarette additive technical fields, and in particular to a kind of method that biofermentation prepares lavender absolute oil
And its application.
Background technology
Currently, as smoking and the problem of health increasingly attract attention, the harmful components in cigarette smoke are reduced, are developed
Low-coke tar cigarette has become the direction of tobacco industry development.It solves cigarette low tar and holding meets smoking property of cigarette availability aspect
Between contradiction, flavoring and casing technology is an effective approach, and one of core technology of tobacco enterprise is exactly individual style
Essence spice for cigarette formula.Wherein natural tobacco aromaticss are since its natural sex receives an acclaim, but preparation method, process are still
The defects of that there are recovery rates is low, production cost is high, purity is relatively low, impurity is more, irritation is larger, characteristic perfume covers cigarette perfume.
Lavender (Lavandulaangustifolia Mill.) belongs to Labiatae lavender category, originates in Mediterranean edge
Bank, throughout Europe and Oceania archipelago, after planted extensively in Britain and Yugoslavia, by Xinjiang Yili pears 10 years essences of number
The heart is cultivated, and in day, at the foot of the hill Yilihe River side forms scale to lavender, and the Xinjiang Yili of China Kazak autonomous prefecture on Mountain Ranges of Tian Shan Mountains innerland is
The main base of Chinese lavender plantation processing, is the maximum production of flavor base in Asia.Lavender be it is a kind of rare and
Important natural perfume plant, fragrance faint scent are respectful refreshing, strong pleasant.It is certain that modern pharmacology research shows that lavender has
Physiological activity, have the effects that calmness, sterilization, antimycotic, blood pressure lowering, hypnosis.
Invention content
The object of the present invention is to provide the method and its application that a kind of biofermentation prepares lavender absolute oil, and lavender is done
A certain proportion of water is added in flower spike, carries out Microwave Pretreatment, sour water solution is then added, composite biological agent incubates fermentation, then second
Alcohol reflux extracts, screen filtration, obtains lavender fermentation extraction filtrate, and after reduced pressure, absolute ethyl alcohol precipitation is stood overnight,
Centrifugation removal precipitation, obtains lavender absolute oil prepared by biofermentation of the present invention.It is prepared the present invention also provides the biofermentation
Lavender oil perfumed applications in cigarette are coordinated, cigarette perfume clear and natural very much with flue gas, and fragrance is naturally abundant, new in addition to having
Fragrance and root of Aucklandia lappa Decne note specific to fresh lavandulae flos also carry compound baking, chocolate, fruit, fragrant and sweet gas etc., and to taking a picture
Than irritation reduces, and impurity is reduced, not bitter.Overcome the lavender absolute oil characteristic perfume prepared without biofermentation excessively
It is single, strong, irritation is larger, pleasant impression carry bitter taste defect.
The invention is realized by the following technical scheme：
A kind of biofermentation prepares the preparation method of lavender absolute oil, includes the following steps：
(1) low temperature ultrasonic pre-processes：By lavender dried flower fringe and water in mass ratio 1:10~20 are uniformly mixed, and pour into microwave
It is pre-processed in abstraction instrument, obtains lavender flower spike microwave abstracting mixed material；
(2) fermentation is incubated：The lavender flower spike microwave abstracting mixed material that step (1) obtains is poured into fermentation extractor
In, one or more of malic acid, oxalic acid, citric acid, maleic acid is added, composite biological agent is then added and stirs evenly,
35~55 DEG C are heated to, fermentation 1d~4d is incubated；
The composite biological agent is beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus
(L.rhamnosus) mixing is food-grade, and enzyme activity is 500~50000u/g, is 1 in mass ratio between biological agent:
0.5~2:0.5~2:0.5~2, the composite biological agent accounts for the 0.1~0.3% of lavender dried flower fringe mass ratio；
(3) refluxing extraction：The ethyl alcohol of 10~50 times of lavender dried flower fringe quality is added in the extractor that ferments, adjusts temperature
Be 60~90 DEG C, refluxing extraction 1~3 time, screen filtration, merging filtrate, obtain lavender fermentation extracting solution, be concentrated under reduced pressure into phase
The lavender fermentation extraction medicinal extract for being 1.20~1.32 to density；
(4) alcohol precipitation purifies：The lavender fermentation extraction medicinal extract that step (3) is obtained, is added 3~6 times of quality absolute ethyl alcohols,
0~4 DEG C stands overnight, and high-speed low temperature centrifugation stays supernatant, obtains the biofermentation lavender absolute oil of the present invention.
Further, the Microwave Extraction Apparatus operating condition described in step (1) is 0~10 DEG C of temperature, microwave frequency：
2450MHz, microwave power are 0~1000W of power, 3~15min of time.
Further, the malic acid, oxalic acid, citric acid, maleic acid are food-grade, account for lavender flower spike material quality
0.1~0.5%, between in mass ratio be 1:0.5~2:0.5~2:0.5~2.
Further, the ethyl alcohol in step (3) is food-grade.
Further, the high-speed low temperature centrifugation described in step (4), operating condition are 12000~30000rpm, temperature 0~5
℃。
The present invention also provides biofermentations prepared by a kind of above method to prepare lavender absolute oil.
The present invention also provides biofermentations prepared by a kind of above method to prepare lavender absolute oil in traditional cigarette or novel
The perfumed applications in the cigarette composition pipe tobacco that do not burn are heated, additive amount accounts for 0.01~0.1ppm of tobacco quality.
The beneficial effects of the invention are as follows：
(1) inside and outside to heat simultaneously by Microwave Pretreatment lavender flower spike aqueous solution, thus homogeneous heating, the thermal efficiency compared with
Height, the temperature gradient not being heated at high temperature, and heating speed is fast, the heated time of material is short, thus is conducive to lavender temperature-sensitive
Property flavor matter extraction, improve extraction efficiency, it is propagated in medium can cause the intermolecular severe friction of medium and heat
It dissipates, takes low temperature ultrasonic, lavender bioactive ingredients can be made not by high temperature；
(2) one or more of malic acid, oxalic acid, citric acid, maleic acid is added, plays and adjusts pH value to acidity, promote
The fracture of lavender flower spike plant polyose key, the acid-hydrolyzed effect of polysaccharide, while enzyme activity higher under acid condition under into acid condition,
Conducive to the later stage complex enzyme formulation to the bioconversion of lavender, and these organic acids play the work of soft flue gas in cigarette
With；
(3) complex enzyme formulation (beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus are used
(L.rhamnosus)) fermentation lavender flower spike, by the macromolecular substances in lavender flower spike such as cellulose, protein, Polyphenols
Deng decomposing, converting, being oxidized to the small-molecule substances such as glucose, amino acid, aroma component and other flavor precursors, improve cause it is fragrant
Constituents extraction rate generates more flavor substances and its precursor substance；In low temperature ultrasonic, organic acid, complex enzyme formulation bioconversion
The potent effect of collaboration under, keep the holdings such as lavender aroma component, anti-oxidant and pharmaceutical component more intact；
(4) high-speed low temperature centrifugation technique is combined, low temperature, rapidly the biofermentation lavender of the purifies and separates present invention is net
Oil removes the macromoleculars such as remaining protein, polysaccharide in extractive from fermentative and is unfavorable for inhaling the substance of taste, retain natural scents at
Point.
The method of the present invention improves the flavouring essence quality of lavender absolute oil, and fragrance is more rich naturally, biofermentation system of the present invention
Standby lavender oil flavoring in cigarette is coordinated, cigarette perfume clear and natural very much with flue gas, and fragrance is naturally abundant, new in addition to having
Fragrance and root of Aucklandia lappa Decne note specific to fresh lavandulae flos also carry compound baking, chocolate, fruit aroma etc., compared with the control,
Irritation reduces, and impurity is reduced, not bitter, and mouthfeel improves, and overcomes lavenderessential oil lavender feature breath protrusion, pleasant impression
With bitter taste, slightly irritating defect；This method is raw materials used to be derived from a wealth of sources, and process conditions are environmentally protective, improve and smoke clothing
The application economic value of grass has industrialization prospect, further promotes the economic development in the raw material region place of production, improve the receipts of flower-grower
Enter, there is good social benefit.
Specific implementation mode
The present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
A kind of biofermentation prepares the preparation method of lavender absolute oil, includes the following steps：
(1) low temperature ultrasonic pre-processes：By lavender dried flower fringe and water in mass ratio 1:10 are uniformly mixed, and pour into microwave abstracting
It is pre-processed in instrument, obtains lavender flower spike microwave abstracting mixed material；
Further, the Microwave Extraction Apparatus operating condition described in step (1) is 2 DEG C of temperature, microwave frequency：It is 2450MHz, micro-
Wave power is power 300W, time 12min；
(2) fermentation is incubated：The lavender flower spike microwave abstracting mixed material that step (1) obtains is poured into fermentation extraction together
In tank, malic acid, oxalic acid, citric acid is added, composite biological agent is then added and stirs evenly, is heated to 36 DEG C, incubates fermentation
3.5d；
The malic acid, oxalic acid, citric acid are food-grade, account for the 0.12% of lavender flower spike material quality, between press
Mass ratio is 1:0.6:1；
The composite biological agent is beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus
(L.rhamnosus) mixing, is food-grade, and enzyme activity is respectively 800u/g, 5000u/g, 10000u/g, 2000u/g, biology
It is 1 in mass ratio between preparation:0.5:0.6:0.8:1, the composite biological agent accounts for lavender dried flower fringe mass ratio
0.12%；
(3) refluxing extraction：It ferments in extractor, the ethyl alcohol of 12 times of lavender dried flower fringe quality is added, adjustment temperature is 64
DEG C, refluxing extraction 3 times, screen filtration, merging filtrate, obtain lavender fermentation extracting solution, being concentrated under reduced pressure to give relative density is
1.25 lavender fermentation extraction medicinal extract；
Ethyl alcohol described in step (3) is food-grade；
(4) alcohol precipitation purifies：The lavender fermentation extraction medicinal extract that step 3) is obtained, 3 times of quality absolute ethyl alcohols of addition, 0 DEG C
It stands overnight, high-speed low temperature centrifugation stays supernatant, obtains the biofermentation lavender absolute oil of the present invention.
High-speed low temperature centrifugation described in step 4), operating condition 12000rpm, 1 DEG C of temperature；
The embodiment of the present invention also provides a kind of biofermentation preparation lavender absolute oil prepared by the above method.
The embodiment of the present invention also provides biofermentation prepared by a kind of above method and prepares lavender absolute oil in traditional cigarette
Or Novel heating does not burn the perfumed applications in cigarette composition pipe tobacco, additive amount accounts for the 0.01ppm of tobacco quality.
Embodiment 2
A kind of biofermentation prepares the preparation method of lavender absolute oil, includes the following steps：
(1) low temperature ultrasonic pre-processes：By lavender dried flower fringe and water in mass ratio 1:15 are uniformly mixed, and pour into microwave abstracting
It is pre-processed in instrument, obtains lavender flower spike microwave abstracting mixed material；
Further, the Microwave Extraction Apparatus operating condition described in step (1) is 5 DEG C of temperature, microwave frequency：It is 2450MHz, micro-
Wave power is power 500W, time 9min；
(2) fermentation is incubated：The lavender flower spike microwave abstracting mixed material that step (1) obtains is poured into fermentation extraction together
In tank, oxalic acid, citric acid, maleic acid is added, composite biological agent is then added and stirs evenly, is heated to 45 DEG C, incubates fermentation
2.5d；
The oxalic acid, citric acid, maleic acid are food-grade, account for the 0.24% of lavender flower spike material quality, between press
Mass ratio is 1:1.2:0.8；
The composite biological agent is beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus
(L.rhamnosus) mixing, is food-grade, and enzyme activity is respectively 2000u/g, 10000u/g, 20000u/g, 4000u/g, life
It is 1 in mass ratio between object preparation:1.5:0.8:1.2, the composite biological agent accounts for lavender dried flower fringe mass ratio
0.25%；
(3) refluxing extraction：It ferments in extractor, the ethyl alcohol of 10~50 times of lavender dried flower fringe quality is added, adjust temperature
It it is 70 DEG C, reflux carries 2 times, screen filtration, merging filtrate, obtains lavender fermentation extracting solution, is concentrated under reduced pressure to give relative density
For 1.22 lavender fermentation extraction medicinal extract；
Ethyl alcohol described in step 3) is food-grade；
(4) alcohol precipitation purifies：The lavender fermentation extraction medicinal extract that step 3) is obtained, 4 times of quality absolute ethyl alcohols of addition, 1 DEG C
It stands overnight, high-speed low temperature centrifugation stays supernatant, obtains the biofermentation lavender absolute oil of the present invention.
High-speed low temperature centrifugation described in step 4), operating condition 18000rpm, 2 DEG C of temperature；
The embodiment of the present invention also provides a kind of biofermentation preparation lavender absolute oil prepared by the above method.
The embodiment of the present invention also provides biofermentation prepared by a kind of above method and prepares lavender absolute oil in traditional cigarette
Or Novel heating does not burn the perfumed applications in cigarette composition pipe tobacco, additive amount accounts for the 0.02ppm of tobacco quality.
Embodiment 3
A kind of biofermentation prepares the preparation method of lavender absolute oil, includes the following steps：
(1) low temperature ultrasonic pre-processes：By lavender dried flower fringe and water in mass ratio 1:20 are uniformly mixed, and pour into microwave abstracting
It is pre-processed in instrument, obtains lavender flower spike microwave abstracting mixed material；
Further, the Microwave Extraction Apparatus operating condition described in step (1) is 6 DEG C of temperature, microwave frequency：It is 2450MHz, micro-
Wave power is power 900W, time 3min；
(2) fermentation is incubated：The lavender flower spike microwave abstracting mixed material that step (1) obtains is poured into fermentation extraction together
In tank, malic acid, oxalic acid, citric acid, maleic acid is added, composite biological agent is then added and stirs evenly, is heated to 52 DEG C, temperature
Educate fermentation 2.5d；
The malic acid, oxalic acid, citric acid, maleic acid are food-grade, account for the 0.27% of lavender flower spike material quality,
It is 1 in mass ratio:0.5:0.5:0.5；
The composite biological agent is beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus
(L.rhamnosus) mixing, is food-grade, and enzyme activity is respectively 10000u/g, 50000u/g, 30000u/g, 12000u/g,
It is 1 in mass ratio between biological agent:1:1.5:0.9, the composite biological agent accounts for lavender dried flower fringe mass ratio
0.27%；
(3) refluxing extraction：It ferments in extractor, the ethyl alcohol of 45 times of lavender dried flower fringe quality is added, adjustment temperature is 80
DEG C, refluxing extraction 1 time, screen filtration, merging filtrate, obtain lavender fermentation extracting solution, being concentrated under reduced pressure to give relative density is
1.30 lavender fermentation extraction medicinal extract；
Ethyl alcohol described in step 3) is food-grade；
(4) alcohol precipitation purifies：The lavender fermentation extraction medicinal extract that step 3) is obtained, 6 times of quality absolute ethyl alcohols of addition, 0 DEG C
It stands overnight, high-speed low temperature centrifugation stays supernatant, obtains the biofermentation lavender absolute oil of the present invention.
High-speed low temperature centrifugation described in step 4), operating condition 30000rpm, 0 DEG C of temperature；
The embodiment of the present invention also provides a kind of biofermentation preparation lavender absolute oil prepared by the above method.
The embodiment of the present invention also provides biofermentation prepared by a kind of above method and prepares lavender absolute oil in traditional cigarette
Or Novel heating does not burn the perfumed applications in cigarette composition pipe tobacco, additive amount accounts for the 0.015ppm of tobacco quality.
Test example 1：The sensory effects of application are evaluated
Lavender absolute oil prepared by embodiment 1-3 biofermentations is rolled into cigarette in cigarette composition pipe tobacco and carries out sense organ matter
Amount evaluation, sample are to be applied with cutting filler for lavender absolute oil prepared by biofermentation of the present invention to roll cigarette, and control group is
Apply cutting filler for the lavender absolute oil without biofermentation and roll cigarette, blank group is the volume that cuts filler of the non-flavoring of blank
Tobacco curing branch.
The result shows that：Lavender oil prepared by the biofermentation of the present invention flavoring in cigarette, coordinates, cigarette perfume very much with flue gas
Clear and natural, fragrance is naturally abundant, in addition to fragrance specific to fresh lavandulae flos and root of Aucklandia lappa Decne note, also carrying compound baking
Roasting, chocolate, fruit aroma etc., compared with the control, irritation reduce, and impurity is reduced, not bitter.
The sensory evaluation of lavender absolute oil prepared by 1 biofermentation of table in cutting filler
Test example 2：The HS-SPME-GC/MS comparative analyses of biofermentation lavender absolute oil volatile ingredient
Weigh biofermentation lavender absolute oil and compare (not ultrasound, biofermentation lavender absolute oil) respectively prepared by the present invention
1g is placed in the special headspace extraction sample bottles of 15mL；100 μm of PDMS extracting heads are selected, with aging 30min under the conditions of 250 DEG C,
The special headspace extraction sample bottles of 15mL equipped with sample are inserted into, after extracting 60min at 80 DEG C, carry out the GC/MS of volatile ingredient
Analysis.
GC/MS analysis conditions
(1) chromatographic condition：50 DEG C of column initial temperature keeps 2min, is warming up to 180 DEG C with the rate of 5 DEG C/min, keeps 1min,
280 DEG C are warming up to the rate of 15 DEG C/min again, keeps 20min；Carrier gas be helium (He, purity 99.99%), constant current mode,
Flow velocity is 1.0mL/min；Splitless injecting samples mode, solvent-free delay；250 DEG C of injector temperature.
(2) Mass Spectrometry Conditions：Ionization mode：The sources EI；Electron energy:70eV；Multiplier voltage：1.2kV；Ion source temperature：
230℃；Level four bars temperature:150℃；Interface temperature：280 DEG C, 280 DEG C of transmission line；Scanning range：33-350m/z.It uses
NIST standard spectrums library carries out retrieval analysis, and compound percentage contents are calculated by areas of peak normalization method.
The HS-SPME-GC/MS comparative analyses of 2 biofermentation lavender absolute oil of table and control sample volatile ingredient
As shown in Table 2,
(1) biofermentation of the present invention prepares lavender absolute oil, identifies 88 kinds of volatile ingredients altogether, total percentage contains
Amount is 91.12%, alcohol 24 kinds (16.28%), ketone 11 kinds (37.78%), alkanes 7 kinds (11.39%), 8 kinds of ester
(6.67%), alkenes 9 kinds (2.31%), acids 4 kinds (1.27%), aldehydes 4 kinds (3.09%), phenols a kind (4.81%)；
The control of lavender absolute oil identifies 88 kinds of volatile ingredients altogether, and total percentage contents are 84.68%, 18 kinds of alcohols
(15.96%), esters 13 kinds (8.25%), alkenes 12 kinds (4.90%), ketone 8 kinds (2.69%), acids 7 kinds (2.34%),
Alkanes 6 kinds (6.91%), aldehyde 5 kinds (3.92%), 19 kinds of other heterocyclics.
Biofermentation of the present invention is prepared in lavender absolute oil volatile ingredient, the highest object of single component percentage contents
Matter is 1,2- benzopyrones, 21.17%；Secondly it is 7- methoxyl group -1,2- benzopyrones, 13.88%；It is 1,2- rings again
Oxygen -2- methybutanes, 8.35%；Followed by m- 5- dimethlbenzenes, 4.81%；5th is the different nonyl ester of phthalic acid 2.88%；
(3) volatile ingredient that biofermentation of the present invention prepares lavender absolute oil is sent out compared with its non-biofermentation control
Larger variation is given birth to：
Newly there is fragrance component：69 kinds.
Identical ingredient：17 kinds, wherein percentage contents are increased 11 kinds, and reduction has 6 kinds；
The volatile ingredient of disappearance：70 kinds.
Lavender absolute oil prepared by biofermentation has the compound fragrance of nature, it may be possible to its macromolecular pungent or
Fragrance precursor substance is more converted into small molecule flavor matter or even is purified and gets rid of：Ethyl acetate is pleasantly sweet, 2- methyl
Furans carries a kind of chocolate odors, and isopentyl aldehyde has apple fragrance, has unique cocoa and coffee after 2 methyl butyraldehyde dilution
Fragrance, (+)-australene has a breath of pine, needle and resin-like, myrcenol have the fresh faint scent-fragrance of a flower-limette,
There is the fragrance of nut and baked goods, perilla alcohol to have faint amber (imperial saliva) fragrance, fragrance for Cologne fragrance, 2- methylpyrazines
Exquisiteness etc., these fragrant breaths rub up and assign lavender absolute oil prepared by the biofermentation of the present invention together, in addition to having
With fragrance specific to fresh lavandulae flos and root of Aucklandia lappa Decne note, compound baking, chocolate, fruit aroma etc., stimulation are also carried
Property reduce, impurity reduce, it is not bitter.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Belong to those skilled in the art in the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in all are answered
It is included within the scope of the present invention.
Claims (7)
1. a kind of method that biofermentation prepares lavender absolute oil, it is characterised in that include the following steps：
(1) low temperature ultrasonic pre-processes：By lavender dried flower fringe and water in mass ratio 1:10~20 are uniformly mixed, and pour into microwave abstracting
It is pre-processed in instrument, obtains lavender flower spike microwave abstracting mixed material；
(2) fermentation is incubated：The lavender flower spike microwave abstracting mixed material that step (1) obtains is poured into fermentation extractor, is added
Enter one or more of malic acid, oxalic acid, citric acid, maleic acid, composite biological agent is then added and stirs evenly, is heated to
35~55 DEG C, incubate fermentation 1d~4d；
The composite biological agent is beta-glucosidase, laccase, cellulase, Lactobacillus rhamnosus (L.rhamnosus)
Mixing, be food-grade, enzyme activity is 500~50000u/g, is 1 in mass ratio between biological agent:0.5~2:0.5~2:
0.5~2, the composite biological agent accounts for the 0.1~0.3% of lavender dried flower fringe mass ratio；
(3) refluxing extraction：The ethyl alcohol of 10~50 times of lavender dried flower fringe quality is added in the extractor that ferments, adjustment temperature is 60
~90 DEG C, refluxing extraction 1~3 time, screen filtration, merging filtrate, obtain lavender fermentation extracting solution, be concentrated under reduced pressure into relatively close
Degree extracts medicinal extract for 1.20~1.32 lavender fermentation；
(4) alcohol precipitation purifies：The lavender fermentation extraction medicinal extract that step (3) is obtained, 3~6 times of quality absolute ethyl alcohols of addition, 0~4
It DEG C stands overnight, high-speed low temperature centrifugation stays supernatant, obtains the biofermentation lavender absolute oil of the present invention.
2. the method that biofermentation as described in claim 1 prepares lavender absolute oil, it is characterised in that：The malic acid,
Oxalic acid, citric acid, maleic acid be food-grade, account for the 0.1~0.5% of lavender flower spike material quality, between in mass ratio be 1:
0.5~2:0.5~2:0.5~2.
3. the method that biofermentation as described in claim 1 prepares lavender absolute oil, it is characterised in that：Described in step (1)
Microwave Extraction Apparatus operating condition is 0~10 DEG C of temperature, microwave frequency：2450MHz, microwave power are 0~1000W of power, time 3
~15min.
4. the method that biofermentation as described in claim 1 prepares lavender absolute oil, it is characterised in that：Second in step (3)
Alcohol is food-grade.
5. the method that biofermentation as described in claim 1 prepares lavender absolute oil, it is characterised in that：Described in step (4)
High-speed low temperature centrifuges, and operating condition is 12000~30000rpm, 0~5 DEG C of temperature.
6. a kind of lavender absolute oil prepared such as any one of claim 1-5 the methods.
7. a kind of lavender absolute oil prepared such as any one of claim 1-5 the method traditional cigarette or Novel heating not
Perfumed applications in burning cigarette composition pipe tobacco, additive amount account for 0.01~0.1ppm of tobacco quality.
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