CN101671601A - Terpene essence for cigarettes, preparation method and use thereof - Google Patents
Terpene essence for cigarettes, preparation method and use thereof Download PDFInfo
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- CN101671601A CN101671601A CN200910196163A CN200910196163A CN101671601A CN 101671601 A CN101671601 A CN 101671601A CN 200910196163 A CN200910196163 A CN 200910196163A CN 200910196163 A CN200910196163 A CN 200910196163A CN 101671601 A CN101671601 A CN 101671601A
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- terpene
- cigarettes
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- tensio
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- 150000003505 terpenes Chemical class 0.000 title claims abstract description 78
- 235000019504 cigarettes Nutrition 0.000 title claims abstract description 66
- 235000007586 terpenes Nutrition 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 claims abstract description 59
- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
- 102000004882 Lipase Human genes 0.000 claims abstract description 22
- 108090001060 Lipase Proteins 0.000 claims abstract description 22
- 239000004367 Lipase Substances 0.000 claims abstract description 21
- 235000019421 lipase Nutrition 0.000 claims abstract description 21
- -1 terpene compounds Chemical class 0.000 claims abstract description 10
- 241000208125 Nicotiana Species 0.000 claims description 46
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 46
- 239000013543 active substance Substances 0.000 claims description 42
- 239000000243 solution Substances 0.000 claims description 34
- 102000004190 Enzymes Human genes 0.000 claims description 31
- 108090000790 Enzymes Proteins 0.000 claims description 31
- 230000008569 process Effects 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 15
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 235000019505 tobacco product Nutrition 0.000 claims description 12
- URAYPUMNDPQOKB-UHFFFAOYSA-N triacetin Chemical compound CC(=O)OCC(OC(C)=O)COC(C)=O URAYPUMNDPQOKB-UHFFFAOYSA-N 0.000 claims description 12
- 230000007062 hydrolysis Effects 0.000 claims description 11
- 238000006460 hydrolysis reaction Methods 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 239000003960 organic solvent Substances 0.000 claims description 10
- 239000000872 buffer Substances 0.000 claims description 9
- LOKCTEFSRHRXRJ-UHFFFAOYSA-I dipotassium trisodium dihydrogen phosphate hydrogen phosphate dichloride Chemical compound P(=O)(O)(O)[O-].[K+].P(=O)(O)([O-])[O-].[Na+].[Na+].[Cl-].[K+].[Cl-].[Na+] LOKCTEFSRHRXRJ-UHFFFAOYSA-I 0.000 claims description 9
- 239000002953 phosphate buffered saline Substances 0.000 claims description 9
- NIDGCIPAMWNKOA-WOJBJXKFSA-N Neophytadiene Natural products [C@H](CCC[C@@H](CCCC(C)C)C)(CCCC(C=C)=C)C NIDGCIPAMWNKOA-WOJBJXKFSA-N 0.000 claims description 7
- SZCBXWMUOPQSOX-WVJDLNGLSA-N all-trans-violaxanthin Chemical compound C(\[C@]12[C@@](O1)(C)C[C@@H](O)CC2(C)C)=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(\C)/C=C/C=C(\C)/C=C/[C@]1(C(C[C@H](O)C2)(C)C)[C@]2(C)O1 SZCBXWMUOPQSOX-WVJDLNGLSA-N 0.000 claims description 7
- NIDGCIPAMWNKOA-UHFFFAOYSA-N neophytadiene Chemical compound CC(C)CCCC(C)CCCC(C)CCCC(=C)C=C NIDGCIPAMWNKOA-UHFFFAOYSA-N 0.000 claims description 7
- 239000000376 reactant Substances 0.000 claims description 7
- 235000019245 violaxanthin Nutrition 0.000 claims description 7
- PVNVIBOWBAPFOE-UHFFFAOYSA-N Dinoxanthin Natural products CC1(O)CC(OC(=O)C)CC(C)(C)C1=C=CC(C)=CC=CC(C)=CC=CC=C(C)C=CC=C(C)C=CC1(C(CC(O)C2)(C)C)C2(C)O1 PVNVIBOWBAPFOE-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- PGYAYSRVSAJXTE-CLONMANBSA-N all-trans-neoxanthin Chemical compound C(\[C@]12[C@@](O1)(C)C[C@@H](O)CC2(C)C)=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(\C)/C=C/C=C(\C)C=C=C1C(C)(C)C[C@H](O)C[C@@]1(C)O PGYAYSRVSAJXTE-CLONMANBSA-N 0.000 claims description 6
- OWAAYLVMANNJOG-OAKWGMHJSA-N neoxanthin Natural products CC(=C/C=C(C)/C=C/C=C(C)/C=C=C1C(C)(C)CC(O)CC1(C)O)C=CC=C(/C)C=CC23OC2(C)CC(O)CC3(C)C OWAAYLVMANNJOG-OAKWGMHJSA-N 0.000 claims description 6
- 239000011942 biocatalyst Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 235000011187 glycerol Nutrition 0.000 claims description 5
- 238000012423 maintenance Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 229920000136 polysorbate Polymers 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 235000019506 cigar Nutrition 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 abstract description 10
- 239000000779 smoke Substances 0.000 abstract description 7
- 150000001875 compounds Chemical class 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004227 thermal cracking Methods 0.000 abstract description 4
- 239000002304 perfume Substances 0.000 abstract description 3
- 230000000391 smoking effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 125000003118 aryl group Chemical group 0.000 abstract 1
- 239000002440 industrial waste Substances 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 18
- 239000003546 flue gas Substances 0.000 description 18
- 238000005516 engineering process Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 238000004519 manufacturing process Methods 0.000 description 7
- 230000001737 promoting effect Effects 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 4
- 239000003205 fragrance Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- GYUZHTWCNKINPY-UHFFFAOYSA-N theaspirane Chemical compound O1C(C)CCC21C(C)(C)CCC=C2C GYUZHTWCNKINPY-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- 239000000796 flavoring agent Substances 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 235000019633 pungent taste Nutrition 0.000 description 2
- SGAWOGXMMPSZPB-UHFFFAOYSA-N safranal Chemical compound CC1=C(C=O)C(C)(C)CC=C1 SGAWOGXMMPSZPB-UHFFFAOYSA-N 0.000 description 2
- 230000001953 sensory effect Effects 0.000 description 2
- PQDRXUSSKFWCFA-CFNZNRNTSA-N solanone Chemical compound CC(=O)CC[C@@H](C(C)C)\C=C\C(C)=C PQDRXUSSKFWCFA-CFNZNRNTSA-N 0.000 description 2
- PQDRXUSSKFWCFA-UHFFFAOYSA-N solanone Natural products CC(=O)CCC(C(C)C)C=CC(C)=C PQDRXUSSKFWCFA-UHFFFAOYSA-N 0.000 description 2
- LDVVTQMJQSCDMK-UHFFFAOYSA-N 1,3-dihydroxypropan-2-yl formate Chemical compound OCC(CO)OC=O LDVVTQMJQSCDMK-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- IMKHDCBNRDRUEB-UHFFFAOYSA-N Dihydroactinidiolide Natural products C1CCC(C)(C)C2=CC(=O)OC21C IMKHDCBNRDRUEB-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 241000282326 Felis catus Species 0.000 description 1
- YKVWPZJHENXDAJ-VOTSOKGWSA-N Megastigmatrienone Chemical compound CC1=CC(=O)CC(C)(C)C1\C=C\C=C YKVWPZJHENXDAJ-VOTSOKGWSA-N 0.000 description 1
- 244000061458 Solanum melongena Species 0.000 description 1
- 235000002597 Solanum melongena Nutrition 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001574 biopsy Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 150000005690 diesters Chemical class 0.000 description 1
- IMKHDCBNRDRUEB-LLVKDONJSA-N dihydroactinidiolide Chemical compound C1CCC(C)(C)C2=CC(=O)O[C@@]21C IMKHDCBNRDRUEB-LLVKDONJSA-N 0.000 description 1
- 125000005594 diketone group Chemical group 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 239000004519 grease Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000003262 industrial enzyme Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 230000002366 lipolytic effect Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 239000006225 natural substrate Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000010525 oxidative degradation reaction Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 235000017509 safranal Nutrition 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229940089401 xylon Drugs 0.000 description 1
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to terpene essence for cigarettes prepared by utilizing terpene compounds, a preparation method and a use thereof. The preparation method of terpene essence for cigarettes comprises a preparation step of surfactant-coated lipase and an enzymolysis step of terpene compounds. Terpene essence for cigarettes can be used for smoking materials and has a good effect of aromatic flavoring and obviously improves plumpness and harmony of smoke. The method provided by the invention can shorten the reaction time of essence from 10-15 hours to 5-6 hours in a preparation of terpene compounds, reduce the reaction temperature from 120-160 DEG C to 25-40 DEG C, therefore volatilization loss of perfume compounds is reduced from 11-18% to 0.5-1.0% through a thermal cracking method, thequality of products is improved, and meanwhile no discharge of industrial wastes is achieved.
Description
[technical field]
The present invention relates to the cigarette technical field.More specifically, the present invention relates to a kind of terpene essence for cigarettes that uses the terpene compound preparation, also relate to the preparation method of described terpene essence for cigarettes and their purposes.
[background technology]
The fragrance of cigarette, pleasant impression, assorted gas, pungency, Harmony etc. are the important quality features of tobacco product.Current both at home and abroad to these control of index of quality methods, mainly be to control by adding some distinctive compounds.Main micro-characterization compound mainly comprises jononeionone, oxo-beta-trans-Damascenone, Megastigmatrienone, oxidation isophorone, dihydroactinidiolide, dihydro-actinidia alcohol, solanone, falls eggplant diketone, different solanone, epoxy theaspirane, theaspirane, dihydro safranal, acetate oxo α-serial related compounds such as violet alcohol ester in the tobacco.No matter these compounds are to promote cigarette perfume (or spice), improving the flue gas pleasant impression, have still all brought into play vital role to improving tobacco quality at aspects such as reducing flue gas pungency, enhancement suction flavor.What have been found that in the tobacco at present has the characteristic compound of castering action can reach more than hundreds of to the flue gas quality.
Terpenoid in tobacco is the general name of a class polyene hydrocarbon macromolecular substance, and they can generate the less fragrance matter of many molecular weight through after the oxidative degradation, are the important sources of fragrance matter in the tobacco.No matter domestic or now use the method for terpenoid abroad as the feedstock production flavouring essence for tobacco, all be employing normal pressure pyrolytic method.Adopt this method to produce flavouring essence for tobacco and have following defective usually: 1. long reaction time, energy consumption is big, production efficiency is low; 2. product yield is low, cost is high; 3. temperature of reaction height, aroma component volatilization loss are bigger.
Current both at home and abroad to how changing terpenoid pyrolysis method production flavouring essence for tobacco technology, invent a kind of reaction times short, production efficiency is high, less energy consumption, cracking temperature is low, aroma component volatilization loss is few, product effective content height, the terpenoid flavouring essence for tobacco novel method that consumption is few, cost is low yet there are no report; Do not retrieve the document of producing the terpenoid flavouring essence for tobacco without thermal-cracking method at home and abroad in the patent documentation yet.
Therefore invent and a kind ofly can effectively overcome the shortcoming that pyrolysis method is produced the terpenoid flavouring essence for tobacco, have that reaction times weak point, less energy consumption, aroma component volatilization loss are little, the novel preparation method of product effective content height, terpenoid flavouring essence for tobacco that cost is low is very necessary.For this reason, the inventor has finished the present invention finally through lot of experiments.
[summary of the invention]
[technical problem that will solve]
The purpose of this invention is to provide a kind of terpene essence for cigarettes.
Another object of the present invention provides the preparation method of described terpene essence for cigarettes.
Another object of the present invention provides the purposes of described terpene essence for cigarettes.
[technical scheme]
The present invention is achieved through the following technical solutions.
The present invention relates to a kind of preparation method of terpene essence for cigarettes, it is characterized in that the step of this method is as follows:
The preparation of A, tensio-active agent dressing enzyme:
(1) 0.3-0.5 weight part lipase is joined in 200-300 part phosphate buffered saline buffer, adopt supersound process to dissolving fully;
(2) 0.1-0.6 weight part tensio-active agent is joined in 150-300 part water, adopt supersound process to dissolving fully;
(3) solution that obtains of step (1) adopts supersound process to mix 20-30min with the solution that step (2) obtains, and uses after 4 ℃ of temperature are placed 24h down in refrigerator then;
(4) mixed solution that step (3) is obtained is divided in the culture dish, control liquid level thickness is 3-5mm, place the precooling temperature-20 ℃ following 6h of maintenance then, again at the lyophilize temperature-30 ℃ following 10h that keeps, then under drying chamber pressure 0.1-0.3 millibar, carry out lyophilize 20-30h, so obtain described tensio-active agent dressing enzyme;
B, terpenoid enzymolysis
(1) 0.5-2.5 weight part cigarette is joined in 95-105 part organic solvent with the terpene recombiner, adopt supersound process to dissolving fully;
(2) the tensio-active agent dressing enzyme of 0.05-0.2 weight part step (A) preparation is joined in the solution that 90-100 part step (1) obtains; Resulting solution is put into reactor, reacts 5-10h under the condition of low whipping speed 100-300 rev/min, hydrolysis temperature 25-40 ℃ and reaction solution pH 5.5-6.5, after reaction finishes reactant is cooled to room temperature and obtains described terpene essence for cigarettes.
A preferred embodiment of the invention, described lipase are one or more lipase that are selected from the Lipoxygenase-I of Britain BIOCATALYSTS company, Lipoxygenase-II or Lipoxygenase-III.
According to another kind of preferred implementation of the present invention, the pH of described phosphate buffered saline buffer is 7.0-7.5.
According to another kind of preferred implementation of the present invention, described tensio-active agent is one or more nonionogenic tenside or other class tensio-active agents of being selected from tween, sapn or glycerin fatty acid ester.
According to another kind of preferred implementation of the present invention, described cigarette is made up of 0.2-0.3 weight part neoxanthin, 0.1-0.2 weight part zeaxanthin diepoxide, 0.1-0.3 weight part Lyeopene and 0.1-0.3 weight part neophytadiene with the terpene recombiner.
According to another kind of preferred implementation of the present invention, described organic solvent is one or more tensio-active agents that are selected from glycerine triacetate, ethanol, propylene glycol or ethyl acetate.
In the present invention, described supersound process is ultrasonic frequency 30-50kHz, supersound process time 15-20min.
In addition, the invention still further relates to the resulting terpene essence for cigarettes of the previously defined method of employing.
The invention still further relates to the purposes of described terpene essence for cigarettes in tobacco product, it is characterized in that it contains in this tobacco product gross weight 0.01-0.10 weight % to adopt the resulting terpene essence for cigarettes of front define method.
In the present invention, described tobacco product is cigarette, cigar, pipe tobacco or redried leaf tobacco.
Below the present invention will be described in more detail.
The present invention relates to a kind of preparation method of terpene essence for cigarettes, this method divides two steps to finish, and the first prepares tensio-active agent dressing enzyme; It two is terpenoid enzymolysis.
The preparation of A, tensio-active agent dressing enzyme:
(1) 0.3-0.5 weight part lipase is joined in 200-300 part phosphate buffered saline buffer, adopt supersound process to dissolving fully;
(2) 0.1-0.6 weight part tensio-active agent is joined in 150-300 part water, adopt supersound process to dissolving fully;
(3) solution that obtains of step (1) adopts supersound process to mix 20-30min with the solution that step (2) obtains, and uses after 4 ℃ of temperature are placed 24h down in refrigerator then;
(4) mixed solution that step (3) is obtained is divided in the culture dish, control liquid level thickness is 3-5mm, place the precooling temperature-20 ℃ following 6h of maintenance then, again at the lyophilize temperature-30 ℃ following 10h that keeps, then under drying chamber pressure 0.1-0.3 millibar, carry out lyophilize 20-30h, so obtain described tensio-active agent dressing enzyme.
People know that lipase is the triacylglycerol Acyl-hydrolase, are one of important industrial enzyme preparation kinds, can catalysis separate reactions such as fat, transesterify, ester is synthetic, and its catalysis natural substrate fat hydrolysis generates lipid acid, glycerine and monoglyceride or diester.Lipase essentially consist unit only is an amino acid, and its catalytic activity only is decided by its protein structure.Lipase is widely used in industry such as grease processing, food, medicine, daily use chemicals.The lipase of different sources has different catalysis characteristics and catalysis activity.
In the present invention, lipase should be appreciated that be a class have hydrolysis have the isoprene fat chain structure, have an enzyme of multiple catalytic capability simultaneously.
Described lipase is one or more lipase that are selected from the Lipoxygenase-I of Britain BIOCATALYSTS company, Lipoxygenase-II or Lipoxygenase-III.
More preferably, described lipase is one or more lipase that are selected from Lipoxygenase-I or Lipoxygenase-III.
Described phosphate buffered saline buffer is with NaH
2PO
4And Na
2HPO
4Blended phosphate buffered saline buffer by a certain percentage.
People know that tensio-active agent is meant to have fixed hydrophilic and oleophilic group, align at the surface energy of solution, and the material that surface tension is significantly descended, they comprise positively charged ion, negatively charged ion, nonionic or zwitterionics.
In the present invention, described tensio-active agent can be a nonionogenic tenside.
Described tensio-active agent is one or more nonionogenic tenside or other class tensio-active agents of being selected from tween, sapn or glycerin fatty acid ester.
More preferably, described tensio-active agent is one or more tensio-active agents that are selected from tween or glycerin fatty acid ester.
People know, ultrasonic wave is meant vibrational frequency greater than more than the 20KHz, the sound wave that the people can't hear and experience under physical environment.When ultrasonic wave is propagated in liquid, because the high vibration of liquid particle can produce little cavity at liquid internal.These little cavities swell rapidly and are closed, can make the fierce effect of impact of generation between the liquid particle, thereby produce several thousand to up to ten thousand atmospheric pressure.This violent interaction between particulate can make the temperature of liquid raise suddenly, has played good stirring action, thereby makes two kinds of immiscible liquid generation emulsifications, and adds the dissolving of fast solute, can impel to take place or the acceleration chemical reaction.
In the present invention, the condition of described supersound process is ultrasonic frequency 30-50kHz, supersound process time 15-20min,
The supersound process equipment that uses is that Shanghai Branson Ultrasonics Corp. reaches ultrasonic device company with trade(brand)name SDQ-1001 product sold with commodity CQX25-12 product sold, the Baoan district of Shenzhen city rising sun.
In the present invention, described tensio-active agent dressing enzyme is by Freeze Drying Technique lipase to be wrapped in the tensio-active agent.
The enzyme biopsy survey method of described tensio-active agent dressing enzyme is to make index with acid value, makes terminator with 95% ethanol, by the lipolytic degree of mensuration reflection lipase of acid value, thereby tries to achieve enzyme activity.
B, terpenoid enzymolysis
(1) 0.5-2.5 weight part cigarette is joined in 95-105 part organic solvent with the terpene recombiner, adopt supersound process to dissolving fully.
Preferably, use 1.0-2.0 weight part cigarette terpene recombiner and 95-105 part organic solvent.
More preferably, use 1.5-2.0 weight part cigarette terpene recombiner and 95-105 part organic solvent.
In the present invention, described cigarette is made up of 0.2-0.3 weight part neoxanthin, 0.1-0.2 weight part zeaxanthin diepoxide, 0.1-0.3 weight part Lyeopene and 0.1-0.3 weight part neophytadiene with the terpene recombiner.
Wherein: neoxanthin for example is that Chengdu Fu Run moral company is with trade(brand)name xenthophylls (food grade) product sold.Zeaxanthin diepoxide for example is that Chengdu Fu Run moral company is with trade(brand)name zeaxanthin diepoxide product sold.Lyeopene for example is that company of Shanghai PCI-SLR Technology natural food pigment company limited is with trade(brand)name Lyeopene product sold.Neophytadiene for example is that HuaBao flavor composition and spice company is with trade(brand)name neophytadiene product sold.
Described organic solvent is one or more tensio-active agents that are selected from glycerine triacetate, ethanol, propylene glycol or ethyl acetate.
Preferably, described organic solvent is one or more tensio-active agents that are selected from glycerine triacetate, propylene glycol or ethyl acetate.
More preferably, described organic solvent is one or more tensio-active agents that are selected from glycerine triacetate or ethyl acetate.
(2) the tensio-active agent dressing enzyme of 0.05-0.2 weight part step (A) preparation is joined in the solution that 90-100 part step (1) obtains.
Preferably, use the tensio-active agent dressing enzyme of 0.05-0.12 weight part step (A) preparation and the solution that 90-100 part step (1) obtains.
More preferably, use the tensio-active agent dressing enzyme of 0.09-0.12 weight part step (A) preparation and the solution that 90-100 part step (1) obtains.
Resulting solution is put into reactor, reacts 5-10h under the condition of low whipping speed 100-300 rev/min, hydrolysis temperature 25-40 ℃ and reaction solution pH 5.5-6.5, after reaction finishes reactant is cooled to room temperature and obtains described terpene essence for cigarettes.
Preferably carry out enzymolysis: stirring velocity 200-300 rev/min, hydrolysis temperature 25-38 ℃, reaction solution pH 5.5-6.0 and reaction times 5-8h under the following conditions.
More preferably carry out enzymolysis: stirring velocity 200-300 rev/min, hydrolysis temperature 35-38 ℃, reaction solution pH 5.6-6.0 and reaction times 5-8h under the following conditions.
In addition, the invention still further relates to the resulting terpene essence for cigarettes of the previously defined method of employing.
The invention still further relates to the purposes of described terpene essence for cigarettes in tobacco product, it is characterized in that it contains in this tobacco product gross weight 0.01-0.10 weight % to adopt the resulting terpene essence for cigarettes of front define method.
In the present invention, described tobacco product is cigarette, cigar, pipe tobacco or redried leaf tobacco.
Can be sprayed at pipe tobacco or be coated on the tobacco sheet according to conventional perfuming process program, balance 48 hours in climatic chamber be then played cigarette or chopping again and is beaten cigarette and make cigarette and prop up, and carries out sensory evaluating smoking's evaluation at last.
Described sensory evaluating smoking's authentication method is that five cigarettes of magnificent precious essence and flavoring agent company are formed evaluation group with the perfumer by our company, adopt the method for secretly commenting, carry out grade estimation according to fragrance matter, amount, harmony, assorted gas, stimulation, strength and six index grade standards of pleasant impression that our company sets up, so that the cigarette influence of terpenes essence among relatively more existing essence and the present invention to the tobacco product quality.
[beneficial effect]
The present invention has following positively effect:
1, realized no trade waste discharging.Produce the terpenoid flavouring essence for tobacco with respect to traditional pyrolysis technology that passes through, owing in enzymolysis process, do not need to add catalyzer such as heavy metal ion, so this technology is real environmentally friendly essence production technology.
2, shorten the reaction times, prepare 10-15 hour of terpenoid flavouring essence for tobacco reaction times, shorten to 5-6 hour, improved production efficiency by thermal-cracking method.
3, reduce temperature of reaction, prepare 120-160 ℃ of terpenoid flavouring essence for tobacco temperature of reaction, be reduced to 25-40 ℃ by non-pressure process.Because temperature of reaction reduces, make aroma component volatilization loss be reduced to 0.5-1.0% by thermal-cracking method loss 11-18%, improved product production.
[embodiment]
Embodiment 1: the preparation of terpene essence for cigarettes
Preparation process is as follows:
The preparation of A, tensio-active agent dressing enzyme:
(1) 0.4 gram BIOCATALYSTS company is joined in the 250ml phosphate buffered saline buffer (pH7.0) with the lipase that trade(brand)name Lipoxygenase-I sells, the ultrasonoscope that uses Shanghai Branson Ultrasonics Corp. to sell with trade(brand)name CQX25-12 carries out supersound process to dissolving fully;
(2) nonionogenic tenside that 0.4 gram Yingzheng Scirnce and Technology Co., Ltd., Shanghai is sold with trade(brand)name tween (food grade) joins in the 200ml water, uses with above-mentioned same ultrasonoscope and carries out supersound process to dissolving fully;
(3) solution that obtains of step (1) and solution that step (2) obtains use and carry out supersound process with above-mentioned same ultrasonoscope and mixes 25min, use behind 4 ℃ times placements of temperature 24h in refrigerator then;
(4) mixed solution that step (3) is obtained is divided in the culture dish, control liquid level thickness is 4mm, place the precooling temperature-20 ℃ following 6h of maintenance then, again at the lyophilize temperature-30 ℃ following 10h that keeps, then under 0.2 millibar of drying chamber pressure, carry out lyophilize 25h, so obtain described tensio-active agent dressing enzyme;
B, terpenoid enzymolysis
(1) prepares tobacco terpene recombiner earlier, 0.25 gram neoxanthin, 0.15 gram zeaxanthin diepoxide, 0.2 gram Lyeopene, 0.2 gram neophytadiene are mixed, obtain tobacco terpene recombiner of the present invention.Then, this cigarette is joined in the 100ml glycerine triacetate with the terpene recombiner, use with above-mentioned same ultrasonoscope and carry out supersound process to dissolving fully;
(2) the tensio-active agent dressing enzyme with 0.1 gram above-mentioned steps (A) preparation joins 100ml in the solution that step (1) obtains; Resulting solution is put into reactor, reacts 5h under the condition of 35 ℃ of 200 rev/mins of low whipping speeds, hydrolysis temperature and reaction solution pH6.0, after reaction finishes reactant is cooled to room temperature and obtains described terpene essence for cigarettes.
According to the ratio of tobacco gross weight 3/10000ths, the terpene essence for cigarettes that makes is added to Guizhou B in 2006
3Smoke panel test in the F pipe tobacco, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Embodiment 2: the preparation of terpene essence for cigarettes
Preparation process is as follows:
The embodiment of this embodiment is identical with embodiment 1, only be to use 2.50 gram tobacco terpene recombiners of embodiment 1 preparation, the tensio-active agent dressing enzyme of 0.12 gram embodiment, 1 preparation, 200 rev/mins of low whipping speeds, 38 ℃ of hydrolysis temperatures, reaction solution pH 5.6 and reaction times 7h are cooled to room temperature with reactant and obtain described terpene essence for cigarettes after reaction finishes.
According to the ratio of tobacco gross weight 3/10000ths, the terpene essence for cigarettes that makes is added to Yunnan B in 2006
3Smoke panel test in the F pipe tobacco, it is clean that the result shows that this product can effectively improve pleasant impression, the oral cavity of flue gas, and this product also can play good perfuming effect simultaneously, obviously improves the plumpness and the Harmony of flue gas.
Embodiment 3: the preparation of terpene essence for cigarettes
Preparation process is as follows:
The embodiment of this embodiment is identical with embodiment 1, only be to use 1.50 gram tobacco terpene recombiners of embodiment 1 preparation, the tensio-active agent dressing enzyme of 0.09 gram embodiment, 1 preparation, 150 rev/mins of low whipping speeds, 38 ℃ of hydrolysis temperatures, reaction solution pH 6.0 and reaction times 8h are cooled to room temperature with reactant and obtain described terpene essence for cigarettes after reaction finishes.
According to the ratio of tobacco gross weight 3/10000ths, the terpene essence for cigarettes that makes is added to Shandong B in 2006
3Smoke panel test in the F pipe tobacco, the result shows that this product can effectively cover xylon gas in the tobacco and blue foreign smell, reduction strength, obviously improve assorted gas, gives tobacco product with good fresh and sweet perfume (or spice), also can effectively improve the soften and the sophistication of flue gas simultaneously.
Embodiment 4: the preparation of terpene essence for cigarettes
Preparation process is as follows:
The preparation of A, tensio-active agent dressing enzyme:
(1) 0.3 gram BIOCATALYSTS company is joined in the 250ml phosphate buffered saline buffer (pH7.0) with the lipase that trade(brand)name Lipoxygenase-III sells, the ultrasonoscope that uses Shanghai Branson Ultrasonics Corp. to sell with trade(brand)name CQX25-12 carries out supersound process to dissolving fully;
(2) nonionogenic tenside that the positive Science and Technology Ltd. in 0.6 gram sea is sold with the trade(brand)name sapn joins in 300 parts of water, uses with above-mentioned same ultrasonoscope and carries out supersound process to dissolving fully;
(3) solution that obtains of step (1) and solution that step (2) obtains use and carry out supersound process with above-mentioned same ultrasonoscope and mixes 205min, use behind 4 ℃ times placements of temperature 24h in refrigerator then;
(4) mixed solution that step (3) is obtained is divided in the culture dish, control liquid level thickness is 4mm, place the precooling temperature-20 ℃ following 6h of maintenance then, again at the lyophilize temperature-30 ℃ following 10h that keeps, then under 0.2 millibar of drying chamber pressure, carry out lyophilize 25h, so obtain described tensio-active agent dressing enzyme.
B, terpenoid enzymolysis
(1) prepares tobacco terpene recombiner earlier, 0.20 gram neoxanthin, 0.20 gram zeaxanthin diepoxide, 0.28 gram Lyeopene, 0.10 gram neophytadiene are mixed, obtain tobacco terpene recombiner of the present invention.Then, this cigarette is joined in the 90ml ethanol with the terpene recombiner, use with above-mentioned same ultrasonoscope and carry out supersound process to dissolving fully;
(2) the tensio-active agent dressing enzyme with 0.1 gram above-mentioned steps (A) preparation joins 100ml in the solution that step (1) obtains; Resulting solution is put into reactor, reacts 9h under the condition of 25 ℃ of 100 rev/mins of low whipping speeds, hydrolysis temperature and reaction solution pH6.5, after reaction finishes reactant is cooled to room temperature and obtains described terpene essence for cigarettes.
According to the ratio of tobacco gross weight 2/10000ths, the terpene essence for cigarettes that makes is added to Guizhou B in 2006
3Smoke panel test in the F pipe tobacco, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Embodiment 5: the preparation of terpene essence for cigarettes
The embodiment of this embodiment is identical with embodiment 4, only is to use the tensio-active agent dressing enzyme of 0.2 gram above-mentioned steps (A) preparation and the solution that 90ml obtains in step (1).
According to the ratio of tobacco gross weight 8/10000ths, the terpene essence for cigarettes that makes is added to Guizhou B in 2006
3Smoke panel test in the F pipe tobacco, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Embodiment 6: the preparation of terpene essence for cigarettes
The embodiment of this embodiment is identical with embodiment 4, but the anion surfactant that uses the positive Science and Technology Ltd. in 0.2 gram sea to sell with the trade(brand)name Sodium dodecylbenzene sulfonate.
According to the ratio of tobacco gross weight 3/10000ths, the terpene essence for cigarettes that makes added to smoked panel test in the B3F pipe tobacco of Guizhou in 2006, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Embodiment 7: the preparation of terpene essence for cigarettes
The embodiment of this embodiment is identical with embodiment 4, but the cats product that uses the positive Science and Technology Ltd. in 0.4 gram sea to sell with the quaternized thing of trade(brand)name.
According to the ratio of tobacco gross weight 8/10000ths, the terpene essence for cigarettes that makes added to smoked panel test in the B3F pipe tobacco of Guizhou in 2006, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Embodiment 8: the preparation of terpene essence for cigarettes
The embodiment of this embodiment is identical with embodiment 4, but the zwitterionics that uses the positive Science and Technology Ltd. in 0.4 gram sea to sell with trade(brand)name Yelkin TTS.
According to the ratio of tobacco gross weight 8/10000ths, the terpene essence for cigarettes that makes is added to Guizhou B in 2006
3Smoke panel test in the F pipe tobacco, the result shows that this product can be good at promoting the quality of flue gas, and flue gas is soft, fine and smooth, and Harmony all has greatly improved.
Claims (10)
1, a kind of preparation method of terpene essence for cigarettes is characterized in that the step of this method is as follows:
The preparation of A, tensio-active agent dressing enzyme:
(1) 0.3-0.5 weight part lipase is joined in 200-300 part phosphate buffered saline buffer, adopt supersound process to dissolving fully;
(2) 0.1-0.6 weight part tensio-active agent is joined in 150-300 part water, adopt supersound process to dissolving fully;
(3) solution that obtains of step (1) adopts supersound process to mix 20-30min with the solution that step (2) obtains, and uses after 4 ℃ of temperature are placed 24h down in refrigerator then;
(4) mixed solution that step (3) is obtained is divided in the culture dish, control liquid level thickness is 3-5mm, place the precooling temperature-20 ℃ following 6h of maintenance then, again at the lyophilize temperature-30 ℃ following 10h that keeps, then under drying chamber pressure 0.1-0.3 millibar, carry out lyophilize 20-30h, so obtain described tensio-active agent dressing enzyme;
B, terpenoid enzymolysis
(1) 0.5-2.5 weight part cigarette is joined in 95-105 part organic solvent with the terpene recombiner, adopt supersound process to dissolving fully;
(2) the tensio-active agent dressing enzyme of 0.05-0.2 weight part step (A) preparation is joined in the solution that 90-100 part step (1) obtains; Resulting solution is put into reactor, reacts 5-10h under the condition of low whipping speed 100-300 rev/min, hydrolysis temperature 25-40 ℃ and reaction solution pH 5.5-6.5, after reaction finishes reactant is cooled to room temperature and obtains described terpene essence for cigarettes.
2, method according to claim 1 is characterized in that described lipase is one or more lipase that are selected from the Lipoxygenase-I of Britain BIOCATALYSTS company, Lipoxygenase-II or Lipoxygenase-III.
3, method according to claim 1, the pH that it is characterized in that described phosphate buffered saline buffer is 7.0-7.5.
4, method according to claim 1 is characterized in that described tensio-active agent is one or more nonionogenic tenside or other class tensio-active agents that are selected from tween, sapn or glycerin fatty acid ester.
5, method according to claim 1 is characterized in that described cigarette is made up of 0.2-0.3 weight part neoxanthin, 0.1-0.2 weight part zeaxanthin diepoxide, 0.1-0.3 weight part Lyeopene and 0.1-0.3 weight part neophytadiene with the terpene recombiner.
6, method according to claim 1 is characterized in that described organic solvent is one or more tensio-active agents that are selected from glycerine triacetate, ethanol, propylene glycol or ethyl acetate.
7, method according to claim 1 is characterized in that described supersound process is ultrasonic frequency 30-50kHz, supersound process time 15-20min.
8, according to the resulting terpene essence for cigarettes of the described method of each claim among the claim 1-7.
9, the purposes of terpene essence for cigarettes according to claim 8 in tobacco product is characterized in that it contains in this tobacco product gross weight 0.01-0.10 weight % according to the resulting terpene essence for cigarettes of the described method of each claim among the claim 1-7.
10, purposes according to claim 9 is characterized in that described tobacco product is cigarette, cigar, pipe tobacco or redried leaf tobacco.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102127489A (en) * | 2011-02-14 | 2011-07-20 | 云南省玉溪市云溪香精香料有限责任公司 | Preparation method of tobacco spice neophytadiene carvone methyl palmitate megastigmatrienone essential oil |
| CN102559831A (en) * | 2011-12-23 | 2012-07-11 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of 3, 6, 6-trimethylcycloheptyl-2-alkene-1-ketone fragrance |
| CN103391949A (en) * | 2011-01-28 | 2013-11-13 | R·J·雷诺兹烟草公司 | Polymeric materials derived from tobacco |
| CN103451019A (en) * | 2013-09-04 | 2013-12-18 | 湖北中烟工业有限责任公司 | Microcapsule essence perfume for cigarettes as well as preparation method of microcapsule essence perfume |
| CN105746981A (en) * | 2014-12-17 | 2016-07-13 | 味特生物科技股份有限公司 | Method for manufacturing natural milk-flavor essence |
| CN110140993A (en) * | 2011-04-27 | 2019-08-20 | R·J·雷诺兹烟草公司 | Component and material from tobacco |
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| CN1205161C (en) * | 2003-01-24 | 2005-06-08 | 华宝香化科技发展（上海）有限公司 | Process for synthesizing megastigmatrienone perfume |
| CN1205160C (en) * | 2003-01-24 | 2005-06-08 | 华宝香化科技发展（上海）有限公司 | Method for producing perfume using ionol ester as raw material by thermo-wacking rectifying |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103391949A (en) * | 2011-01-28 | 2013-11-13 | R·J·雷诺兹烟草公司 | Polymeric materials derived from tobacco |
| CN103391949B (en) * | 2011-01-28 | 2015-10-07 | R·J·雷诺兹烟草公司 | The polymer materials that tobacco is derivative |
| CN102127489A (en) * | 2011-02-14 | 2011-07-20 | 云南省玉溪市云溪香精香料有限责任公司 | Preparation method of tobacco spice neophytadiene carvone methyl palmitate megastigmatrienone essential oil |
| CN110140993A (en) * | 2011-04-27 | 2019-08-20 | R·J·雷诺兹烟草公司 | Component and material from tobacco |
| CN102559831A (en) * | 2011-12-23 | 2012-07-11 | 华宝食用香精香料（上海）有限公司 | Preparation method and application of 3, 6, 6-trimethylcycloheptyl-2-alkene-1-ketone fragrance |
| CN103451019A (en) * | 2013-09-04 | 2013-12-18 | 湖北中烟工业有限责任公司 | Microcapsule essence perfume for cigarettes as well as preparation method of microcapsule essence perfume |
| CN105746981A (en) * | 2014-12-17 | 2016-07-13 | 味特生物科技股份有限公司 | Method for manufacturing natural milk-flavor essence |
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| CN101671601B (en) | 2013-01-09 |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Patentee after: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee before: Huabao flavor Ltd. Patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. |
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Address after: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Patentee after: Huabao flavor Ltd. Patentee after: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. Address before: 201821 Yecheng Road, Shanghai, No. 1299, No. Patentee before: Huabao Flavours & Fragrances Co.,Ltd Patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. |
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Address after: 850000, Tibet, Lhasa Economic Development Zone, Lhasa sang road investment building, 6 floor Co-patentee after: Wuxi Huaxin essence Co.,Ltd. Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Address before: 850000 Lhasa economic and Technological Development Zone, Tibet autonomous region, road, investment building, Co-patentee before: Wuxi Huaxin Flavor & Fragrance Co.,Ltd. Patentee before: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. |
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Effective date of registration: 20180718 Address after: 850000 the 6 floor of investment building, Ge sang Road, Lhasa Economic Development Zone, Lhasa, Tibet. Patentee after: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. Address before: 850000 the 6 floor of investment building, Ge sang Road, Lhasa Economic Development Zone, Lhasa, Tibet. Co-patentee before: Wuxi Huaxin essence Co.,Ltd. Patentee before: HUABAO FLAVOURS & FRAGRANCES CO.,LTD. |