CN105132166A - Tobacco apple perfume and preparation method thereof - Google Patents
Tobacco apple perfume and preparation method thereof Download PDFInfo
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- CN105132166A CN105132166A CN201510445524.6A CN201510445524A CN105132166A CN 105132166 A CN105132166 A CN 105132166A CN 201510445524 A CN201510445524 A CN 201510445524A CN 105132166 A CN105132166 A CN 105132166A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 235000002637 Nicotiana tabacum Nutrition 0.000 title abstract description 10
- 239000002304 perfume Substances 0.000 title abstract description 7
- 244000061176 Nicotiana tabacum Species 0.000 title abstract 3
- 239000000706 filtrate Substances 0.000 claims abstract description 53
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims abstract description 27
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000001914 filtration Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 150000002148 esters Chemical class 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 claims abstract description 9
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 claims abstract description 9
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229960001285 quercetin Drugs 0.000 claims abstract description 9
- 235000005875 quercetin Nutrition 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 75
- 239000004615 ingredient Substances 0.000 claims description 50
- 238000003756 stirring Methods 0.000 claims description 42
- 235000019504 cigarettes Nutrition 0.000 claims description 40
- 235000013599 spices Nutrition 0.000 claims description 35
- 239000000919 ceramic Substances 0.000 claims description 30
- 238000005374 membrane filtration Methods 0.000 claims description 26
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 24
- 239000004744 fabric Substances 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 20
- XINCECQTMHSORG-UHFFFAOYSA-N Isoamyl isovalerate Chemical compound CC(C)CCOC(=O)CC(C)C XINCECQTMHSORG-UHFFFAOYSA-N 0.000 claims description 17
- 102000004190 Enzymes Human genes 0.000 claims description 16
- 108090000790 Enzymes Proteins 0.000 claims description 16
- 229940088598 enzyme Drugs 0.000 claims description 16
- PPXUHEORWJQRHJ-UHFFFAOYSA-N ethyl isovalerate Chemical compound CCOC(=O)CC(C)C PPXUHEORWJQRHJ-UHFFFAOYSA-N 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 9
- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-UHFFFAOYSA-N 0.000 claims description 8
- 239000004382 Amylase Substances 0.000 claims description 8
- 102000013142 Amylases Human genes 0.000 claims description 8
- 108010065511 Amylases Proteins 0.000 claims description 8
- 108010059892 Cellulase Proteins 0.000 claims description 8
- 102000035195 Peptidases Human genes 0.000 claims description 8
- 108091005804 Peptidases Proteins 0.000 claims description 8
- 235000019418 amylase Nutrition 0.000 claims description 8
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 claims description 8
- 229940106157 cellulase Drugs 0.000 claims description 8
- 230000008719 thickening Effects 0.000 claims description 8
- 238000013467 fragmentation Methods 0.000 claims description 4
- 238000006062 fragmentation reaction Methods 0.000 claims description 4
- 239000003205 fragrance Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 5
- 150000007524 organic acids Chemical class 0.000 abstract description 5
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 5
- 235000013824 polyphenols Nutrition 0.000 abstract description 5
- 150000002772 monosaccharides Chemical class 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 2
- 241000220225 Malus Species 0.000 abstract 7
- 235000021016 apples Nutrition 0.000 abstract 2
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 abstract 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 235000011090 malic acid Nutrition 0.000 abstract 1
- 239000001630 malic acid Substances 0.000 abstract 1
- 235000005985 organic acids Nutrition 0.000 abstract 1
- 239000012528 membrane Substances 0.000 description 18
- 238000002137 ultrasound extraction Methods 0.000 description 12
- 150000004676 glycans Chemical class 0.000 description 8
- 229920001282 polysaccharide Polymers 0.000 description 8
- 239000005017 polysaccharide Substances 0.000 description 8
- 241000208125 Nicotiana Species 0.000 description 7
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 238000009288 screen filtration Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Abstract
The invention provides a preparation method of a tobacco apple perfume. The preparation method include following steps: 1) crushing apples, adding quercetin and malic acid, performing extraction and filtration to obtain a filter residue and a filtrate; 2) concentrating the filtrate, adding water to the filter residue to perform filtration, and adding an enzymolysis solution, and then filtering and concentrating the mixed liquid; 3) mixing the components obtained after concentration of the filtrate and the filter residue according to proportion, adding propylene glycol, mixing the mixture uniformly and performing filtration; and 4) finally adding esters to obtain the apple perfume. In the method, the tobacco apple perfume maintains the ester substances which have the characteristic fragrances of apples, and organic acids, monosaccharide, polyphenols and the like substances, which achieves excellent effects, from apple is extracted as more as possible. In addition, by means of polysaccharase enzymolysis process, the content of the monosaccharides in the apple perfume is increased further.
Description
Technical field
The present invention relates to a kind of preparation method of tobacco aromatics using, specifically a kind of preparation method of cigarette apple spice.
Background technology
Apple is a kind of fruit that china natural resources is very abundant, and ripe apple, because have graceful comfortable fragrance containing Ester, has and enriches cigarette flavor, cover the effect of cigarette foreign gas in cigarette.The monose, organic acid, polyphenols and the Ester that are rich in apple have simultaneously in cigarette increases flue gas concentration preferably, enrich cigarette perfume (or spice), reduce the effect stimulating and improve mouthfeel.Chinese Patent Application No. 200810073706.5 " a kind of apple extractum and preparation method thereof and the application in perfuming cigarette " directly apple fragmentation is extracted, and this extracting method obtains apple extractum does not have apple fragrance originally, and contents of monosaccharides is low.Chinese Patent Application No. 201310173732.6 " a kind of preparation method of cigarette apple extractum " carries out a series of extraction by after apple fragmentation, and medicinal extract prepared by the method does not have apple fragrance.Chinese Patent Application No. 201110365359.5 " a kind of natural apple essence and preparation method thereof " adds spices after being squeezed the juice by apple to allocate, and the method is difficult to the Ester extracted in apple, and contents of monosaccharides in extracting solution is relatively low.
Summary of the invention
The present invention is exactly the deficiency according to existing in above-mentioned technology of preparing, a kind of preparation method of cigarette apple spice is provided, the standby cigarette apple spice of this legal system remains the Ester of apple characteristic perfume, be extracted in apple organic acid, monose, the polyphenols in cigarette with better effect to greatest extent, and make use of polysaccharide enzymolysis process, increase the content of monose in apple spice further.
The present invention solves the problems of the technologies described above adopted technical scheme: the preparation method providing a kind of cigarette apple spice, comprises the following steps:
(1) make apple pulp by after apple fragmentation, then add the Quercetin of apple pulp weight 0.1 ~ 0.2% and the oxysuccinic acid of 0.1 ~ 0.2%, stir and obtain mixing apple pulp;
(2) add ethanol to ethanol mass percent concentration 80% ~ 90% in the mixing apple pulp obtained to step (1), stirring at normal temperature evenly after, extraction;
Wherein: the composition that can work in cigarette in apple is mainly some Esters, organic acid, polyphenols and monose, these materials can be dissolved in ethanol, contribute maximum Ester boiling point lower to fragrance in these materials, water insoluble, therefore use the alcohol at normal temperature supersound extraction apple pulp of concentration 80%-90%, most of aroma substance in apple can be extracted;
(3) after extraction, filtration obtains first step filtrate and first step filter residue;
(4) the first apple ingredient is obtained by concentrated for the first step filtrate obtained in step (3);
(5) add the water of first step filter residue quality 4 ~ 6 times in the first step filter residue obtained in step (3), be heated to 90 ~ 100 DEG C, stirring, filtration obtain second stage filtrate; Second stage filtrate is cooled to 38 ~ 42 DEG C, add the mixed enzyme solution enzymolysis of first step filter residue quality 0.1 ~ 0.3%, after enzymolysis, add the mass percent concentration of ethanol to ethanol 40 ~ 60%, filtration obtains third stage filtrate, store after 12 ~ 36 hours at 5 ~ 10 DEG C of temperature, filter, concentratedly obtain the second apple ingredient;
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to mass ratio 1:1 ~ 1:6, obtain mixed solution, add the propylene glycol of mixed solution quality 20% ~ 40%, filter after stirring, obtain the 3rd apple ingredient;
Wherein: heated and stirred can promote the dissolving of water-soluble polysaccharide, the solubleness of water-soluble polysaccharide can be improved simultaneously.Thus the content of polysaccharide in solution can be allowed higher, even if having par-tial polysaccharide in the process of low temperature enzymolysis because temperature reduces and separate out, but the polysaccharide of separating out still keeps the state suspended in the solution, still enzymolysis can be participated in, ensure that relatively many water-soluble polysaccharides are hydrolyzed into monose, improve the content of monose in enzymolysis solution, high-temperature stirring can kill the microorganism in solution for 30 minutes in addition, allow in enzymolysis process and there is no microbial reproduction, the acid avoiding the amount reproduction because of various microorganism to produce reduces the pH value of solution, thus have impact on the activity of enzyme, reduce enzymolysis efficiency,
(7) add ester class in the 3rd apple ingredient obtained in step (6), after stirring, obtain cigarette apple spice.
Further, in described step (4), thickening temperature is 45 ~ 60 DEG C, and first step filtrate is concentrated into density 1.1 ± 0.05g/cm
3.
Further, the filtration detailed process in described step (5) before enzymolysis is: filter with aperture 20 ~ 60 object screen cloth, then use the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, obtain second stage filtrate; Filtration procedure after enzymolysis is: filter with aperture 20 ~ 60 object screen cloth, then the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, aperture is used, obtain third stage filtrate, 5 ~ 10 DEG C of storages are after 12 ~ 36 hours, with the membrane filtration in 0.7 ~ 0.9 μm, aperture, thus at utmost retain the fragrance in apple.
Further, the filtration detailed process of described step (3) is: filter with aperture 20 ~ 60 object screen cloth, then uses the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, obtains first step filtrate.
Further, in described step (5), the third stage filtrate obtained is concentrated into density 1.2 ± 0.05g/cm after filtering
3.
Further, the enzymolysis process in described step (5) is: add mixed enzyme solution, ultrasonic enzymolysis 2 ~ 4 hours, temperature 38 DEG C ~ 42 DEG C; Wherein, in enzymolysis process, carry out ultrasound-assisted enzymolysis, can increase enzyme and polysaccharide in conjunction with probability, improve enzymolysis efficiency.
Further, in described step (2) and step (5), ethanol used is the food-grade ethanol of mass concentration 95%.
Further, in described step (5), mixed enzyme solution is the mixed enzyme solution of chitoanase, cellulase, amylase, proteolytic enzyme.
Further, in described step (7) ester class be account for the 3rd apple ingredient quality 0.2 ~ 0.7% isoamyl isovalerate, 0.5 ~ 1.0% Ethylisovalerate, the ethyl acetate of 0.1 ~ 0.3%, the ethyl butyrate mixing of 0.1 ~ 0.5%, adding mixed ester class makes apple feature fruital more obvious, and fragrance is more plentiful true to nature.
A kind of cigarette apple spice, the cigarette apple spice that described cigarette apple spice is prepared for the preparation method of cigarette apple spice described in above-mentioned any one.
The present invention has following characteristics: cigarette apple spice prepared by the present invention is rich in abundant monose, organic acid, polyphenols and Ester, has obvious apple fragrance; Add ester class to stir, natural cigarette apple spice can be obtained, make apple feature fruital more obvious, and fragrance is more plentiful true to nature.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
Embodiment 1
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.1% and the oxysuccinic acid of 0.2%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 85%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 20 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 100nm aperture, obtain the first step filtrate of clarifying, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out vacuum concentration, thickening temperature 50 DEG C, being concentrated into density is 1.15g/cm
3, obtain the first apple ingredient;
(5) step (3) is merged the pure water adding 4 times of quality in the first step filter residue obtained, be heated to 95 DEG C and stir 30 minutes.Tentatively filter with aperture 20 object screen cloth while hot, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the second stage filtrate of clarifying, be cooled to 40 DEG C, add the mixed enzyme solution that step (3) merges the chitoanase of the first step filter residue quality 0.1-0.3% obtained, cellulase, amylase, proteolytic enzyme, ultrasonic enzymolysis 4 hours, control temperature is constant in 40 DEG C.After enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 20 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 5 DEG C of low-temperature storage, after 24 hours, are filtered with the filter membrane in 0.8 μm, aperture, and being concentrated into density is 1.25g/cm
3, obtain the second apple ingredient;
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to 1:4, obtain mixed solution, add the propylene glycol of mixed solution massfraction 20%, filter with the filter membrane in 0.8 μm, aperture after stirring, obtain the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.2%, Ethylisovalerate 0.5%, ethyl acetate 0.1%, the ethyl butyrate 0.1% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
Embodiment 2
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.2% and the oxysuccinic acid of 0.1%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 90%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 40 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 100nm aperture, obtain first step filtrate, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out vacuum concentration, thickening temperature 55 DEG C, being concentrated into density is 1.14g/cm
3, obtain the first apple ingredient.(5) step (3) is merged the pure water adding 6 times of quality in the first step filter residue obtained, be heated to 90 DEG C and stir 30 minutes.Tentatively filter with aperture 40 object screen cloth while hot, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain second stage filtrate, be cooled to 38 DEG C, add the mixed enzyme solution that step (3) merges the chitoanase of the filter residue quality 0.2% obtained, cellulase, amylase, proteolytic enzyme, ultrasonic enzymolysis 2-4 hour, control temperature is constant in 38 DEG C.After enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 40 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 6 DEG C of low-temperature storage, after 24 hours, are filtered with the filter membrane in 0.8 μm, aperture, and being concentrated into density is 1.23g/cm
3, obtain the second apple ingredient;
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to 1:3, add the propylene glycol of mixed solution massfraction 25%, filter with the filter membrane in 0.8 μm, aperture after stirring, obtain natural cigarette the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.3%, Ethylisovalerate 0.6%, ethyl acetate 0.2%, the ethyl butyrate 0.2% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
Embodiment 3
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.2% and the oxysuccinic acid of 0.1%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 90%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 40 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 100nm aperture, obtain the first step filtrate of clarifying, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out vacuum concentration, thickening temperature 55 DEG C, being concentrated into density is 1.1g/cm
3, obtain the first apple ingredient;
(5) step (3) is merged the pure water adding 6 times of quality in the first step filter residue obtained, be heated to 90 DEG C and stir 30 minutes.Tentatively filter with aperture 40 object screen cloth while hot, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the second stage filtrate of clarifying, be cooled to 38 DEG C, add the mixed enzyme solution that step (3) merges the chitoanase of the first step filter residue quality 0.2% obtained, cellulase, amylase, proteolytic enzyme, ultrasonic enzymolysis 3 hours, control temperature is constant in 38 DEG C.After enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 30 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 6 DEG C of low-temperature storage, after 24 hours, are filtered with the filter membrane in 0.8 μm, aperture, and being concentrated into density is 1.2g/cm
3, obtain the second apple ingredient;
(6) the first apple ingredient and the second apple ingredient are carried out being mixed to get mixed solution according to the ratio of 1:3, add the propylene glycol of mixed solution massfraction 25%, filter with the filter membrane in 0.8 μm, aperture after stirring, obtain natural cigarette the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.3%, Ethylisovalerate 0.6%, ethyl acetate 0.2%, the ethyl butyrate 0.2% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
Embodiment 4
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.2% and the oxysuccinic acid of 0.1%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 90%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 40 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 100nm aperture, obtain the first step filtrate of clarifying, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out vacuum concentration, thickening temperature 55 DEG C, being concentrated into density is 1.08g/cm
3, obtain the first apple ingredient;
(5) step (3) is merged the pure water adding 6 times of quality in the first step filter residue obtained, be heated to 90 DEG C and stir 30 minutes.Tentatively filter with aperture 40 object screen cloth while hot, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the second stage filtrate of clarifying, be cooled to 38 DEG C, add the mixed enzyme solution that step (3) merges the chitoanase of the first step filter residue quality 0.2% obtained, cellulase, amylase, proteolytic enzyme, ultrasonic enzymolysis 2 hours, control temperature is constant in 38 DEG C.After enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 40 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 6 DEG C of low-temperature storage, after 24 hours, are filtered with the filter membrane in 0.8 μm, aperture, and being concentrated into density is 1.16g/cm
3, obtain the second apple ingredient;
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to 1:4, add the propylene glycol of mixed solution massfraction 25%, filter with the filter membrane in 0.8 μm, aperture after stirring, obtain natural cigarette the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.3%, Ethylisovalerate 0.6%, ethyl acetate 0.2%, the ethyl butyrate 0.2% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
Embodiment 5
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.2% and the oxysuccinic acid of 0.2%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 85%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 40 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 110nm aperture, obtain the first step filtrate of clarifying, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out vacuum concentration, thickening temperature 50 DEG C, being concentrated into density is 1.11g/cm
3, obtain the first apple ingredient;
(5) step (3) is merged the pure water adding 6 times of quality in the filter residue obtained, be heated to 90 DEG C stir 30 minutes, tentatively filter with aperture 40 object screen cloth while hot, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the second stage filtrate of clarifying, be cooled to 40 DEG C, add the chitoanase that step (3) merges the first step filter residue quality 0.2% obtained, cellulase, amylase, the mixed enzyme solution of proteolytic enzyme, ultrasonic enzymolysis 3 hours, control temperature is constant in 38 DEG C, after enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 50 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 8 DEG C of low-temperature storage are after 24 hours, filter with the filter membrane in 0.8 μm, aperture, being concentrated into density is 1.16g/cm
3, obtain the second apple ingredient,
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to 1:4, add the propylene glycol of mixed solution massfraction 25%, filter with the filter membrane in 0.8 μm, aperture after stirring, obtain natural cigarette the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.3%, Ethylisovalerate 0.6%, ethyl acetate 0.2%, the ethyl butyrate 0.2% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
Embodiment 6
(1) make apple pulp by after selected transparent apple Mechanical Crushing, then add the Quercetin of apple weight 0.2% and the oxysuccinic acid of 0.2%, stir immediately;
(2) add the food-grade ethanol of 95% in the apple pulp stirred in step (1), make the concentration of final ethanol control 80%, stirring at normal temperature, after 30 minutes, carries out ultrasonic extraction 30 minutes;
(3) tentatively filter with aperture 40 object screen cloth after ultrasonic extraction, then use the inorganic ceramic membrane filtration in 100nm aperture, obtain the first step filtrate of clarifying, then merge the first step filter residue that screen filtration and ceramic membrane filter obtain;
(4) first step filtrate obtained in step (3) is carried out cryogenic vacuum to concentrate, thickening temperature 50 DEG C, being concentrated into density is 1.13g/cm
3, obtain the first apple ingredient;
(5) step (3) is merged the pure water adding 6 times of quality in the first step filter residue obtained, be heated to 90 DEG C stir 30 minutes, tentatively filter with aperture 40 object screen cloth while hot, then the inorganic ceramic membrane filtration in 110nm aperture is used, obtain the second stage filtrate of clarifying, be cooled to 40 DEG C, add the chitoanase that step (3) merges the filter residue quality 0.2% obtained, cellulase, amylase, the mixed enzyme solution of proteolytic enzyme, ultrasonic enzymolysis 4 hours, control temperature is constant in 40 DEG C, after enzymolysis, the food-grade ethanol adding concentration 95% in filtrate makes the final concentration of ethanol control 50%, tentatively filter with aperture 50 object screen cloth, then the inorganic ceramic membrane filtration in 100nm aperture is used, obtain the third stage filtrate of clarifying, 8 DEG C of low-temperature storage are after 24 hours, filter with the filter membrane in 0.9 μm, aperture, being concentrated into density is 1.15g/cm
3, obtain the second apple ingredient,
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to 1:5, add the propylene glycol of mixed solution massfraction 25%, filter with the filter membrane in 0.9 μm, aperture after stirring, obtain natural cigarette the 3rd apple ingredient;
(7) add isoamyl isovalerate 0.3%, Ethylisovalerate 0.6%, ethyl acetate 0.2%, the ethyl butyrate 0.2% of natural origin in natural 3rd apple ingredient obtained in step 6, stir and namely obtain final natural tobacco apple spice.
The above; be only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly belongs to those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claim.
Claims (10)
1. a preparation method for cigarette apple spice, is characterized in that: comprise the following steps:
(1) make apple pulp by after apple fragmentation, then add the Quercetin of apple pulp weight 0.1 ~ 0.2% and the oxysuccinic acid of 0.1 ~ 0.2%, stir and obtain mixing apple pulp;
(2) add ethanol to ethanol mass percent concentration 80% ~ 90% in the mixing apple pulp obtained to step (1), stirring at normal temperature evenly after, extraction;
(3) after extraction, filtration obtains first step filtrate and first step filter residue;
(4) the first apple ingredient is obtained by concentrated for the first step filtrate obtained in step (3);
(5) add the water of first step filter residue quality 4 ~ 6 times in the first step filter residue obtained in step (3), be heated to 90 ~ 100 DEG C, stirring, filtration obtain second stage filtrate; Second stage filtrate is cooled to 38 ~ 42 DEG C, add the mixed enzyme solution enzymolysis of first step filter residue quality 0.1 ~ 0.3%, after enzymolysis, add the mass percent concentration of ethanol to ethanol 40 ~ 60%, filtration obtains third stage filtrate, store after 12 ~ 36 hours at 5 ~ 10 DEG C of temperature, filter, concentratedly obtain the second apple ingredient;
(6) the first apple ingredient is mixed with the ratio of the second apple ingredient according to mass ratio 1:1 ~ 1:6, obtain mixed solution, add the propylene glycol of mixed solution quality 20% ~ 40%, filter after stirring, obtain the 3rd apple ingredient;
(7) add ester class in the 3rd apple ingredient obtained in step (6), after stirring, obtain cigarette apple spice.
2. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: in described step (4), thickening temperature is 45 ~ 60 DEG C, and first step filtrate is concentrated into density 1.1 ± 0.05g/cm
3.
3. the preparation method of a kind of cigarette apple spice according to claim 1, it is characterized in that: the filtration detailed process in described step (5) before enzymolysis is: filter with aperture 20 ~ 60 object screen cloth, then use the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, obtain second stage filtrate; Filtration procedure after enzymolysis is: filter with aperture 20 ~ 60 object screen cloth, then uses the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, aperture, obtains third stage filtrate, and 5 ~ 10 DEG C store after 12 ~ 36 hours, with the membrane filtration in 0.7 ~ 0.9 μm, aperture.
4. the preparation method of a kind of cigarette apple spice according to claim 1, it is characterized in that: the filtration detailed process of described step (3) is: filter with aperture 20 ~ 60 object screen cloth, then use the inorganic ceramic membrane filtration in 90 ~ 110nm aperture, obtain first step filtrate.
5. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: in described step (5), and the third stage filtrate obtained is concentrated into density 1.2 ± 0.05g/cm after filtering
3.
6. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: the enzymolysis process in described step (5) is: add mixed enzyme solution, ultrasonic enzymolysis 2 ~ 4 hours, temperature 38 DEG C ~ 42 DEG C.
7. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: in described step (2) and step (5), ethanol used is the food-grade ethanol of mass concentration 95%.
8. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: in described step (5), mixed enzyme solution is the mixed enzyme solution of chitoanase, cellulase, amylase, proteolytic enzyme.
9. the preparation method of a kind of cigarette apple spice according to claim 1, is characterized in that: in described step (7) ester class be account for the 3rd apple ingredient quality 0.2 ~ 0.7% isoamyl isovalerate, 0.5 ~ 1.0% Ethylisovalerate, the ethyl acetate of 0.1 ~ 0.3%, the ethyl butyrate mixing of 0.1 ~ 0.5%.
10. a cigarette apple spice, is characterized in that: the cigarette apple spice that described cigarette apple spice is prepared for the preparation method of cigarette apple spice described in claim 1 ~ 9 any one.
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| CN113907394A (en) * | 2021-09-28 | 2022-01-11 | 深圳市真味生物科技有限公司 | Preparation method of apple extract for cigarettes |
| CN114874855A (en) * | 2022-06-15 | 2022-08-09 | 河南省新郑金叶香料有限公司 | Preparation method of grape extract essence and application of grape extract essence in cigarettes |
| CN115624204A (en) * | 2022-11-07 | 2023-01-20 | 广西中烟工业有限责任公司 | Apple spice for cigarettes and application thereof |
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