CN101731749A - Ultrasonic zymohydrolysis extracting method for extracting tobacco perfumes from chrysanthemum natural plant flowers - Google Patents
Ultrasonic zymohydrolysis extracting method for extracting tobacco perfumes from chrysanthemum natural plant flowers Download PDFInfo
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- CN101731749A CN101731749A CN200810197538A CN200810197538A CN101731749A CN 101731749 A CN101731749 A CN 101731749A CN 200810197538 A CN200810197538 A CN 200810197538A CN 200810197538 A CN200810197538 A CN 200810197538A CN 101731749 A CN101731749 A CN 101731749A
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- 241000196324 Embryophyta Species 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 18
- 235000007516 Chrysanthemum Nutrition 0.000 title claims abstract description 13
- 235000002637 Nicotiana tabacum Nutrition 0.000 title claims abstract description 9
- 239000002304 perfume Substances 0.000 title abstract description 4
- 244000189548 Chrysanthemum x morifolium Species 0.000 title abstract 2
- 244000061176 Nicotiana tabacum Species 0.000 title 1
- 239000000284 extract Substances 0.000 claims abstract description 41
- 108090000790 Enzymes Proteins 0.000 claims abstract description 36
- 102000004190 Enzymes Human genes 0.000 claims abstract description 36
- 229940088598 enzyme Drugs 0.000 claims abstract description 25
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 15
- 108010059892 Cellulase Proteins 0.000 claims abstract description 11
- 229940106157 cellulase Drugs 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000001471 micro-filtration Methods 0.000 claims abstract description 9
- 241000208125 Nicotiana Species 0.000 claims abstract description 8
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 7
- 238000009776 industrial production Methods 0.000 claims abstract description 3
- 235000012054 meals Nutrition 0.000 claims description 22
- 239000000706 filtrate Substances 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 12
- 241000723353 Chrysanthemum Species 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 2
- -1 pectase Proteins 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000004480 active ingredient Substances 0.000 abstract description 11
- 238000000605 extraction Methods 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000000843 powder Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 12
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 8
- 229930003944 flavone Natural products 0.000 description 8
- 150000002212 flavone derivatives Chemical class 0.000 description 8
- 235000011949 flavones Nutrition 0.000 description 8
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 8
- 239000007788 liquid Substances 0.000 description 6
- 239000008363 phosphate buffer Substances 0.000 description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 240000005250 Chrysanthemum indicum Species 0.000 description 5
- 235000018959 Chrysanthemum indicum Nutrition 0.000 description 5
- 241001252564 Chrysopsis Species 0.000 description 5
- 241000628997 Flos Species 0.000 description 5
- 238000002955 isolation Methods 0.000 description 5
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 description 5
- 230000002255 enzymatic effect Effects 0.000 description 3
- 241001292339 Adenandra uniflora Species 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000000909 electrodialysis Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
Abstract
The invention discloses an ultrasonic zymohydrolysis extracting method for extracting tobacco perfumes from chrysanthemum natural plant flowers, which belongs to the technical field of a tobacco perfume extracting method. The ultrasonic zymohydrolysis extracting method comprises the following steps of: (1) preparing into crude powder with the fineness smaller than 20 meshes; (2) adding 1-3% of compound enzyme solution into a phosphate buffer solution with the pH value of 3.5-4.5; (3) performing zymohydrolysis for 10-30 minutes on the mixing liquor by 20 kHz ultrasonic waves; (4) leading filter liquor respectively to pass through microfiltration membranes of 0.65 micrometer and 0.45 micrometer and nanometer filtration membranes with the molecular weight of 3000. The obtained transparent filter liquor is an extract. The cellulase, pectase and protein enzyme are industrial production enzymes, but not biological enzymes. The method is simple, the active ingredients in natural plants can be completely extracted, and the industrial implementation is easy. The maximum time of ultrasonic zymohydrolysis extraction is 30 minutes, thus the time and energy consumption are greatly saved.
Description
Technical field
The invention belongs to tobacco aromatics using extracting method technical field, is at the pluses and minuses of prior art cigarette with the extracting method of perfume material specifically, in addition improved new ultrasonic zymohydrolysis extracting method.
Background technology
In the prior art, the contained complex chemical composition of natural plants contains plurality of active ingredients.Active ingredient in the plant need extract from the homogeneous phase of complexity or heterogeneous system, then by separating and removing impurity and finish and purify and refining.Some traditional isolation technics such as filtration, sedimentation, centrifugation, distillation, extraction, chromatography, crystallization, absorption, molecular clock, ultrafiltration, electrodialysis, counter-infiltration etc. are longer as the means history that effective ingredients in plant separates, and use more; And some isolation technics that newly-developed gets up having obvious superiority aspect selectivity, operating efficiency, the energy-conservation and environmental protection, demonstrate great application prospect as enzymatic isolation method, ultrasonic extraction and NF membrane partition method or the like.But these methods are carrying out also there are some problems when suitability for industrialized production is used, and, energy consumption long as enzymolysis time is big or the like.The shortest time of general enzymolysis is more than 3-4 hour, and is consuming time longer, needs the certain temperature of maintenance, needs the energy consumption of heating bigger, and production cost is higher.
Summary of the invention
Above-mentioned deficiency at prior art, the technical problem to be solved in the present invention provides a kind of ultrasonic zymohydrolysis extracting method that extracts tobacco aromatics using from chrysanthemum material natural plant flowers, it can shorten extraction time, energy efficient, and can improve the yield and the active constituent content of extract.
Technical scheme of the present invention is: the ultrasonic zymohydrolysis extracting method step in the following sequence of extracting tobacco aromatics using from chrysanthemum material natural plant flowers is extracted:
(1), chrysanthemum material natural plant flowers to be extracted is ground into particle diameter less than 20 purpose meal;
(2), in pH is 3.5～4.5 phosphate buffer solution, add 1～3% composite enzyme solution, described complex enzyme is a cellulase: pectase: protein enzyme=2: 1: 1;
(3), with the chrysanthemum material natural plant flowers meal of pulverizing: the above-mentioned pH that is added with complex enzyme is 3.5～4.5 a phosphate buffer solution=1: 10, the pH that is added with complex enzyme that will prepare while stirring is that 3.5～4.5 phosphate buffer solution joins in the chrysanthemum material natural plant flowers meal and forms mixed liquor, the mixed liquor temperature is controlled at 37 ± 0.5 ℃, above-mentioned mixed liquor is put into the ultrasonic wave extractor, enzymolysis 10～30min under the 20KHz ultrasonic wave;
(4), with the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
Described cellulase, pectase, protein enzyme are the industrial production enzyme; And unorganized ferment.
Method of the present invention is simple, can extract fully active ingredients in natural plants, and less energy consumption, industrializing implementation is easy.The ultrasonic enzymolysis and extraction time of the present invention is the longest to be 30 minutes, has saved time and energy consumption greatly.
The specific embodiment
Below embodiments of the invention are described:
Embodiment 1.
Spend 2 kilograms with Dendranthema indicum are ground into meal, cross 20 mesh sieves; The pH that preparation contains 1.2% composite enzyme solution is 20 kilograms of 4.5 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; While stirring the cushioning liquid of preparation is joined during the Dendranthema indicum that is ground into meal spends, water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 15min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate is 3000 NF membrane successively again by 0.65 μ m, 0.45 μ m micro-filtration membrane and molecular weight, and the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 14.29%, analyzes with ultraviolet-visible spectrophotometry, and the active ingredient content of total flavone is 6.55% in the calculating extract.
Embodiment 2.
Spend 2 kilograms with Dendranthema indicum are ground into meal, cross 20 mesh sieves; The pH that preparation contains 1.5% composite enzyme solution is 20 kilograms of 4.5 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; While stirring the cushioning liquid of preparation is joined during the Dendranthema indicum that is ground into meal spends, water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 15min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate is 3000 NF membrane successively again by 0.65 μ m, 0.45 μ m micro-filtration membrane and molecular weight, and the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 15.89%, analyzes with ultraviolet-visible spectrophotometry, and the active ingredient content of total flavone is 7.12% in the calculating extract.
Embodiment 3.
Spend 2 kilograms with golden aster are ground into meal, cross 20 mesh sieves; The pH that preparation contains 2% composite enzyme solution is 20 kilograms of 3.5 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; Cushioning liquid with preparation joins in the meal of the golden aster that is ground into meal while stirring, and water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 10min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 15.38%, analyzes with ultraviolet-visible spectrophotometry, and the active ingredient content of total flavone is 6.05% in the calculating extract.
Embodiment 4.
Spend 2 kilograms with golden aster are ground into meal, cross 20 mesh sieves; The pH that preparation contains 2% composite enzyme solution is 20 kilograms of 3.5 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; Cushioning liquid with preparation joins in the meal of the golden aster that is ground into meal while stirring, and water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 20min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the coarse filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 16.57%, analyzes with ultraviolet-visible spectrophotometry, calculates active ingredient content of total flavone in the extract, is 6.73%.
Embodiment 5.
Spend 2 kilograms with FLOS CHRYSANTHEMI ALBA from Haizhou of China are ground into meal, cross 20 mesh sieves; The pH that preparation contains 2.5% composite enzyme solution is 20 kilograms of 3.8 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; Cushioning liquid with preparation joins in the FLOS CHRYSANTHEMI ALBA from Haizhou of China flower meal that is ground into meal while stirring, and water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 25min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 15.10%, analyzes with ultraviolet-visible spectrophotometry, calculates active ingredient content of total flavone in the extract, is 6.76%.
Embodiment 6.
Spend 2 kilograms with FLOS CHRYSANTHEMI ALBA from Haizhou of China are ground into meal, cross 20 mesh sieves; The pH that preparation contains 2.5% composite enzyme solution is 20 kilograms of 4.5 phosphate buffer solutions, and wherein the proportioning of complex enzyme is, cellulase: pectase: protein enzyme=2: 1: 1; Cushioning liquid with preparation joins in the FLOS CHRYSANTHEMI ALBA from Haizhou of China flower meal that is ground into meal while stirring, and water temperature is controlled at 37 ± 0.5 ℃, places the ultrasonic wave extractor, with the ultrasonic enzymolysis 25min of 20KHz; With the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
With this extract simmer down to medicinal extract shape, yield is 16.21%, analyzes with ultraviolet-visible spectrophotometry, calculates active ingredient content of total flavone in the extract, is 7.68%.
From the foregoing description the relevant technologies problem is described in further detail.The applicant carries out conventional enzymolysis processing to Dendranthema indicum, golden aster and FLOS CHRYSANTHEMI ALBA from Haizhou of China and extracts and conventional ultrasonic extraction, handle extract and analyze according to the conventional method of prior art, result of calculation shows that its yield of extract is 9.08%～15.10%, and general flavone content is 4.78%～6.89%.The extract that obtains with ultrasonic enzymatic isolation method in the above-described embodiments, in order to compare with prior art, extract made to calculate yield of extract behind the medicinal extract be 14.29%～16.57%, general flavone content is 6.05%～7.68%, all be higher than conventional extracting method gained, therefore, ultrasonic enzymatic isolation method can be used for the extraction of other active ingredient of natural plant also than prior art suitable advantage being arranged aspect extraction yield and the active constituent content.
Claims (2)
1. ultrasonic zymohydrolysis extracting method that from chrysanthemum material natural plant flowers, extracts tobacco aromatics using, it is characterized in that: described extracting method step is in the following sequence extracted:
(1), chrysanthemum material natural plant flowers to be extracted is ground into particle diameter less than 20 purpose meal;
(2), in pH is 3.5～4.5 phosphate buffer solution, add 1～3% composite enzyme solution, described complex enzyme is a cellulase: pectase: protein enzyme=2: 1: 1;
(3), with the chrysanthemum material natural plant flowers meal of pulverizing: the above-mentioned pH that is added with complex enzyme is 3.5～4.5 a phosphate buffer solution=1: 10, the pH that is added with complex enzyme that will prepare while stirring is that 3.5～4.5 phosphate buffer solution joins in the chrysanthemum material natural plant flowers meal and forms mixed liquor, the mixed liquor temperature is controlled at 37 ± 0.5 ℃, above-mentioned mixed liquor is put into the ultrasonic wave extractor, enzymolysis 10～30min under the 20KHz ultrasonic wave;
(4), with the mixed liquor behind the ultrasonic enzymolysis, after the filtration, filtrate successively again micro-filtration membrane by 0.65 μ m, 0.45 μ m and molecular weight be 3000 NF membrane, the transparent filtrate of gained is extract.
2. the ultrasonic zymohydrolysis extracting method that extracts tobacco aromatics using from chrysanthemum material natural plant flowers according to claim 1, it is characterized in that: described cellulase, pectase, protein enzyme are the industrial production enzyme.
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| CN102653703A (en) * | 2011-03-01 | 2012-09-05 | 湖北中烟工业有限责任公司 | Top dressing flavor for improving influence of Chinese herbal medicine extract on cigarette taste |
| CN103060091A (en) * | 2012-12-14 | 2013-04-24 | 湖北中烟工业有限责任公司 | Preparation method of feltwort extract |
| CN103497838A (en) * | 2013-10-24 | 2014-01-08 | 洛阳祥和牡丹科技有限公司 | Method for extracting peony essential oil from peonies |
| CN103750546A (en) * | 2014-01-15 | 2014-04-30 | 红云红河烟草(集团)有限责任公司 | Tobacco ageing method by blending tobacco with lavender and marigolds |
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| CN106753790A (en) * | 2016-12-05 | 2017-05-31 | 湖北中烟工业有限责任公司 | Uniform, stable tobacco aromaticss of fragrance and preparation method thereof |
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| CN102653703B (en) * | 2011-03-01 | 2013-07-17 | 湖北中烟工业有限责任公司 | Top dressing flavor for improving influence of Chinese herbal medicine extract on cigarette taste |
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| CN104212625A (en) * | 2014-07-14 | 2014-12-17 | 和县绿源油脂有限公司 | Method for extracting grease through caraway |
| CN104357215A (en) * | 2014-10-22 | 2015-02-18 | 浙江中烟工业有限责任公司 | Selenium-rich tea tobacco flavor, preparation method of selenium-rich tea tobacco flavor and application of selenium-rich tea tobacco flavor to cigarette preparation |
| CN104357215B (en) * | 2014-10-22 | 2017-08-29 | 浙江中烟工业有限责任公司 | A kind of selenium-enriched tea leaf tobacco aromaticss and preparation method thereof and the application in cigarette preparation |
| CN105087160A (en) * | 2015-08-20 | 2015-11-25 | 嘉兴景程生物科技有限公司 | Camomile tobacco flavor as well as preparation method and application thereof |
| CN106753790A (en) * | 2016-12-05 | 2017-05-31 | 湖北中烟工业有限责任公司 | Uniform, stable tobacco aromaticss of fragrance and preparation method thereof |
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| CN101731749B (en) | 2012-06-13 |
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