CN107987972B - Preparation method and application of robinia pseudoacacia flower extract - Google Patents
Preparation method and application of robinia pseudoacacia flower extract Download PDFInfo
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- CN107987972B CN107987972B CN201711274714.1A CN201711274714A CN107987972B CN 107987972 B CN107987972 B CN 107987972B CN 201711274714 A CN201711274714 A CN 201711274714A CN 107987972 B CN107987972 B CN 107987972B
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- 241001493421 Robinia <trematode> Species 0.000 title claims abstract description 95
- 239000000284 extract Substances 0.000 title claims abstract description 78
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 45
- 235000019504 cigarettes Nutrition 0.000 claims abstract description 24
- HNZUNIKWNYHEJJ-FMIVXFBMSA-N geranyl acetone Chemical compound CC(C)=CCC\C(C)=C\CCC(C)=O HNZUNIKWNYHEJJ-FMIVXFBMSA-N 0.000 claims abstract description 16
- HNZUNIKWNYHEJJ-UHFFFAOYSA-N geranyl acetone Natural products CC(C)=CCCC(C)=CCCC(C)=O HNZUNIKWNYHEJJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000019719 rose oil Nutrition 0.000 claims abstract description 16
- 239000010666 rose oil Substances 0.000 claims abstract description 16
- 235000010254 Jasminum officinale Nutrition 0.000 claims abstract description 15
- 239000010648 geranium oil Substances 0.000 claims abstract description 15
- 235000019717 geranium oil Nutrition 0.000 claims abstract description 15
- VWMVAQHMFFZQGD-UHFFFAOYSA-N p-Hydroxybenzyl acetone Natural products CC(=O)CC1=CC=C(O)C=C1 VWMVAQHMFFZQGD-UHFFFAOYSA-N 0.000 claims abstract description 15
- NJGBTKGETPDVIK-UHFFFAOYSA-N raspberry ketone Chemical compound CC(=O)CCC1=CC=C(O)C=C1 NJGBTKGETPDVIK-UHFFFAOYSA-N 0.000 claims abstract description 15
- JLIDRDJNLAWIKT-UHFFFAOYSA-N 1,2-dimethyl-3h-benzo[e]indole Chemical compound C1=CC=CC2=C(C(=C(C)N3)C)C3=CC=C21 JLIDRDJNLAWIKT-UHFFFAOYSA-N 0.000 claims abstract description 14
- DULCUDSUACXJJC-UHFFFAOYSA-N benzeneacetic acid ethyl ester Natural products CCOC(=O)CC1=CC=CC=C1 DULCUDSUACXJJC-UHFFFAOYSA-N 0.000 claims abstract description 14
- POIARNZEYGURDG-FNORWQNLSA-N beta-damascenone Chemical compound C\C=C\C(=O)C1=C(C)C=CCC1(C)C POIARNZEYGURDG-FNORWQNLSA-N 0.000 claims abstract description 14
- 229930007850 β-damascenone Natural products 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 238000002156 mixing Methods 0.000 claims abstract description 9
- AAANUTWSKMHKQS-UHFFFAOYSA-N 2,6,10-trimethyldodecanal Chemical compound CCC(C)CCCC(C)CCCC(C)C=O AAANUTWSKMHKQS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 241000219784 Sophora Species 0.000 claims abstract description 6
- 240000005385 Jasminum sambac Species 0.000 claims abstract 4
- 238000000605 extraction Methods 0.000 claims description 30
- 239000000843 powder Substances 0.000 claims description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 238000010992 reflux Methods 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 14
- 239000003921 oil Substances 0.000 claims description 14
- 235000019198 oils Nutrition 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 125000005456 glyceride group Chemical group 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 8
- LTUMRKDLVGQMJU-IUBLYSDUSA-N farnesyl acetone Chemical compound CC(C)=CCC\C(C)=C\CC\C(C)=C\CCC(C)=O LTUMRKDLVGQMJU-IUBLYSDUSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000012528 membrane Substances 0.000 claims description 7
- 244000046101 Sophora japonica Species 0.000 claims description 6
- 235000010586 Sophora japonica Nutrition 0.000 claims description 6
- LTUMRKDLVGQMJU-UHFFFAOYSA-N famesylacetone Natural products CC(C)=CCCC(C)=CCCC(C)=CCCC(C)=O LTUMRKDLVGQMJU-UHFFFAOYSA-N 0.000 claims description 6
- 244000061176 Nicotiana tabacum Species 0.000 claims description 5
- 235000002637 Nicotiana tabacum Nutrition 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000003085 diluting agent Substances 0.000 claims description 2
- 235000013305 food Nutrition 0.000 claims description 2
- 239000003205 fragrance Substances 0.000 abstract description 40
- 235000009508 confectionery Nutrition 0.000 abstract description 31
- 241000207840 Jasminum Species 0.000 description 11
- 239000000287 crude extract Substances 0.000 description 8
- 239000000796 flavoring agent Substances 0.000 description 6
- 235000019634 flavors Nutrition 0.000 description 6
- 241000628997 Flos Species 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000000341 volatile oil Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000001953 sensory effect Effects 0.000 description 4
- 240000007472 Leucaena leucocephala Species 0.000 description 3
- 235000010643 Leucaena leucocephala Nutrition 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- WRMNZCZEMHIOCP-UHFFFAOYSA-N 2-phenylethanol Chemical compound OCCC1=CC=CC=C1 WRMNZCZEMHIOCP-UHFFFAOYSA-N 0.000 description 2
- GLZPCOQZEFWAFX-UHFFFAOYSA-N Geraniol Chemical compound CC(C)=CCCC(C)=CCO GLZPCOQZEFWAFX-UHFFFAOYSA-N 0.000 description 2
- 241000745768 Pluchea carolinensis Species 0.000 description 2
- 239000013068 control sample Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 2
- 235000012907 honey Nutrition 0.000 description 2
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- FQTLCLSUCSAZDY-UHFFFAOYSA-N (+) E(S) nerolidol Natural products CC(C)=CCCC(C)=CCCC(C)(O)C=C FQTLCLSUCSAZDY-UHFFFAOYSA-N 0.000 description 1
- 239000001490 (3R)-3,7-dimethylocta-1,6-dien-3-ol Substances 0.000 description 1
- CDOSHBSSFJOMGT-JTQLQIEISA-N (R)-linalool Natural products CC(C)=CCC[C@@](C)(O)C=C CDOSHBSSFJOMGT-JTQLQIEISA-N 0.000 description 1
- TUSDEZXZIZRFGC-UHFFFAOYSA-N 1-O-galloyl-3,6-(R)-HHDP-beta-D-glucose Natural products OC1C(O2)COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC1C(O)C2OC(=O)C1=CC(O)=C(O)C(O)=C1 TUSDEZXZIZRFGC-UHFFFAOYSA-N 0.000 description 1
- BGTBFNDXYDYBEY-FNORWQNLSA-N 4-(2,6,6-Trimethylcyclohex-1-enyl)but-2-en-4-one Chemical compound C\C=C\C(=O)C1=C(C)CCCC1(C)C BGTBFNDXYDYBEY-FNORWQNLSA-N 0.000 description 1
- 206010013911 Dysgeusia Diseases 0.000 description 1
- 239000001263 FEMA 3042 Substances 0.000 description 1
- 241000220485 Fabaceae Species 0.000 description 1
- 206010016322 Feeling abnormal Diseases 0.000 description 1
- 239000005792 Geraniol Substances 0.000 description 1
- GLZPCOQZEFWAFX-YFHOEESVSA-N Geraniol Natural products CC(C)=CCC\C(C)=C/CO GLZPCOQZEFWAFX-YFHOEESVSA-N 0.000 description 1
- 235000006679 Mentha X verticillata Nutrition 0.000 description 1
- 235000002899 Mentha suaveolens Nutrition 0.000 description 1
- 235000001636 Mentha x rotundifolia Nutrition 0.000 description 1
- FQTLCLSUCSAZDY-ATGUSINASA-N Nerolidol Chemical compound CC(C)=CCC\C(C)=C\CC[C@](C)(O)C=C FQTLCLSUCSAZDY-ATGUSINASA-N 0.000 description 1
- LRBQNJMCXXYXIU-PPKXGCFTSA-N Penta-digallate-beta-D-glucose Natural products OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-PPKXGCFTSA-N 0.000 description 1
- 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 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229930003944 flavone Natural products 0.000 description 1
- 150000002212 flavone derivatives Chemical class 0.000 description 1
- 235000011949 flavones Nutrition 0.000 description 1
- 229940113087 geraniol Drugs 0.000 description 1
- BAWIJQDONYVQRF-UHFFFAOYSA-N geranylfarnesylacetone Natural products CC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=CCCC(C)=O BAWIJQDONYVQRF-UHFFFAOYSA-N 0.000 description 1
- 229930182478 glucoside Natural products 0.000 description 1
- 150000008131 glucosides Chemical class 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229930007744 linalool Natural products 0.000 description 1
- WASNIKZYIWZQIP-AWEZNQCLSA-N nerolidol Natural products CC(=CCCC(=CCC[C@@H](O)C=C)C)C WASNIKZYIWZQIP-AWEZNQCLSA-N 0.000 description 1
- -1 nitrogen-containing heterocyclic compounds Chemical class 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001920 pimenta acris kostel leaf oil terpeneless Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
- 229920002258 tannic acid Polymers 0.000 description 1
- 229940033123 tannic acid Drugs 0.000 description 1
- 235000015523 tannic acid Nutrition 0.000 description 1
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention provides a preparation method of a black locust flower extract, which comprises the following steps: step one, preparing a coarse extract of robinia pseudoacacia flower; step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 20-80% of sophora flower extract, 0.1-1% of geranium oil, 0.1-1% of rose oil, 0.2-2% of 1% of jasmine absolute, 0.5-2% of 1% of damascenone, 1% of geranylacetone 1.0-5%, 1% of farnesone 1-5%, 10% of raspberry ketone 1-5%, 10% of ethyl phenylacetate 1-5%, and 95% of edible alcohol 0-75.1%. The invention can endow the cigarette with fragrance, flower fragrance, sweet aroma and other aroma, enrich the cigarette aroma, improve the aroma texture and improve the taste.
Description
Technical Field
The invention relates to the technical field of preparation and application of flavors and fragrances, in particular to a preparation method and application of a robinia pseudoacacia flower extract.
Background
The flavors and fragrances are one of the key factors for forming the style characteristics of cigarette products and improving the internal quality of cigarettes. At the moment that the competition in the cigarette market is intensified, the development and application of the essence and the spice with characteristic fragrance are effective means for increasing the bright spots of cigarette products and improving the brand competitiveness, and are also the key directions actively explored by cigarette essence blending personnel.
The 'fresh and sweet' cigarette is deeply loved by consumers due to the characteristics of elegance, nature and softness, wherein the 'fresh and sweet' cigarette represents a brand 'Yunyan' series cigarette, is well sold in the national market and is durable. The fresh and sweet flavor style becomes the aim of competing and imitating various cigarette enterprises, and the development and application of the flavor and fragrance with the fresh and sweet flavor characteristics are always the hot spot traced by the field of tobacco flavors. The robinia pseudoacacia flower is rich in fragrance and sweet, and the extract of the robinia pseudoacacia flower has a good application prospect in cigarettes and has a relatively high development value.
Robinia pseudoacacia L, also known as Robinia pseudoacacia. Leguminosae, Sophora deciduous tree. The flower is white, butterfly, and has strong fragrance, mainly fresh and green flower fragrance, and the sweet fruit fragrance and the sweet honey fragrance have rose-like sweet fragrance. The robinia pseudoacacia flower is rich in various aroma components such as linalool, phenethyl alcohol, geraniol, nerolidol, ethyl caproate, nitrogen-containing heterocyclic compounds and the like and various latent aroma substances such as amino acid, flavone, glucoside and the like. The robinia pseudoacacia flower extract is commonly provided with two types of essential oil and extract, the yield is low, the robinia pseudoacacia flower extract is mainly used for daily chemical essence raw materials, the application condition of the robinia pseudoacacia flower extract in tobacco is rarely reported, the characteristic of robinia pseudoacacia flower is lost mainly because the green aroma note of the robinia pseudoacacia flower extract is light and the sweet aroma note of the robinia pseudoacacia flower extract is heavy, the essential oil is heavier than the green aroma note and the sweet aroma is insufficient, meanwhile, the two types of extract are high in price, and the application cost.
In the prior art, the robinia pseudoacacia flower extract is subjected to multiple operations of refluxing, concentration and extraction in the preparation process, so that the loss of fragrance components is more, and the characteristic fragrance of the robinia pseudoacacia flower extract becomes thinner; the locust flower essential oil is generally prepared by a steam distillation method, and the collection rate of ketones and heterocycles with larger molecular weight is lower, so the fragrance is insufficient.
Therefore, the invention provides an economical and practical extraction method of robinia pseudoacacia flowers, which is simple to operate, and is used for preparing robinia pseudoacacia flower extracts with obvious aroma characteristics and applying the robinia pseudoacacia flower extracts to cigarette flavoring, which is a technical problem to be solved by technical personnel in the field.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the preparation method of the robinia pseudoacacia flower extract for the cigarettes.
The technical scheme of the invention is realized as follows:
a preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry sophora japonica into powder, and extracting the powder with 20-60 meshes; 2) sequentially adding water, 95% alcohol and the robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of the robinia pseudoacacia flower powder to 95% alcohol to water of 100: 600-1000: 200-400, and carrying out reflux extraction for 40-90 minutes; 3) adding 0.5-2.0 times of caprylic-capric glyceride of the sum of the mass of the added 95% alcohol and the mass of the water into an extraction tank, and continuously performing reflux extraction for 30-60 minutes; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) taking supernatant liquor, and filtering the supernatant liquor by using a filter membrane with the diameter of 0.22 to 0.65 mu m under positive pressure to obtain a coarse extract of the robinia pseudoacacia flower with the relative density of 0.93 to 0.97;
step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 20-80% of sophora robusta flower extract, 0.1-1% of geranium oil, 0.1-1% of rose oil, 0.2-2% of 1% of jasmine absolute oil, 0.5-2% of 1% of damascenone, 1.0-5% of geranylacetone, 1-5% of farnesone, 1-5% of 10% of raspberry ketone, 1-5% of ethyl phenylacetate and 0-75.1% of 95% of edible alcohol, wherein the obtained mixture is the sophora robusta flower extract.
Furthermore, the geranium oil, the rose oil, the jasmine absolute oil, the damascenone, the geranylacetone, the farnesone, the raspberry ketone, the ethyl phenylacetate and the 95% edible alcohol are all food grade.
Furthermore, the diluent solvent of 1% geranium oil, 1% rose oil, 1% jasmine absolute oil, 1% damascenone, 1% geranylacetone, 1% farnesyl acetone, 10% raspberry ketone and 10% ethyl phenylacetate is 95% edible alcohol or caprylic capric glyceride or a mixture of the two in any proportion.
The application of the acacia flower extract prepared by the method is characterized in that: adding the sophora japonica flower extract into cut tobacco of cigarettes according to the mass ratio of 0.05-1.0%.
The geranium oil, rose oil and jasmine absolute oil used in the invention are corresponding extracts which are purchased from the market and used as spices.
The invention develops and uses several new raw materials on the basis of cigarette spice, so that the effect of the extract is greatly improved:
and (3) coarse extract of sophora japonica: the main function is to endow the cigarette with fresh green aroma and sweet aroma, rich aroma and sweet smoke. The coarse extract of the robinia pseudoacacia flower prepared by the method has vivid fragrance, sweet aftertaste and finer smoke.
Geranium oil: endows the rose-like fragrance with a slight mint fragrance, and has sweet and fine smoke.
Rose oil: endows elegant flower fragrance and improves the fragrance texture.
And (3) jasmine absolute oil: endows the fragrance with natural and soft feeling, and makes the fragrance round.
Damascone, raspberry ketone: all can give sweet fragrance, damascenone is fine and elegant, raspberry ketone is low in sweet fragrance and heavy, and the two are combined in a proper proportion to enable the sweet fragrance to be mellow and harmonious.
Geranylacetone, farnesylacetone: can endow green aroma and sweet aroma, the aroma is light, the geranyl acetone aroma is sweet in green, the acacia acetone aroma is sweet in green, and the combination of the geranyl acetone aroma and the acacia acetone aroma can make the green and sweet aroma become natural.
Ethyl phenylacetate: endows sweet fragrance and can soften smoke.
The robinia pseudoacacia flower crude extract used in the invention has the functions of endowing the cigarettes with fresh green aroma and sweet aroma, rich aroma and sweet smoke, and compared with the similar extracts sold in the market, the green aroma and the sweet aroma are both retained more, and the whole aroma is stronger, more vivid and more natural. The preparation method of the coarse extract of the robinia pseudoacacia flower uses the caprylic capric acid glyceride as an extraction solvent, and has the main advantages that: 1) the polarity of an extraction solvent can be effectively reduced, so that the extraction rate of substances with negative effects on mouth feel, such as lignin, tannic acid, pectin and the like in the robinia pseudoacacia flower is reduced, the oral residue of a robinia pseudoacacia flower crude extract is effectively controlled, and the extraction rate of potential fragrant substances such as macromolecular esters and the like is higher; 2) the fragrant components are directly transferred into the caprylic capric acid glyceride, and compared with the excessive concentration or steam distillation operation in the traditional method, the loss rate of low boiling point substances is reduced, so that the fragrance of the crude extract is vivid and natural. 3) The solvent of the coarse extract of the robinia pseudoacacia flower is changed into the caprylic capric acid glyceride, and the robinia pseudoacacia flower can be used as essence and directly used as a bead blasting core material.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the specific embodiments.
Example 1
A preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry black locust flower into powder, and extracting the powder with 40 meshes; 2) sequentially adding water, 95% alcohol and robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of robinia pseudoacacia flower powder: 95% alcohol: water: 100: 600: 200, and carrying out reflux extraction for 90 minutes; 3) adding 1.0 time of caprylic/capric glyceride based on the sum of the above 95% ethanol and water into the extraction tank, and continuously extracting under reflux for 60 min; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) collecting supernatant, and filtering with 0.65 μm filter membrane under positive pressure to obtain coarse extract of flos Sophorae Immaturus with relative density of 0.94.
Step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 40% of robinia pseudoacacia flower crude extract, 1% of geranium oil, 1% of rose oil, 0.8% of 1% of jasmine absolute oil, 2% of 1% of damascenone, 2% of geranylacetone, 4% of farnesyl acetone, 5% of raspberry ketone, 1% of ethyl phenylacetate and 43.7% of edible alcohol, wherein the obtained mixture is the robinia pseudoacacia flower extract.
Example 2
A preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry black locust flower into powder, and extracting the powder with 40 meshes; 2) sequentially adding water, 95% alcohol and robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of robinia pseudoacacia flower powder: 95% alcohol: water: 100: 700: 200, and carrying out reflux extraction for 80 minutes; 3) adding 2.0 times of caprylic/capric glyceride of the sum of the above 95% ethanol and water into the extraction tank, and continuously extracting under reflux for 50 min; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) collecting supernatant, and filtering with 0.65 μm filter membrane under positive pressure to obtain coarse extract of flos Sophorae Immaturus with relative density of 0.94.
Step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 50% of a robinia pseudoacacia flower crude extract, 0.8% of 1% of geranium oil, 1.2% of rose oil, 1% of jasmine absolute oil, 1.5% of damascenone 4%, 1% of geranylacetone 1%, 1% of farnesyl acetone 5%, 10% of raspberry ketone 1%, 10% of ethyl phenylacetate 2% and 95% of edible alcohol 33.5%, wherein the obtained mixture is the robinia pseudoacacia flower extract.
Example 3
A preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry black locust flower into powder, and extracting the powder with 20 meshes; 2) sequentially adding water, 95% alcohol and robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of robinia pseudoacacia flower powder: 95% alcohol: water: 100: 800: 300, and carrying out reflux extraction for 70 minutes; 3) adding 1 time of caprylic/capric glyceride of the sum of the above 95% alcohol and water into an extraction tank, and continuously extracting under reflux for 40 min; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) collecting supernatant, and filtering with 0.45 μm filter membrane under positive pressure to obtain coarse extract of flos Sophorae Immaturus with relative density of 0.95.
Step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 60% of robinia pseudoacacia flower crude extract, 0.5% of 1% of geranium oil, 1% of rose oil, 1% of jasmine absolute oil, 1% of damascenone 4%, 1% of geranylacetone 3%, 1% of farnesone 3%, 10% of raspberry ketone 4%, 10% of ethyl phenylacetate 1% and 95% of edible alcohol 22.5%, wherein the obtained mixture is the robinia pseudoacacia flower extract.
Example 4
A preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry black locust flower into powder, and extracting the powder with 60 meshes; 2) sequentially adding water, 95% alcohol and robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of robinia pseudoacacia flower powder: 95% alcohol: water: 100: 900: 300, and carrying out reflux extraction for 60 minutes; 3) adding 1.0 time of caprylic/capric glyceride based on the sum of the above 95% ethanol and water into the extraction tank, and continuously extracting under reflux for 40 min; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) collecting supernatant, and filtering with 0.22 μm filter membrane under positive pressure to obtain coarse extract of flos Sophorae Immaturus with relative density of 0.94.
Step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 70% of robinia pseudoacacia flower crude extract, 0.3% of 1% of geranium oil, 0.5% of 1% of rose oil, 1% of jasmine absolute oil, 1% of damascenone 2%, 1% of geranylacetone 5%, 1% of farnesone 1%, 10% of raspberry ketone 3%, 10% of ethyl phenylacetate 2% and 95% of edible alcohol 15.2%, wherein the obtained mixture is the robinia pseudoacacia flower extract.
Example 5
A preparation method of a black locust flower extract comprises the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry black locust flower into powder, and extracting the powder with 60 meshes; 2) sequentially adding water, 95% alcohol and robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of robinia pseudoacacia flower powder: 95% alcohol: water: 100: 1000: 400, and carrying out reflux extraction for 40 minutes; 3) adding 0.5 time of caprylic/capric glyceride based on the sum of the above 95% ethanol and water into the extraction tank, and continuously extracting under reflux for 60 min; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) collecting supernatant, and filtering with 0.22 μm filter membrane under positive pressure to obtain coarse extract of flos Sophorae Immaturus with relative density of 0.95.
Step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components in percentage by mass: 80% of a robinia pseudoacacia flower crude extract, 0.2% of 1% of geranium oil, 0.3% of 1% of rose oil, 0.5% of 1% of jasmine absolute oil, 1% of damascenone 1%, 1% of geranylacetone 4%, 1% of farnesyl acetone 2%, 10% of raspberry ketone 1%, 10% of ethyl phenylacetate 3% and 95% of edible alcohol 8%, wherein the obtained mixture is the robinia pseudoacacia flower extract.
Adding the robinia pseudoacacia flower extract, the commercially available robinia pseudoacacia flower essential oil and the commercially available robinia pseudoacacia flower extract prepared in the above embodiment into cigarette tobacco shreds according to the mass percentage of 0.5%, rolling into cigarette samples, taking blank samples rolled under the same conditions as a control sample, and performing comparative evaluation on style characteristics and sensory quality of the cigarette samples and the control sample, wherein the results are shown in table 1:
TABLE 1 Style characteristics and sensory evaluation results
From the above table, the robinia pseudoacacia flower extract is superior to commercially available robinia pseudoacacia flower essential oil and robinia pseudoacacia flower extract in the aspects of forming the style characteristics of 'sweet fragrance' of cigarettes and improving the sensory quality of cigarettes. The robinia pseudoacacia flower extract prepared by the method can obviously increase the flower fragrance note by 5-6 minutes, the faint scent note by 3-5 minutes, the green scent note by 1-2 minutes and the sweet scent note by 1.5-4 minutes, and the fruit fragrance note, the spicy fragrance note and the paste fragrance note are slightly increased; the sophora japonica flower extract prepared by the method has the advantages that the effect on the aspects of fragrance amount, richness in fragrance, oral irritation, oral residue and the like is obviously improved, and the comprehensive sensory effect score is improved by about 10 points.
The raw materials with faint scent, sweet fragrance, flower fragrance and compound fragrance such as bay leaf oil, rose oil and the like are used for modifying and adjusting the coarse extract of the robinia pseudoacacia, so that the prepared robinia pseudoacacia extract has stable fragrance quality, and the quality cannot fluctuate greatly due to the quality difference of the dry robinia pseudoacacia and the control level difference of the extraction and preparation process. The geranium oil, the rose oil and the jasmine absolute oil are used in a matching way according to different proportions, and the fragrance and the flower fragrance are mainly adjusted; the damascenone and the raspberry ketone are used in different proportions, and the elegant feeling and the thick feeling of the sweet and fragrant note are mainly adjusted; geranyl acetone and farnesyl acetone are used in different proportions, so that the natural feeling of excess between faint scent and sweet scent is mainly adjusted, and the scent is mellow; the ethyl phenylacetate is mainly used for regulating the sweet note of honey and increasing the sweet note.
The above description is only an embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.
Claims (4)
1. The preparation method of the robinia pseudoacacia flower extract is characterized by comprising the following steps:
step one, preparing a coarse extract of robinia pseudoacacia flower
1) Grinding dry sophora japonica into powder, and extracting the powder with 20-60 meshes; 2) sequentially adding water, 95% alcohol and the robinia pseudoacacia flower powder into an extraction tank according to the mass ratio of the robinia pseudoacacia flower powder to 95% alcohol to water of 100: 600-1000: 200-400, and carrying out reflux extraction for 40-90 minutes; 3) adding 0.5-2.0 times of caprylic-capric glyceride of the sum of the mass of the added 95% alcohol and the mass of the water into an extraction tank, and continuously performing reflux extraction for 30-60 minutes; 4) coarsely filtering the solution to obtain a light yellow filtrate, and discarding filter residues; 5) slowly concentrating the filtrate under reduced pressure until the alcohol is completely volatilized, and standing the concentrated solution for 48 hours; 6) taking supernatant liquor, and filtering the supernatant liquor by using a filter membrane with the diameter of 0.22 to 0.65 mu m under positive pressure to obtain a coarse extract of the robinia pseudoacacia flower with the relative density of 0.93 to 0.97;
step two, uniformly mixing the coarse extract of the robinia pseudoacacia flower prepared in the step one and other raw material components according to the following mass percentage: 20-80% of sophora robusta flower extract, 0.1-1% of geranium oil, 0.1-1% of rose oil, 0.2-2% of 1% of jasmine absolute oil, 0.5-2% of 1% of damascenone, 1.0-5% of geranylacetone, 1-5% of farnesone, 1-5% of 10% of raspberry ketone, 1-5% of ethyl phenylacetate and 0-75.1% of 95% of edible alcohol, wherein the obtained mixture is the sophora robusta flower extract.
2. The method for preparing the robinia pseudoacacia flower extract according to claim 1, wherein the method comprises the following steps: the geranium oil, rose oil, jasmine absolute oil, damascenone, geranylacetone, farnesone, raspberry ketone, ethyl phenylacetate and 95% edible alcohol are all food grade.
3. The method for preparing the robinia pseudoacacia flower extract according to claim 1, wherein the method comprises the following steps: the diluent solvent of 1% of geranium oil, 1% of rose oil, 1% of jasmine absolute oil, 1% of damascenone, 1% of geranylacetone, 1% of farnesyl acetone, 10% of raspberry ketone and 10% of ethyl phenylacetate is 95% of edible alcohol or caprylic capric glyceride or a mixture of the edible alcohol and the caprylic capric glyceride in any proportion.
4. Use of an extract of black locust flower prepared by the process according to any one of claims 1 to 3, wherein: adding the sophora japonica flower extract into cut tobacco of cigarettes according to the mass ratio of 0.05-1.0%.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101606752A (en) * | 2008-06-16 | 2009-12-23 | 湖北中烟工业有限责任公司 | A kind of flavoring essence that is used for tobacco |
| CN103961440A (en) * | 2013-01-24 | 2014-08-06 | 厦门琥珀香料有限公司 | Novel aromatherapy essence and preparation method thereof |
| CN104946393A (en) * | 2015-06-17 | 2015-09-30 | 云南中烟工业有限责任公司 | Pyrus calleryana flower glycerol triacetate extract and application thereof in cigarette |
| CN105053427A (en) * | 2015-08-24 | 2015-11-18 | 王婧婧 | Preparation method of thermal reaction-type coffee flavor |
-
2017
- 2017-12-06 CN CN201711274714.1A patent/CN107987972B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101606752A (en) * | 2008-06-16 | 2009-12-23 | 湖北中烟工业有限责任公司 | A kind of flavoring essence that is used for tobacco |
| CN103961440A (en) * | 2013-01-24 | 2014-08-06 | 厦门琥珀香料有限公司 | Novel aromatherapy essence and preparation method thereof |
| CN104946393A (en) * | 2015-06-17 | 2015-09-30 | 云南中烟工业有限责任公司 | Pyrus calleryana flower glycerol triacetate extract and application thereof in cigarette |
| CN105053427A (en) * | 2015-08-24 | 2015-11-18 | 王婧婧 | Preparation method of thermal reaction-type coffee flavor |
Non-Patent Citations (2)
| Title |
|---|
| 乙醇提取刺槐花浸膏及其在烟草中的作用研究;周富臣，等;《香料香精化妆品》;20090228(第1期);第23-26页 * |
| 石油醚提取刺槐花浸膏及其在烟草中的作用研究;周富臣，等;《林产化学与工业》;20100430;第30卷(第2期);第89-93页 * |
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