CN102304433B - Processing technique of vanilla - Google Patents
Processing technique of vanilla Download PDFInfo
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- CN102304433B CN102304433B CN 201110199346 CN201110199346A CN102304433B CN 102304433 B CN102304433 B CN 102304433B CN 201110199346 CN201110199346 CN 201110199346 CN 201110199346 A CN201110199346 A CN 201110199346A CN 102304433 B CN102304433 B CN 102304433B
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Abstract
The invention discloses a processing technique of vanilla, which comprises the following steps: (1) adding 1 part by weight of vanilla into 2-10 parts by weight of 50-95% alcoholic solution, soaking for 5-10 days, and filtering to obtain a filtrate; (2) carrying out vacuum concentration on the filtrate in the step (1), boiling the concentrated solution, stopping heating when the volume of the filtrate is reduced to 15-20% of the original filtrate, and adjusting to normal pressure to obtain a paste liquid; (3) carrying out microwave drying on the paste liquid in the step (2) in vacuum until the weight percentage of the solvent in the paste is less than 5%; and (4) putting the paste dried in the step (3) into an extraction kettle, carrying out supercritical carbon dioxide extraction for 3-5hours, and separating the yellow oil liquid vanilla extract in the kettle, wherein the brownish black substance in the extraction kettle is vanilla oil resin. Since normal temperature and pressure extraction, vacuum concentration, microwave drying and supercritical carbon dioxide extraction are combined to extract the vanilla so as to simultaneously obtain the vanilla extract and vanilla oil resin, the extraction rate of odorous constituents in the vanilla extract can be enhanced, and the content of vanillin can also be enhanced.
Description
Technical field
The present invention relates to the plant processing technique field, especially a kind of complete processing of Herba vanillae Planifoliae beans.
Background technology
Herba vanillae Planifoliae [Vanilla planifolia (Salisb.) Ames. or V.frangrans Andrews] is the tropical crops with economic worth.Having another name called vanilla, vanilla, Vanilla annamica, Hua Nila, is the expensive perennial large-scale meat torrid zone liana climber of the orchid family Herba vanillae Planifoliae generic name, have the good reputation of " king of food spice ".
The head product chinese cymbidium pod of its bright beanpod of Herba vanillae Planifoliae after giving birth to fragrant processing is commonly called as the chinese cymbidium beans, contains more than 250 kind of volatile aroma composition.Because Herba vanillae Planifoliae contains numerous aromatic components, thereby its note is unique, now has been widely used in modulating the perfume material of joining of the high-grade food and drink such as various high-grade cigarettes, famous brand of wine, superfine tealeaves, cake, biscuit, candy, cream, coffee, cocoa ice-creams, chocolate, ice cream; Be used for the industry of making up, can make high-grade perfume; Also be used as the essence of fermentation, ornament and daily product.
Extract at present the aromatic condiment essential oil method and generally all adopt steam distillation, milling process, solvent-extraction process or supercritical carbon dioxide extraction; And extraction oleo-resinous common methods only is that solvent extration is a kind of, and the product of above-mentioned extracting method gained is single, and extraction yield and dna purity are not high.
Summary of the invention
The present invention is directed to deficiency, propose a kind of complete processing of Herba vanillae Planifoliae beans, can from the Herba vanillae Planifoliae beans, prepare vanilla Lenzin and two kinds of compositions of Herba vanillae Planifoliae oleo-resinous, and improved the extraction yield of vanilla Lenzin.
In order to realize the foregoing invention purpose, the invention provides following technical scheme: a kind of complete processing of Herba vanillae Planifoliae beans may further comprise the steps:
1., the Herba vanillae Planifoliae beans add in 50%～95% spirituous solution by weight 1: 2～10, soaked 5～10 days; Filter to get filtrate;
2., step is 1. concentrated under the filtrate vacuum and be heated to boiling, liquid to be filtered long-pending for original filtrate 15%～20% the time, stopped heating and transfer to normal pressure makes paste liquid;
3., with 2. paste liquid microwave drying under vacuum of step, weight of solvent content is less than 5% to the lotion;
4., to step 3. dried lotion place extraction kettle, carry out supercritical carbon dioxide extraction 3～5h, obtain yellow oily liquid vanilla Lenzin in the separating still; Brownish black material in the extraction kettle is the Herba vanillae Planifoliae oleo-resinous.
Preferably, step is the middle filter residue that obtains that filters 1., in 1: 2～10 addings, 50%～95% spirituous solution, soaks 5～10 days; Repeat to filter and soak three times, merge three times filtrate.
Preferably, step 2. or the vacuum 3. be-0.7MPa～-1.2MPa.
Preferably, the microwave power of step in 3. is 1～2kw.
Preferably, step 4. middle supercritical extraction condition is 40 ℃～45 ℃, 80～90MPa.
Preferably, step 1. in the Herba vanillae Planifoliae beans for being cut in the 0.5～1cm segment adding spirituous solution.
Compared with prior art, the present invention extracts the method for vanilla Lenzin and Herba vanillae Planifoliae oleo-resinous from the Herba vanillae Planifoliae beans, extract Herba vanillae Planifoliae by the method that normal temperature and pressure extraction, vacuum concentration, microwave drying and supercritical carbon dioxide extraction combine, not only can extract simultaneously two kinds of products of vanilla Lenzin and Herba vanillae Planifoliae oleo-resinous, and can improve the extraction yield of aroma component in the vanilla Lenzin, the content of vanillin food grade,1000.000000ine mesh also is improved simultaneously.
In the complete processing of the present invention, because vanilla Lenzin and oleo-resinous all are mixture, the former fat-soluble small molecules is main, latter's macromole is main, utilize the fat-soluble resin of small molecules volatile oil and macromole in alcohol, all to have better solubleness, impel two kinds of compositions to leach fully, in supercritical co, two kinds of products have the characteristics of different solubility, the principle of work that in the short period of time both are effectively separated.Vanilla Lenzin, Herba vanillae Planifoliae oleo-resinous purity with extraction are high, and the product fragrance loss is few, and quality is high, the production cost decrease, and labor savings, and can obtain simultaneously the advantage of two kinds of Herba vanillae Planifoliae deep processed products.
Embodiment
Describe the present invention below in conjunction with specific embodiment, the description of this part only is exemplary and explanatory, should any restriction not arranged to protection scope of the present invention.
Embodiment 1
The complete processing of Herba vanillae Planifoliae beans may further comprise the steps:
1, the Herba vanillae Planifoliae beans that preliminary working is good are cut into 0.5～1cm segment, with 95% spirituous solution be to put into the lixiviate still at 1: 2 by solid-liquid ratio, after fully stirring, under normal temperature and pressure conditions, flooded 5 days, open discharge valve, leach the solvent part.
2, filtrate is poured in the thickner, adjustable pressure vacuum tightness is to-0.9MPa, and heater temperature is 40 ℃, carries out cryoconcentration, regulate heater temperature, make liquid boiling distillation in the thickner, collect distillate, to the flowing liquid volume arrive volume when putting into 85% the time, stopped heating, it is normal pressure that the adjustable pressure valve makes the thickner internal gas pressure, opens sealing cover, takes out paste liquid in the thickner.
3, above-mentioned paste liquid is put into microwave drying oven, adjustable pressure is-0.9MPa, microwave power 1kw, carry out microwave drying to lotion weight of solvent and be gross weight 2% the time, taking-up is cut into small pieces.
4, above-mentioned fritter is put into the supercritical, high pressure extraction kettle, at 45 ℃, under the 90MPa condition, carry out supercritical carbon dioxide extraction 3h, the yellow oily liquid of emitting through the separating still discharge port is the vanilla Lenzin, and left brownish black material is the Herba vanillae Planifoliae oleo-resinous in the extraction kettle.
Embodiment 2
The complete processing of Herba vanillae Planifoliae beans may further comprise the steps:
1, the Herba vanillae Planifoliae beans that preliminary working is good are cut into 0.5～1cm segment, with 50% spirituous solution be to put into the lixiviate still at 1: 10 by solid-liquid ratio, after fully stirring, under normal temperature and pressure conditions, flooded 10 days, open discharge valve, leach the solvent part, add novel solvent by same ratio again, dipping.Then same method 3 times repeatedly mixes 3 filtrates.
2, the mixed solution that leaches for 3 times is poured in the thickner, adjustable pressure vacuum tightness is to-0.7MPa, and heater temperature is 45 ℃, carries out cryoconcentration, regulate heater temperature, make liquid boiling distillation in the thickner, collect distillate, to the flowing liquid volume arrive volume when putting into 80% the time, stopped heating, it is normal pressure that the adjustable pressure valve makes the thickner internal gas pressure, opens sealing cover, takes out paste liquid in the thickner.
3, above-mentioned paste liquid is put into microwave drying oven, adjustable pressure is-0.7MPa, microwave power 2kw, carry out microwave drying to lotion weight of solvent and be gross weight 4% the time, taking-up is cut into small pieces.
4, above-mentioned fritter is put into the supercritical, high pressure extraction kettle, at 40 ℃, under the 80MPa condition, carry out supercritical carbon dioxide extraction 5h, the yellow oily liquid of emitting through the separating still discharge port is the vanilla Lenzin, and left brownish black material is the Herba vanillae Planifoliae oleo-resinous in the extraction kettle.
Embodiment 3
The complete processing of Herba vanillae Planifoliae beans may further comprise the steps:
1, the Herba vanillae Planifoliae beans that preliminary working is good are cut into 0.5～1cm segment, with 68% spirituous solution be to put into the lixiviate still at 1: 6 by solid-liquid ratio, after fully stirring, under normal temperature and pressure conditions, flooded 8 days, open discharge valve, leach the solvent part, add novel solvent by same ratio again, dipping.Then same method 3 times repeatedly mixes 3 filtrates.
2, the mixed solution that leaches for 3 times is poured in the thickner, adjustable pressure vacuum tightness is to-0.8MPa, and heater temperature is 43 ℃, carries out cryoconcentration, regulate heater temperature, make liquid boiling distillation in the thickner, collect distillate, to the flowing liquid volume arrive volume when putting into 84% the time, stopped heating, it is normal pressure that the adjustable pressure valve makes the thickner internal gas pressure, opens sealing cover, takes out paste liquid in the thickner.
3, above-mentioned paste liquid is put into microwave drying oven, adjustable pressure is-0.8MPa, microwave power 1.5kw, carry out microwave drying to lotion weight of solvent and be gross weight 3% the time, taking-up is cut into small pieces.
4, above-mentioned fritter is put into the supercritical, high pressure extraction kettle, at 42 ℃, under the 85MPa condition, carry out supercritical carbon dioxide extraction 4h, the yellow oily liquid of emitting through the separating still discharge port is the vanilla Lenzin, and left brownish black material is the Herba vanillae Planifoliae oleo-resinous in the extraction kettle.
To the resulting vanilla Lenzin of above-described embodiment and Herba vanillae Planifoliae oleo-resinous, carry out aroma component by gas chromatograph-mass spectrometer and detect, the result is shown in following table 1 and 2.
Table 1 vanilla Lenzin product composition contrast table
| The contrast project | Supercritical methanol technology | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Small molecules aroma component extraction yield | 62.3％ | 85.2％ | 86.5％ | 87.2％ |
| Small molecules aroma component purity | 84.9％ | 91.2％ | 92.3％ | 91.5％ |
| Vanillin food grade,1000.000000ine mesh content | 33.9％ | 34.6％ | 34.3％ | 34.8％ |
Table 2 Herba vanillae Planifoliae oleo-resinous product composition contrast table
| The contrast project | Solvent method | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Macromole aroma component extraction yield | 75.6％ | 78.4％ | 77.9％ | 78.2％ |
| Macromole aroma component purity | 72.3％ | 82.6％ | 83.1％ | 83.2％ |
| Vanillin food grade,1000.000000ine mesh content | 18.7％ | 19.2％ | 19.5％ | 19.3％ |
In above-mentioned table 1 and the table 2, the total fragrance content of aroma component extraction yield=proposition/fragrance content * 100% should be arranged; Aroma component purity=(proposing total fragrance content-impurity fragrance content)/fragrance kind content * 100% should be arranged; Vanillin food grade,1000.000000ine mesh content=total fragrance the content of proposition vanillin food grade,1000.000000ine mesh content/proposition * 100%.
The present invention compared with prior art has vanilla Lenzin, the Herba vanillae Planifoliae oleo-resinous purity height of extraction, and the product fragrance loss is few, and quality is high, the production cost decrease, and can obtain simultaneously two kinds of Herba vanillae Planifoliae deep processed products, the advantage of labor savings.
It below only is preferred implementation of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (5)
1. the complete processing of Herba vanillae Planifoliae beans may further comprise the steps:
1., the Herba vanillae Planifoliae beans add in 50%～95% spirituous solution by weight 1 ︰ 2～10, soaked 5～10 days; Filter to get filtrate;
2., step is 1. concentrated under the filtrate vacuum and be heated to boiling, liquid to be filtered long-pending for original filtrate 15%～20% the time, stopped heating and transfer to normal pressure makes paste liquid;
3., with 2. paste liquid microwave drying under vacuum of step, weight of solvent content is less than 5% to the lotion;
4., to step 3. dried lotion place extraction kettle, carry out supercritical carbon dioxide extraction 3～5h, obtain yellow oily liquid vanilla Lenzin in the separating still; Brownish black material in the extraction kettle is the Herba vanillae Planifoliae oleo-resinous;
Step 4. middle supercritical extraction condition is 40 ℃～45 ℃, 80～90MPa.
2. complete processing as claimed in claim 1 is characterized in that: step is filtered the filter residue that obtains in 1., adds in 50%～95% spirituous solution by weight 1 ︰ 2～10, soaks 5～10 days; Repeat to filter and soak three times, merge three times filtrate.
3. complete processing as claimed in claim 1 is characterized in that: step 2. or the vacuum 3. for-0.7MPa～-1.2MPa.
4. complete processing as claimed in claim 1 is characterized in that: the microwave power of step in 3. is 1～2kw.
5. complete processing as claimed in claim 1 is characterized in that: step 1. in the Herba vanillae Planifoliae beans for being cut in 0.5～1cm segment adding spirituous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110199346 CN102304433B (en) | 2011-07-15 | 2011-07-15 | Processing technique of vanilla |
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|---|---|---|---|
| CN 201110199346 CN102304433B (en) | 2011-07-15 | 2011-07-15 | Processing technique of vanilla |
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| CN102304433A CN102304433A (en) | 2012-01-04 |
| CN102304433B true CN102304433B (en) | 2013-04-10 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232890B (en) * | 2012-12-28 | 2014-10-22 | 红塔烟草(集团)有限责任公司 | Method for improving vanilla bean tincture aroma quality |
| CN103351954A (en) * | 2013-07-11 | 2013-10-16 | 大连卓尔高科技有限公司 | Process for extracting eaglewood essential oil by using supercritical carbon dioxide |
| CN103981029B (en) * | 2014-05-21 | 2015-08-19 | 中国热带农业科学院香料饮料研究所 | A kind of bean pod of Herba vanillae Planifoliae extract, its preparation method and application |
| CN104946397A (en) * | 2015-06-19 | 2015-09-30 | 湖北中烟工业有限责任公司 | Method for extracting vanilla extract used for tobacco through high-pressure puffing of supercritical CO2 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US4474994A (en) * | 1982-09-13 | 1984-10-02 | Monsanto Company | Purification of vanillin |
| US20030070188A1 (en) * | 1997-07-15 | 2003-04-10 | Daphna Havkin-Frenkel | Vanillin biosynthetic pathway enzyme from Vanilla planifolia |
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Effective date of registration: 20160302 Address after: 571500 prosperous Tropical Botanical Garden, Hainan, Wanning Patentee after: Hainan branch tropical crop Engineering Technology Co., Ltd. Address before: 571533 Hainan Province, directly under the county level administrative unit, Wanning flourishing town spices Beverage Research Institute Patentee before: Institute of Spices and Beverage, Chinese Academy of Tropical Agricultural Sciences |