CN104740893A - Ultrasonic-assisted accelerated solvent extraction method for vanilla tincture - Google Patents
Ultrasonic-assisted accelerated solvent extraction method for vanilla tincture Download PDFInfo
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- CN104740893A CN104740893A CN201510092733.7A CN201510092733A CN104740893A CN 104740893 A CN104740893 A CN 104740893A CN 201510092733 A CN201510092733 A CN 201510092733A CN 104740893 A CN104740893 A CN 104740893A
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- vanilla
- ultrasonic
- tincture
- solvent extraction
- accelerated solvent
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- 235000009499 Vanilla fragrans Nutrition 0.000 title claims abstract description 48
- 235000012036 Vanilla tahitensis Nutrition 0.000 title claims abstract description 48
- 244000263375 Vanilla tahitensis Species 0.000 title claims abstract description 46
- 229940098465 tincture Drugs 0.000 title claims abstract description 38
- 238000000899 pressurised-fluid extraction Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000000706 filtrate Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 11
- 239000000284 extract Substances 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract description 10
- 238000002525 ultrasonication Methods 0.000 claims description 8
- 230000000717 retained effect Effects 0.000 claims description 7
- 238000012545 processing Methods 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 2
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000428 dust Substances 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000009210 therapy by ultrasound Methods 0.000 abstract 1
- 238000002604 ultrasonography Methods 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 210000004027 cell Anatomy 0.000 description 9
- 239000004480 active ingredient Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 210000000170 cell membrane Anatomy 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 2
- 244000290333 Vanilla fragrans Species 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Seasonings (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses an ultrasonic-assisted accelerated solvent extraction method for vanilla tincture and belongs to the technical field of chemistry. The extraction method comprises the following steps: carrying out washing and dust removing on vanillas and then chopping; adding certain amount of an ethanol solvent into the chopped vanillas and pre-treating in an ultrasonic cell crusher; filtering the sample treated by ultrasounds and remaining a filtrate; transferring filtering dreg into an accelerating solvent extract material bottle to be extracted; and after extracting, cooling and standing to obtain clarified liquid, and mixing the liquid with the filtrate obtained by ultrasonic treatment to obtain the vanilla tincture. Compared with an existing tincture preparation method, the production period of the method can be greatly shortened, the use amount of the extracting solvent is reduced and the yield of effective components is extremely improved. The quality of the vanilla tincture prepared by the method is remarkably better than that of the vanilla tincture prepared by a conventional vanilla extracting method.
Description
Technical field
The present invention relates to the technical field preparing natural plants tincture, particularly a kind of method utilizing ultrasonic wave added accelerated solvent extraction vanilla tincture.
Background technology
Vanilla beans are a kind of famous and precious natural flavors, the fragrance plentiful, strong because of it and be widely used in the field such as medicine, food.Because current tincture preparation technology falls behind, make the leaching process time long, and active ingredient yield is low, causes the serious waste of resource.Therefore, new extraction means are constantly applied in the preparation of tincture, to improve extraction efficiency and the quality of tincture.
Along with the development of science and technology, ultrasonic cell-break and accelerated solvent extraction were used widely in recent years.Ultrasonic cell-break technology utilizes super-pressure energy to make cell membrane and cell membrane destroyed under the effect of external force, and active principle in cell is discharged.Simple to operate, sample loss amount also can keep cytoactive less.Accelerated solvent extraction is in airtight container, is extracted, substantially increases extraction efficiency, decrease solvent consumption by the mode of temperature-pressure.The method can, within the extremely short time, use minimum solvent load to extract sample, and HTHP can make solvent more easily enter in sample substrate, and active ingredient is more easily diffused in solvent.Both methods combining have easy and simple to handle, the province's solvent that saves time, can extract active ingredient to greatest extent.
Utilize ultrasonic cell-break and accelerated solvent extraction to extract natural plants tincture, be with a wide range of applications, have not been reported in current research.
Summary of the invention
Problem to be solved by this invention is the deficiency for traditional tincture preparation method, provides a kind of preparation method of ultrasonic wave added accelerated solvent extraction vanilla tincture.The method, compared with existing tincture preparation method, significantly can shorten the production cycle, reduces the consumption of Extraction solvent, and greatly improves the rate of recovery of active ingredient.Vanilla tincture prepared by the method, quality is obviously better than conventional tincture extraction method.
Technical problem to be solved by this invention is achieved through the following technical solutions:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, it comprises the steps:
(1) carry out after vanilla being rinsed dedusting shearing, segment processing;
(2) add the alcohol solvent that mass ratio is 1:1 ~ 1:5 in the vanilla handled well in step (1), utilize ultrasonic cell disruption instrument to carry out pretreatment;
(3) sample after ultrasonication in step (2) is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) filter residue retained in step (3) is transferred in the bottle for material of accelerated solvent extraction, extracts 1 ~ 5 time;
(5) material of step (4) gained is left standstill 30 ~ 60min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Preferably, in described step (1), carry out segment processing to vanilla, wherein every segment length is 1 ~ 2cm.
Preferably, in described step (2), the volumetric concentration of alcohol solvent is 50 ~ 100%.
Preferably, ultrasonic cell disruption instrument carries out pretreated condition and is in described step (2): ultrasonic power is 200W ~ 600W, and ultrasonic time is 30min ~ 90min, and the intermittent time is 0 ~ 30s.
Preferably, in described step (4), extraction conditions is: power is set to 200 ~ 600W, and extraction time is 1h ~ 3h, and temperature is 50 ~ 100 DEG C, and pressure setting is 3 ~ 10MPa.
The invention has the advantages that:
1, vanilla is carried out segment processing by this extracting method, and when contributing to extracting, fragrance component overflows, and can promote the rate of recovery of active ingredient.
2, this extracting method utilizes ultrasonication technology, cell membrane and cell membrane can be made destroyed under the effect of super-pressure external force, active principle in cell is discharged.
3, this extracting method is by accelerated solvent extraction, solvent can be made at high temperature under high pressure more easily to enter in sample substrate, active ingredient is more easily diffused in solvent.
4, this prepares that tincture method required time is short, solvent load is little, and can extract active ingredient to greatest extent, gained tincture quality is obviously better than other conventional methods.
Detailed description of the invention
Below by way of specific embodiment, the present invention is described in further detail.
Embodiment one:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, its step is as follows:
(1) get vanilla 50g, after being rinsed dedusting, cut into the cut-out that length is 1cm, for subsequent use;
(2) in the vanilla handled well in step (1), add the alcohol solvent that 50g volumetric concentration is 60%, utilize ultrasonic cell disruption instrument to carry out pretreatment: ultrasonic power is 200W, ultrasonic time is 30min, and the intermittent time is 10s;
(3) sample after ultrasonication in step (2) is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) be transferred in the bottle for material of accelerated solvent extraction by the filter residue retained in step (3), power is set to 200W, and the time is 10min, and temperature is 60 DEG C, and pressure is set to 3MPa, extracts 2 times;
(5) material of step (4) gained is left standstill 30min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Embodiment two:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, its step is as follows:
(1) get vanilla 50g, after being rinsed dedusting, cut into the cut-out that length is 1.5cm, for subsequent use;
(2) in the vanilla handled well in step (1), add the alcohol solvent that 80g volumetric concentration is 80%, utilize ultrasonic cell disruption instrument to carry out pretreatment: ultrasonic power is 400W, ultrasonic time is 60min, and the intermittent time is 20s;
(3) sample after ultrasonication in step (2) is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) be transferred in the bottle for material of accelerated solvent extraction by the filter residue retained in step (3), power is set to 400W, and the time is 20min, and temperature is 80 DEG C, and pressure is set to 6MPa, extracts 3 times;
(5) material of step (4) gained is left standstill 40min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Embodiment three:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, its step is as follows:
(1) get vanilla 50g, after being rinsed dedusting, cut into the cut-out that length is 2cm, for subsequent use;
(2) in the vanilla handled well in step (1), add 100g anhydrous ethanol solvent, utilize ultrasonic cell disruption instrument to carry out pretreatment: ultrasonic power is 600W, ultrasonic time is 90min, and the intermittent time is 20s;
(3) sample after step (2) ultrasonication is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) be transferred in the bottle for material of accelerated solvent extraction by the filter residue retained in step (3), power is set to 600W, and the time is 30min, and temperature is 100 DEG C, and pressure is set to 9MPa, extracts 4 times;
(5) material of step (4) gained is left standstill 60min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Embodiment four:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, its step is as follows:
(1) get vanilla 50g, after being rinsed dedusting, cut into the cut-out that length is 2cm, for subsequent use;
(2) in the vanilla handled well in step (1), add 50g anhydrous ethanol solvent, utilize ultrasonic cell disruption instrument to carry out pretreatment: ultrasonic power is 600W, ultrasonic time is 90min, and the intermittent time is 20s;
(3) sample after step (2) ultrasonication is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) be transferred in the bottle for material of accelerated solvent extraction by the filter residue retained in step (3), power is set to 600W, and the time is 30min, and temperature is 100 DEG C, and pressure is set to 9MPa, extracts 4 times;
(5) material of step (4) gained is left standstill 60min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Embodiment five:
A method for ultrasonic wave added accelerated solvent extraction vanilla tincture, its step is as follows:
(1) get vanilla 50g, after being rinsed dedusting, cut into the cut-out that length is 1.5cm, for subsequent use;
(2) in the vanilla handled well in step (1), add the alcohol solvent that 200g volumetric concentration is 80%, utilize ultrasonic cell disruption instrument to carry out pretreatment: ultrasonic power is 400W, ultrasonic time is 60min, and the intermittent time is 20s;
(3) sample after ultrasonication in step (2) is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) be transferred in the bottle for material of accelerated solvent extraction by the filter residue retained in step (3), power is set to 400W, and the time is 20min, and temperature is 80 DEG C, and pressure is set to 6MPa, extracts 3 times;
(5) material of step (4) gained is left standstill 40min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
Claims (5)
1. a preparation method for ultrasonic wave added accelerated solvent extraction vanilla tincture, it comprises the steps:
(1) carry out after vanilla being rinsed dedusting shearing, segment processing;
(2) add the alcohol solvent that mass ratio is 1:1 ~ 1:5 in the vanilla handled well in step (1), utilize ultrasonic cell disruption instrument to carry out pretreatment;
(3) sample after ultrasonication in step (2) is filtered, collect filtrate, and it is stand-by to retain filter residue;
(4) filter residue retained in step (3) is transferred in the bottle for material of accelerated solvent extraction, extracts 1 ~ 5 time;
(5) material of step (4) gained is left standstill 30 ~ 60min, obtain the liquid clarified;
(6) liquid of gained in step (5) is mixed with filtrate collected in step (3), be vanilla tincture.
2. the preparation method of a kind of ultrasonic wave added accelerated solvent extraction vanilla tincture according to claim 1, is characterized in that: in described step (1), carry out segment processing to vanilla, and wherein every segment length is 1 ~ 2cm.
3. the preparation method of a kind of ultrasonic wave added accelerated solvent extraction vanilla tincture according to claim 1 and 2, it is characterized in that: in described step (2), the volumetric concentration of alcohol solvent is 50 ~ 100%.
4. the preparation method of a kind of ultrasonic wave added accelerated solvent extraction vanilla tincture according to claim 1 and 2, it is characterized in that: the middle ultrasonic cell disruption instrument of described step (2) carries out pretreated condition and is: ultrasonic power is 200W ~ 600W, ultrasonic time is 30min ~ 90min, and the intermittent time is 0 ~ 30s.
5. the preparation method of a kind of ultrasonic wave added accelerated solvent extraction vanilla tincture according to claim 1 and 2, it is characterized in that: in described step (4), extraction conditions is: power is set to 200 ~ 600W, extraction time is 1h ~ 3h, temperature is 50 ~ 100 DEG C, and pressure setting is 3 ~ 10MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2642641C1 (en) * | 2016-11-16 | 2018-01-25 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Membrane extractor |
| CN109105947A (en) * | 2018-07-05 | 2019-01-01 | 湖北中烟工业有限责任公司 | A kind of multistage solvent extraction preparation method and applications of cocoa extract |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101498701A (en) * | 2009-03-09 | 2009-08-05 | 南京大学 | Detection method for phthalate ester residue |
| US20100058973A1 (en) * | 2006-11-15 | 2010-03-11 | Skin'up | Control and/or monitoring method for the salting-out of at least one active ingredient impregnated in a textile |
| CN103525558A (en) * | 2013-09-27 | 2014-01-22 | 福建中烟工业有限责任公司 | Tea flower essence with fruity flavor characteristic and application thereof to cigarettes |
| CN103783226A (en) * | 2014-02-19 | 2014-05-14 | 郭景龙 | Soy sauce flavor type tea |
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2015
- 2015-02-28 CN CN201510092733.7A patent/CN104740893B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100058973A1 (en) * | 2006-11-15 | 2010-03-11 | Skin'up | Control and/or monitoring method for the salting-out of at least one active ingredient impregnated in a textile |
| CN101498701A (en) * | 2009-03-09 | 2009-08-05 | 南京大学 | Detection method for phthalate ester residue |
| CN103525558A (en) * | 2013-09-27 | 2014-01-22 | 福建中烟工业有限责任公司 | Tea flower essence with fruity flavor characteristic and application thereof to cigarettes |
| CN103783226A (en) * | 2014-02-19 | 2014-05-14 | 郭景龙 | Soy sauce flavor type tea |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2642641C1 (en) * | 2016-11-16 | 2018-01-25 | федеральное государственное бюджетное образовательное учреждение высшего образования "Алтайский государственный университет" | Membrane extractor |
| CN109105947A (en) * | 2018-07-05 | 2019-01-01 | 湖北中烟工业有限责任公司 | A kind of multistage solvent extraction preparation method and applications of cocoa extract |
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| CN104740893B (en) | 2016-09-21 |
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