CN106749340A - A kind of method that surfactant collaboration aqueous two-phase extracts nimbin - Google Patents
A kind of method that surfactant collaboration aqueous two-phase extracts nimbin Download PDFInfo
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- CN106749340A CN106749340A CN201611062098.9A CN201611062098A CN106749340A CN 106749340 A CN106749340 A CN 106749340A CN 201611062098 A CN201611062098 A CN 201611062098A CN 106749340 A CN106749340 A CN 106749340A
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- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D519/00—Heterocyclic compounds containing more than one system of two or more relevant hetero rings condensed among themselves or condensed with a common carbocyclic ring system not provided for in groups C07D453/00 or C07D455/00
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/06—Peri-condensed systems
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/12—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains three hetero rings
- C07D493/18—Bridged systems
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Abstract
The method that a kind of surfactant collaboration aqueous two-phase involved in the present invention extracts nimbin, it is deoiled by printing the crushing of chinaberry seed, it is ultrasonically treated, the double region of rivers and lakes extractions of surfactant inorganic salts, purifying, obtain nimbin, the present invention is by the use of surfactant as extract solution, making full use of it had not only had lipophile but also with hydrophilic unique physicochemical property as good solubilizer, and cooperatively form aqueous two-phase with inorganic salts, under the synergy of ultrasonic wave, effective smudge cells tissue, so that nimbin is substantially dissolved in solvent, greatly improve the recovery rate of nimbin, especially improve the recovery rate of nimbin A, efficiently solve traditional extraction technology extraction time long, the low problem of extraction efficiency.
Description
Technical field
The invention belongs to active substance of plant extractive technique field, more particularly to a kind of aqueous two-phase method extracts the side of nimbin
Method.
Background technology
Nimbin is the active component in chinaberry fruit, has significant Antifeedant Effects and growth inhibition effect to insect,
And it is safe and harmless to vertebrate, it is the novel substance for developing environment friendly agricultural.
In recent years, each accomplished expert and mechanism are all continuing to increase the research to nimbin extractive technique both at home and abroad.Tradition is carried
The method for taking nimbin is mainly conventional extraction, ultrasonic extraction, microwave method, rapid extraction -ASE etc..But, conventional extraction
Time-consuming, completes once extracting needs the time of nearly 6 days；The equipment investment of ultrasonic extraction and microwave method is big, production efficiency
It is limited, and ultrasound and microwave cause different injuries to people's cognition respectively, to add corresponding auxiliary equipment, then can increase life
Produce cost；Rapid extraction -ASE is reduced compared to the equipment cost of ultrasonic extraction and microwave loss mechanisms, but recovery rate is relatively low, only
0.3% or so can be reached.
Therefore, seek a kind of low cost, the investment nimbin extracting method that small, security is good and recovery rate is high to become urgently
Problem to be solved.
The content of the invention
In order to overcome the shortcomings of existing for above-mentioned prior art, the invention provides a kind of cost it is relatively low, recovery rate is high, can
Nimbin contact light, heat, alkali for a long time are prevented effectively from, and extraction conditions are gentle, help to maintain the surface work of nimbin activity
Property agent collaboration aqueous two-phase extract nimbin method.
The technical scheme that the present invention is used to achieve these goals is that surfactant collaboration aqueous two-phase extracts print
The method of chinaberry element is comprised the steps of：
(1) chinaberry seed natural air drying will be printed, peeling, benevolence oil expression, the cake ground-slag after deoiling is broken, crosses 40~60 mesh sieves, obtains
It is standby to the benevolence powder that deoils；
(2) aqueous surfactant solution that mass fraction is 1%~10% is prepared, is 1 by solid-liquid ratio:5~25g/mL's
Ratio adds the benevolence powder that deoils, and is 5~10W/cm in ultrasonic power density2, supersonic frequency be 28~50kHz, ultrasonic radiation side
Formula is ultrasonically treated 15~20min under the ultrasound condition of 10s~15s/20s, and ultrasonic transmitting element is distributed in the side for extracting chamber
Wall and bottom；
(3) inorganic salts are added in the extraction system according to the ratio that mass fraction is 5%~15% to step (2), is stirred
Dissolving, forms double-aqueous phase system, and target product nimbin is enriched in upper surface activating agent phase, and small molecular weight impurity and carbohydrate are enriched with
In lower floor's water phase, phase in taking-up, purifying obtains nimbin.
Further, the surfactant of the step (2) is nonionic surface active agent or ionic surfactant.
Further, the nonionic surface active agent is Triton X-100, Tween-20, Tween-80, polyoxy second
Any one or more combination in alkene fatty acid ester, Dodecyl Polyoxyethylene Ether and NPE.
Further, the ionic surfactant is sodium dodecylbenzenesulfonate, lauryl sodium sulfate, 16
In alkyl trimethyl ammonium bromide, dodecyl benzyl dimethyl ammonium chloride and OPEO sulfate any one
Or various combinations.
Further, the inorganic salts are any in dipotassium hydrogen phosphate, disodium hydrogen phosphate, sodium nitrate and potassium dihydrogen phosphate
A kind of or any combination.
Further, the purification process of the step (3) is：It is 600 that upper surface activating agent is mutually loaded into molecular cut off
In the bag filter of~1000Da, dialysed with deionized water, the nimbin for being purified.
Further, step (2) described ultrasonic transmitting element is symmetrically distributed in the side wall in extraction chamber, and be oppositely arranged
The distance between two ultrasonic transmitting elements are the integral multiples of ultrasonic wavelength.
Further, the step (2) is specifically：The aqueous surfactant solution that mass fraction is 5%~8% is prepared, is pressed
Solid-liquid ratio is 1:The ratio of 10~20g/mL adds the benevolence powder that deoils, and is 5~10W/cm in ultrasonic power density2, supersonic frequency
For 28~50kHz, ultrasonic radiation mode are ultrasonically treated 15~20min under the ultrasound condition of 10s~15s/20s, ultrasonic wave hair
Penetrate cell distribution and extracting the side wall in chamber and bottom, be symmetrical on the wall of side, and the two ultrasonic waves transmitting being oppositely arranged
The distance between unit is the integral multiple of ultrasonic wavelength, forms resonance and standing wave to promote aqueous surfactant solution in turbidity shape
The nimbin in raw material is fully dissolved under state.
The method that surfactant of the invention collaboration aqueous two-phase extracts nimbin, by the use of surfactant as extraction
Liquid, makes full use of it not only to have lipophile but also with hydrophilic unique physicochemical property as good solubilizer, and with
Inorganic salts cooperatively form aqueous two-phase, under the synergy of ultrasonic wave, effective smudge cells tissue, so that nimbin is fully molten
Solution in a solvent, greatly improves the recovery rate of nimbin, especially the recovery rate of active component nimbin A, efficiently solves biography
The system problem that extractive technique extraction time is long, extraction efficiency is low, easy to operate, low cost of the invention, the rate of recovery are high in addition, do not have
Use organic solvent, it is to avoid environmental problem, health problem that organic solvent is caused, with good ecological benefits, may be used also
Light, heat, alkali are touched for a long time to be prevented effectively from nimbin, and extraction conditions are gentle, help to maintain the activity of nimbin, and energy
A step removal of impurities in extraction process is realized, Simplified flowsheet is suitable to industrialization promotion.
Brief description of the drawings
Fig. 1 is the chromatogram of nimbin mark product.
Fig. 2 is the extract chromatogram of embodiment 1.
Specific embodiment
Technical scheme is further described in conjunction with experiment and embodiment, but the present invention is not limited only to
Following implementation situations.
The method that the present invention extracts nimbin is realized by following steps：
(1) chinaberry seed natural air drying is printed, peeling, benevolence oil expression, the cake ground-slag after deoiling is broken, crosses 40~60 mesh sieves, standby.
(2) aqueous surfactant solution that mass fraction is 1%~10% is prepared, the benevolence powder that deoils is added, in ultrasonic work(
Rate density is 2~10W/cm2, supersonic frequency be 25~60kHz, ultrasonic radiation mode for 10s~15s/20s ultrasound condition under
Ultrasonically treated 15~20min, ultrasonic transmitting element is distributed in the side wall and bottom for extracting chamber, on the wall of side be it is symmetrical,
And the distance between two ultrasonic transmitting elements being oppositely arranged are the integral multiples of ultrasonic wavelength, form resonance and standing wave to promote
Nimbin in making aqueous surfactant solution fully dissolve raw material under turbidity state；
(3) inorganic salts are added in the extraction system according to certain ratio to step (2), stirring and dissolving forms aqueous two-phase
System, target product nimbin is enriched in upper surface activating agent phase, and small molecular weight impurity and carbohydrate are enriched in lower floor's water phase, takes out
Upper phase, gained extract solution is fitted into the bag filter of 600~1000Da of retention, is dialysed with deionized water, obtains preliminary purification
Nimbin.
Specific process conditions and recovery rate correspondence such as table 1 below：
Table 1 is the process conditions and recovery rate of various embodiments of the present invention
Surfactant used is nonionic surface active agent or ionic surfactant in the various embodiments described above
Agent, nonionic surface active agent is Triton X-100, Tween-20, Tween-80, polyoxyethylene fatty acid ester, 12
Any one or any combination in alcohol APEO and NPE,.Ionic surfactant can
Being sodium dodecylbenzenesulfonate, lauryl sodium sulfate, cetyl trimethylammonium bromide, dodecyl dimethyl benzyl
Any one or any combination in ammonium chloride and OPEO sulfate,.
Thus also can be explained, the effect of nonionic surface active agent involved in the present invention and ionic surfactant
Effect it is identical, its effect is close, and the raising for recovery rate can form aqueous two-phase with inorganic salt solution, and in ultrasonic bar
Synergy is produced under part, it is ensured that recovery rate is more than 0.5%.
The product extracted to the various embodiments described above with high performance liquid chromatograph identifies that the chromatogram of products therefrom is such as
Shown in Fig. 2, it is compared with chromatogram Fig. 1 of commercially available nimbin A mark product, as a result can be seen that：Nimbin A marks product liquid
Mutually the retention time at detection peak is 13.937min；Under identical liquid-phase condition, products therefrom has maximum inspection at 13.961min
Survey peak, and peak shape it is sharp, without hangover, illustrate can effectively to be extracted containing content nimbin A higher, the i.e. present invention in product,
Separate nimbin A.
In order to verify technique effect of the invention, applicant done it is substantial amounts of verified, be with following experiments now
Example is illustrated.
Comparative example 1
Conventional ultrasound-organic solvent extraction：Ethanol cooks extractant；Solid-liquid ratio 1:2；Ultrasonic power density is 2.5W/
cm2, ultrasonic time is 50min, and recovery rate is 0.36%.
Comparative example 2
Conventional ultrasound-ethanol aqueous two-phase extraction method：Ethanol aqueous two-phase composition is the sulphur of addition 0.62g/mL in 75% ethanol
Sour ammonium, solid-liquid ratio is 1:10(g:mL)；Power density is 2.4w/cm2；Ultrasonic time is 60min, and recovery rate is 0.32%.
Comparatively speaking, nimbin A recovery rates of the invention are up to more than 0.5%, and low cost of the invention, by-product
Thing is few.
Claims (8)
1. a kind of method that surfactant collaboration aqueous two-phase extracts nimbin, it is characterised in that comprise the steps of：
(1) chinaberry seed natural air drying will be printed, peeling, benevolence oil expression, the cake ground-slag after deoiling is broken, crosses 40~60 mesh sieves, is gone
Oily benevolence powder, it is standby；
(2) aqueous surfactant solution that mass fraction is 1%~10% is prepared, is 1 by solid-liquid ratio:The ratio of 5~25g/mL
Addition is deoiled benevolence powder, is 2~10W/cm in ultrasonic power density2, supersonic frequency be that 25~60kHz, ultrasonic radiation mode are
Ultrasonically treated 15~20min under the ultrasound condition of 10s~15s/20s, ultrasonic transmitting element be distributed in extract chamber side wall and
Bottom；
(3) inorganic salts are added in the extraction system according to the ratio that mass fraction is 5%~15% to step (2), stirring and dissolving,
Double-aqueous phase system is formed, target product nimbin is enriched in upper surface activating agent phase, and small molecular weight impurity and carbohydrate are enriched in down
Layer water phase, phase in taking-up, purifying obtains nimbin.
2. the method that surfactant collaboration aqueous two-phase according to claim 1 extracts nimbin, it is characterised in that：It is described
The surfactant of step (2) is nonionic surface active agent or ionic surfactant.
3. the method that surfactant collaboration aqueous two-phase according to claim 2 extracts nimbin, it is characterised in that：It is described
Nonionic surface active agent is Triton X-100, Tween-20, Tween-80, polyoxyethylene fatty acid ester, lauryl alcohol polyoxy
Any one or more combination in vinethene and NPE.
4. the method that surfactant collaboration aqueous two-phase according to claim 2 extracts nimbin, it is characterised in that：It is described
Ionic surfactant is sodium dodecylbenzenesulfonate, lauryl sodium sulfate, cetyl trimethylammonium bromide, 12
The combination of any one or more in zephiran and OPEO sulfate.
5. the method that surfactant collaboration aqueous two-phase according to claim 1 extracts nimbin, it is characterised in that：It is described
Inorganic salts are any one or any combination in dipotassium hydrogen phosphate, disodium hydrogen phosphate, sodium nitrate and potassium dihydrogen phosphate.
6. the method that the surfactant collaboration aqueous two-phase according to claim 3 or 4 or 5 extracts nimbin, its feature exists
In：The purification process of the step (3) is：It is the saturating of 600~1000Da that upper surface activating agent is mutually loaded into molecular cut off
In analysis bag, dialysed with deionized water, the nimbin for being purified.
7. the method that surfactant collaboration aqueous two-phase according to claim 6 extracts nimbin, it is characterised in that：Step
(2) ultrasonic transmitting element is symmetrically distributed in the side wall for extracting chamber, and two ultrasonic transmitting elements being oppositely arranged
The distance between be ultrasonic wavelength integral multiple.
8. the method that surfactant collaboration aqueous two-phase according to claim 7 extracts nimbin, it is characterised in that described
Step (2) is specifically：The aqueous surfactant solution that mass fraction is 5%~8% is prepared, is 1 by solid-liquid ratio:10~20g/mL
Ratio add and deoil benevolence powder, be 5~10W/cm in ultrasonic power density2, supersonic frequency be 28~50kHz, ultrasonic radiation
Mode is ultrasonically treated 15~20min under the ultrasound condition of 10s~15s/20s, and ultrasonic transmitting element is distributed in and extracts chamber
Side wall and bottom, are symmetrical on the wall of side, and the distance between two ultrasonic transmitting elements being oppositely arranged are ultrasounds
The integral multiple of wavelength, forms resonance and standing wave come in promoting aqueous surfactant solution fully to dissolve raw material under turbidity state
Nimbin.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413166A (en) * | 2019-11-08 | 2020-07-14 | 杭州师范大学 | Method for extracting and enriching phenolic substances in dendrobium nobile |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN102430265A (en) * | 2011-09-26 | 2012-05-02 | 武汉大学 | Aqueous two-phase extraction system of mixed surfactant |
| CN103191581A (en) * | 2013-04-09 | 2013-07-10 | 江苏大学 | Method for separating/gathering trace ciprofloxacin in food |
| CN103432193A (en) * | 2013-09-10 | 2013-12-11 | 武汉工程大学 | Microwave-assisted aqueous two-phase extraction and separation method of kudzu root total flavones |
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- 2016-11-25 CN CN201611062098.9A patent/CN106749340B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102319282A (en) * | 2011-09-21 | 2012-01-18 | 武汉工程大学 | Aqueous two-phase extraction method for total flavones in kudzu root |
| CN102430265A (en) * | 2011-09-26 | 2012-05-02 | 武汉大学 | Aqueous two-phase extraction system of mixed surfactant |
| CN103191581A (en) * | 2013-04-09 | 2013-07-10 | 江苏大学 | Method for separating/gathering trace ciprofloxacin in food |
| CN103432193A (en) * | 2013-09-10 | 2013-12-11 | 武汉工程大学 | Microwave-assisted aqueous two-phase extraction and separation method of kudzu root total flavones |
Non-Patent Citations (2)
| Title |
|---|
| 《声学技术》 * |
| 《陕西师范大学学报（自然科学版）》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111413166A (en) * | 2019-11-08 | 2020-07-14 | 杭州师范大学 | Method for extracting and enriching phenolic substances in dendrobium nobile |
| CN111413166B (en) * | 2019-11-08 | 2023-02-14 | 杭州师范大学 | Method for extracting and enriching phenolic substances in dendrobium nobile |
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Granted publication date: 20181102 Termination date: 20211125 |