CN106187727A - A kind of method extracting 6 paradol from paradise green pepper fruit - Google Patents
A kind of method extracting 6 paradol from paradise green pepper fruit Download PDFInfo
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- CN106187727A CN106187727A CN201610601987.1A CN201610601987A CN106187727A CN 106187727 A CN106187727 A CN 106187727A CN 201610601987 A CN201610601987 A CN 201610601987A CN 106187727 A CN106187727 A CN 106187727A
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- paradol
- green pepper
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
- C07C45/79—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Medicines Containing Plant Substances (AREA)
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Abstract
The present invention provides a kind of method of isolated and purified 6 paradol from paradise green pepper fruit, mainly solves prior art and extracts 6 paradol content and yield is low, containing more impurity, the problem being unfavorable for industrialized production.The method that should extract 6 paradol from paradise green pepper fruit comprises the following steps: 1] extract；2] concentrate；3] isolated and purified；4] concentration is collected.Should extract from paradise green pepper fruit the method for 6 paradol quickly, low cost, simple and effective.
Description
Technical field
The present invention relates to a kind of method extracting 6-paradol from paradise green pepper.
Technical background
Research finds, Fructus Capsici, and the piquancy component capsaicin in Fructus Piperis has the well promotion metabolic effect of body,
It is the good product of health slimming, but owing to capsaicin constituents has strong impulse effect to oral cavity and digestive organs, wants
Acquisition effective dose is extremely difficult.
Paradise green pepper is Zingiberaceae Zingiberaceae Amomum Aframomum plant paradise green pepper Aframomum
Melegueta, originates in Africa western, and its fruit and Fructus Capsici, Fructus Piperis etc. is all a kind of spice with acid.6-paradol is
Pungency component distinctive and main in spice paradise green pepper, it is similar with capsaicin chemical constitution, but its pungent only has capsaicin
One of percentage, even one thousandth, and zest is the least.
Japanese scholars finds in the clinical trial of month, and the essence that paradise green pepper is extracted has shown good fat-reducing
Effect, in tested personnel's body, metabolism is substantially accelerated, thus causes body fat proportion to reduce, and waistline reduces with hip circumference, and
And not yet find any side effect.Research shows, the 6-paradol extracted in paradise green pepper not only can efficiently enhance metabolism, and
And zest is little, have no side effect, become the new hope of fat-reducing personage's health slimming.
At present, from paradise green pepper, method content and the yield of isolated and purified 6-paradol is low, and containing more in extract
Impurity；Meanwhile, existing method complex process, the production cycle is longer, is unfavorable for industrialized production.
Summary of the invention
The present invention provides a kind of method of isolated and purified 6-paradol from paradise green pepper fruit, mainly solves prior art
Extract 6-paradol content and yield is low, containing more impurity, the problem being unfavorable for industrialized production.
The concrete technical solution of the present invention is as follows:
The method that should extract 6-paradol from paradise green pepper fruit comprises the following steps:
1] extract
By paradise green pepper sample comminution, then reflux with the organic solvent of 5～10 times of volumes or supersound extraction 2～5 times, every time
40～80min, extracting solution filters and merges；Described organic solvent is ethanol, acetone or ethyl acetate；
2] concentrate
The extracting solution preparing gained through step 1 is concentrated into proportion is 1.0～1.5, admixes concentrated solution 1～2 times of volumes
Adsorbent after, volatilize the reagent of residual；Described adsorbent is silica gel or neutral alumina；
3] isolated and purified
Joining in chromatographic column by the adsorbent processing gained through step 2, in chromatographic column, filler is sorbent used with step 2
Identical；On chromatographic column, addition petroleum ether, ethyl acetate, the mixed solvent of acetone carry out eluting again；Described petroleum ether, acetic acid second
Ester, the volume ratio of acetone are 10～8:5～3:2～1.
4] concentration is collected
Being collected the eluent containing 6-paradol, being concentrated into proportion is 0.9～1.2, obtains rich in high-load 6-
The oily product of paradol.
Chromatographic column in above-mentioned steps 3 uses dry column-packing, is first loaded in post by filler during dress post, then will inhale in step 2
Loading in post with the adsorbent of paradise green pepper, making paradise green pepper raw material is 0.9～1.1:1 with adsorbent mass ratio.
The invention have the advantages that
1] use 5～10 times amount organic phase solvent (ethanol, acetone or ethyl acetate) to extract, reduce polarity in sample
The interference of composition.
2] add adsorbent after extracting solution concentrates, make the homodisperse absorption of sample on the sorbent.
3] use silica gel or alumina column to be purified separation, effectively achieve separation and the purification of 6-paradol.
4] should extract from paradise green pepper fruit method of 6-paradol quickly, low cost, simple and effective.
Detailed description of the invention
The principle of the present invention is:
One, pretreatment of raw material: raw material pulverizing is standby.
Two, solvent extracts: for the character of 6-paradol, uses organic solvent to extract, greatly reduces polar component
Dissolution, reduces the interference of impurity component.
Three, concentrate: extracting solution is concentrated, after adding adsorbent, volatilize reagent.
Four, isolated and purified: to be purified separation with chromatographic column, observe the purification feelings of 6-paradol by thin layer chromatography simultaneously
Condition, is collected the eluent containing 6-paradol.
Five: eluent concentrates: concentrate the eluent collected, obtain producing rich in the oily of high-load 6-paradol
Product.
The detailed description of the invention of the present invention is as follows:
Embodiment one
Paradise green pepper raw material after crushed, add 8 times amount 80% ethanol, reflux, extract, 3 times, each 1 hour.Filter,
United extraction liquid.
It is 1.3 that extracting solution is concentrated into proportion, adds the silica gel of concentrated solution 1.5 times amount, after stirring, volatilizes ethanol.
Using dry column-packing, a diameter of 10cm of pretreatment column, a height of 50cm, filler used is silica gel, and its ratio is 1:1
(paradise green pepper raw material and the ratio of silica gel).The silica gel being adsorbed with sample is added on the silicagel column that fills in advance, with petroleum ether:
Ethyl acetate: the mixed solvent of acetone=8:5:2 carries out eluting, will be collected containing the eluent of 6-paradol composition.
The eluent collected is evaporated to proportion is 1.1, obtains the oily product rich in high-load 6-paradol,
The content of its 6-paradol is 78.21%.
Embodiment two
Paradise green pepper raw material after crushed, add 9 times amount acetone, reflux, extract, 3 times, each 1 hour.Filter, merge
Extracting solution.
It is 1.5 that extracting solution is concentrated into proportion, adds the silica gel of concentrated solution 1.8 times amount, after stirring, volatilizes acetone.
Using dry column-packing, a diameter of 10cm of pretreatment column, a height of 50cm, filler used is silica gel, and its ratio is 1:1
(paradise green pepper raw material and the ratio of silica gel).The silica gel being adsorbed with sample is added on the silicagel column that fills in advance, with petroleum ether:
Ethyl acetate: the mixed solvent of acetone=8:5:2 carries out eluting, will be collected containing the eluent of 6-paradol composition.
The eluent collected is evaporated to proportion is 1.1, obtains the oily product rich in high-load 6-paradol,
The content of its 6-paradol is 79.75%.
Embodiment three
Paradise green pepper raw material after crushed, adds the ethyl acetate of 10 times amount, reflux, extract, 3 times, each 1 hour.Filter, close
And extracting solution.
It is 1.0 that extracting solution is concentrated into proportion, adds the silica gel of concentrated solution 1.2 times amount, after stirring, volatilizes acetic acid second
Ester.
Using dry column-packing, a diameter of 10cm of pretreatment column, a height of 50cm, filler used is silica gel, and its ratio is 1:1
(paradise green pepper raw material and the ratio of silica gel).The silica gel being adsorbed with sample is added on the silicagel column that fills in advance, with petroleum ether:
Ethyl acetate: the mixed solvent of acetone=8:5:2 carries out eluting, will be collected containing the eluent of 6-paradol composition.
The eluent collected is evaporated to proportion is 0.9, obtains the oily product rich in high-load 6-paradol,
The content of its 6-paradol is 81.56%.
Embodiment four
Paradise green pepper raw material after crushed, add 8 times amount acetone, reflux, extract, 3 times, each 1 hour.Filter, merge
Extracting solution.
It is 1.4 that extracting solution is concentrated into proportion, adds the neutral alumina of concentrated solution 1.4 times amount, after stirring, volatilizes
Acetone.
Using dry column-packing, a diameter of 10cm of pretreatment column, a height of 50cm, filler used is neutral alumina, its ratio
Example is 1:1 (paradise green pepper raw material and the ratio of neutral alumina).It is added to fill in advance by the neutral alumina being adsorbed with sample
Neutral alumina column on, with petroleum ether: ethyl acetate: the mixed solvent of acetone=10:3:1 carries out eluting, will be containing 6-Rhizoma Zingiberis Recens
The eluent of ketone phenol composition is collected.
The eluent collected is evaporated to proportion is 1.0, obtains the oily product rich in high-load 6-paradol,
The content of its 6-paradol is 79.43%.
Embodiment five
Paradise green pepper raw material after crushed, add 9 times amount ethyl acetate, reflux, extract, 3 times, each 1 hour.Filter,
United extraction liquid.
It is 1.2 that extracting solution is concentrated into proportion, adds the neutral alumina of concentrated solution 2.0 times amount, after stirring, volatilizes
Ethyl acetate.
Using dry column-packing, a diameter of 10cm of pretreatment column, a height of 50cm, filler used is neutral alumina, its ratio
Example is 1:1 (paradise green pepper raw material and the ratio of neutral alumina).It is added to fill in advance by the neutral alumina being adsorbed with sample
Neutral alumina column on, with petroleum ether: ethyl acetate: the mixed solvent of acetone=10:3:1 carries out eluting, will be containing 6-Rhizoma Zingiberis Recens
The eluent of ketone phenol composition is collected.
The eluent collected is evaporated to proportion is 1.0, obtains the oily product rich in high-load 6-paradol,
The content of its 6-paradol is 80.17%.
Claims (2)
1. the method extracting 6-paradol from paradise green pepper fruit comprises the following steps:
1] extract
By paradise green pepper sample comminution, then reflux with the organic solvent of 5～10 times of volumes or supersound extraction 2～5 times, each 40～
80min, extracting solution filters and merges；Described organic solvent is ethanol, acetone or ethyl acetate；
2] concentrate
The extracting solution preparing gained through step 1 is concentrated into proportion is 1.0～1.5, admixes concentrated solution 1～the suction of 2 times of volumes
After attached dose, volatilize the reagent of residual；Described adsorbent is silica gel or neutral alumina；
3] isolated and purified
The adsorbent processing gained through step 2 is joined in chromatographic column, filler phase sorbent used with step 2 in chromatographic column
With；On chromatographic column, addition petroleum ether, ethyl acetate, the mixed solvent of acetone carry out eluting again；Described petroleum ether, acetic acid second
Ester, the volume ratio of acetone are 10～8:5～3:2～1；
4] concentration is collected
Being collected the eluent containing 6-paradol, being concentrated into proportion is 0.9～1.2, obtains rich in high-load 6-zingiberone
The oily product of phenol.
The method extracting 6-paradol from paradise green pepper fruit the most according to claim 1, it is characterised in that: described step
Chromatographic column in 3 uses dry column-packing, is first loaded in post by filler, then will be adsorbed with the absorption of paradise green pepper in step 2 during dress post
Agent loads in post, and making paradise green pepper raw material is 0.9～1.1:1 with adsorbent mass ratio.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610601987.1A CN106187727A (en) | 2016-07-27 | 2016-07-27 | A kind of method extracting 6 paradol from paradise green pepper fruit |
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| CN201610601987.1A CN106187727A (en) | 2016-07-27 | 2016-07-27 | A kind of method extracting 6 paradol from paradise green pepper fruit |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013185A (en) * | 2019-11-19 | 2020-04-17 | 苏州永健生物医药有限公司 | Method for enriching characteristic phenols in alligator pepper |
| WO2024032090A1 (en) * | 2022-08-11 | 2024-02-15 | 南京纽邦生物科技有限公司 | Composition and method for improving lipid metabolism function of subject |
| WO2024240211A1 (en) * | 2023-05-24 | 2024-11-28 | Nanjing Nutrabuilding Bio-Tech Co., Ltd. | Compositions and methods for improving benefit of an exercise |
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| JPH0616590A (en) * | 1992-06-30 | 1994-01-25 | Res Dev Corp Of Japan | Novel ketones, method for producing the same, and termite control agent containing the compound as an active ingredient |
| CN101018537A (en) * | 2004-08-30 | 2007-08-15 | 花王株式会社 | Wrinkle reduction agent, lipolysis accelerator, composition for external use on skin, and food or beverage composition |
| CN101735030A (en) * | 2009-12-08 | 2010-06-16 | 中国药科大学 | Method for preparing 6-shogaol |
| CN101781184A (en) * | 2010-03-23 | 2010-07-21 | 浙江工商大学 | Method for separating 6-gingerol monomer from ginger |
| CN102215857A (en) * | 2008-11-19 | 2011-10-12 | 庆熙大学校产学协力团 | Pharmaceutical composition containing ginger extract or shogaol |
| CN102260152A (en) * | 2011-06-02 | 2011-11-30 | 中国药科大学 | Preparation method and medicinal application of shogaol extract |
| CN102266547A (en) * | 2011-08-31 | 2011-12-07 | 南京财经大学 | Preparation method of ginger extract with detoxifying effect on exogenous carcinogens and product |
| CN102976909A (en) * | 2012-12-19 | 2013-03-20 | 中国科学院西北高原生物研究所 | Method for extracting and purifying 6-gingerol from ginger |
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2016
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| JPH0616590A (en) * | 1992-06-30 | 1994-01-25 | Res Dev Corp Of Japan | Novel ketones, method for producing the same, and termite control agent containing the compound as an active ingredient |
| CN101018537A (en) * | 2004-08-30 | 2007-08-15 | 花王株式会社 | Wrinkle reduction agent, lipolysis accelerator, composition for external use on skin, and food or beverage composition |
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| CN102260152A (en) * | 2011-06-02 | 2011-11-30 | 中国药科大学 | Preparation method and medicinal application of shogaol extract |
| CN102266547A (en) * | 2011-08-31 | 2011-12-07 | 南京财经大学 | Preparation method of ginger extract with detoxifying effect on exogenous carcinogens and product |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111013185A (en) * | 2019-11-19 | 2020-04-17 | 苏州永健生物医药有限公司 | Method for enriching characteristic phenols in alligator pepper |
| CN111013185B (en) * | 2019-11-19 | 2022-01-04 | 苏州永健生物医药有限公司 | Method for enriching characteristic phenols in alligator pepper |
| WO2024032090A1 (en) * | 2022-08-11 | 2024-02-15 | 南京纽邦生物科技有限公司 | Composition and method for improving lipid metabolism function of subject |
| WO2024240211A1 (en) * | 2023-05-24 | 2024-11-28 | Nanjing Nutrabuilding Bio-Tech Co., Ltd. | Compositions and methods for improving benefit of an exercise |
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Application publication date: 20161207 |