CN104892411A - Method for separating and extracting microcomponent monoglyceride from coix seed oil - Google Patents
Method for separating and extracting microcomponent monoglyceride from coix seed oil Download PDFInfo
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- CN104892411A CN104892411A CN201510332491.4A CN201510332491A CN104892411A CN 104892411 A CN104892411 A CN 104892411A CN 201510332491 A CN201510332491 A CN 201510332491A CN 104892411 A CN104892411 A CN 104892411A
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- monoglyceride
- moving phase
- chromatographically pure
- oily matter
- concentrated
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Liquids With Adsorbents In General (AREA)
- Fats And Perfumes (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a method for separating and extracting microcomponent monoglyceride from coix seed oil. The method comprises the following steps: (1), the coix seed oil is diluted with petroleum ether and is applied to on a chromatographic column Silica flash column for isocratic elution through a medium-pressure preparation system, and flow components are shunted and detected by an evaporative light-scattering detector; (2), a prepared target peak receiving solution is concentrated to obtain an oily matter; (3), the oily matter is detected by a TLC (thin layer chromatography) silica gel plate; (4), the oily matter is applied to an Innoval C18 chromatographic column for gradient elution through a high-pressure preparation system, flow components are shunted and detected by an evaporative light-scattering detector, and receiving solutions of target peaks are collected; (5), the receiving solutions of the target peaks are concentrated respectively until no solvent flows out; (6), concentrated solutions are subjected to reversed phase liquid chromatography detection to obtain two types of monoglyceride monomer components with the purity higher than 95%. The microcomponents are obtained from a complex matrix, the period for one-time separation is 3-4 h, time is saved, and the operation is easy.
Description
Technical field
The present invention relates to a kind of preparative chromatography method, particularly relate to and a kind ofly from Semen Coicis oil, be separated the method for monoglyceride of obtaining.
Background technology
In Semen Coicis oil, the content of triglyceride level is up to 87% ~ 95%, and secondly, and the content of monoglyceride belongs to trace for the content of triglyceride, and be multi-component mixture, separating difficulty greatly,
In Semen Coicis oil, the acquisition of monoglyceride is tested for research Semen Coicis oil composition and pharmacological toxicology and is had very large meaning.But not yet there is the report that in Semen Coicis oil, monoglyceride extracts at present.
Summary of the invention
The object of this invention is to provide the method for a kind of favorable reproducibility separation and Extraction Trace Components monoglyceride from Semen Coicis oil.
Technical scheme of the present invention is summarized as follows:
From Semen Coicis oil, a method for separation and Extraction Trace Components monoglyceride, comprises the steps:
(1) get the sherwood oil dilution doubly of 5-25mL Semen Coicis oil 1-5 volume, press preparation system in passing through, at chromatographic column Silica flash post, moving phase: A is chromatographically pure sherwood oil, and B is chromatographically pure dehydrated alcohol, isocratic elution; Flow point detects with light scattering detector after shunting;
(2) by the target peak receiving liquid for preparing in Rotary Evaporators at 34 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa, obtain oily matter;
(3) oily matter TLC silica-gel plate, the sherwood oil of developping agent to be volume ratio be 85:14:1: acetone: formic acid detects; The Rf of target compound is 0.1;
(4) oily matter is used high pressure preparation system, in Innoval C18 chromatographic column, packing material size is 6 μm, and aperture is
moving phase: C is chromatographically pure acetonitrile, and D is chromatographically pure methylene dichloride, gradient elution; Flow point detects with light scattering detector after shunting, collects the receiving liquid of the target peak of retention time difference 11min and 14min;
(5) by the receiving liquid of each target peak that obtains respectively at Rotary Evaporators at 32 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa;
(6) concentrated solution detects through reversed-phase liquid chromatography, and testing conditions is: Innoval C18 chromatographic column, light scattering detector, moving phase: A is chromatographically pure sherwood oil, B is chromatographically pure dehydrated alcohol, isocratic elution, and obtaining 2 kinds of purity is more than 95% monoglyceride monomer component.
The filler specification of Silica flash post be preferably 20 ~ 35 μm,
spherical silica gel.
Step (1) described isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min.
Step (4) described gradient elution is: 0 ~ 16min, moving phase D keep 25%; 16 ~ 16.1min, moving phase D is from 25% to 60%; 16.1 ~ 23min, moving phase D keep 60%; 23.1 ~ 30min, moving phase D is from 60% to 25%.
Step (6) described isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min.
Advantage of the present invention:
1. make use of positive enrichment, the feature of reverse phase separation, obtains minor component from complex matrices;
2. the cycle of flash liberation is 3 ~ 4 hours, saves time easy to operate;
3. the present invention's separation and Extraction Trace Components monoglyceride from Semen Coicis oil is tested for research Semen Coicis oil composition and pharmacological toxicology and is had very large meaning.
Accompanying drawing explanation
Fig. 1 method of the present invention once prepares enrichment monoglyceride color atlas.(wherein 50 ~ 54min chromatographic peak is an ester products)
One ester component to be separated by method of the present invention and to obtain 10 ~ 12min, 13.2 ~ 14.4min, two monoglyceride monomers by Fig. 2 again.All the other peaks are triglyceride.
10 ~ 12min cut purity detecting after Fig. 3 is separated again.
13.2 ~ 14.4min cut purity detecting after Fig. 4 is separated again.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
From Semen Coicis oil, a method for separation and Extraction Trace Components monoglyceride, comprises the steps:
(1) get the sherwood oil dilution doubly of 10mL Semen Coicis oil 3 volumes, press preparation system in passing through, at chromatographic column Silica flash post, moving phase: A is chromatographically pure sherwood oil, and B is chromatographically pure dehydrated alcohol, isocratic elution; Flow point detects with light scattering detector after shunting; The filler specification of Silica flash post is 20 ~ 35 μm,
spherical silica gel; Isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min, sees Fig. 1;
(2) by the target peak receiving liquid for preparing in Rotary Evaporators at 34 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa, obtain oily matter;
(3) oily matter TLC silica-gel plate, the sherwood oil of developping agent to be volume ratio be 85:14:1: acetone: formic acid detects; The Rf of target compound is 0.1;
(4) oily matter is used high pressure preparation system, in Innoval C18 chromatographic column, packing material size is 6 μm, and aperture is
moving phase: C is chromatographically pure acetonitrile, and D is chromatographically pure methylene dichloride, gradient elution; Flow point detects with light scattering detector after shunting, collects the receiving liquid of retention time difference 11min and 14min target peak; Gradient elution is: 0 ~ 16min, and moving phase D keeps 25%; 16 ~ 16.1min, moving phase D is from 25% to 60%; 16.1 ~ 23min, moving phase D keep 60%; 23.1 ~ 30min, moving phase D is from 60% to 25%; See Fig. 2;
(5) by the receiving liquid of each target peak that obtains respectively at Rotary Evaporators at 32 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa;
(6) concentrated solution detects through reversed-phase liquid chromatography, testing conditions is: Innoval C18 chromatographic column, light scattering detector, moving phase: A is chromatographically pure sherwood oil, B is chromatographically pure dehydrated alcohol, isocratic elution, and isocratic elution is: the volume content of Mobile phase B is 28%, keep 60min, obtaining 2 kinds of purity is more than 95% monoglyceride monomer component.10 ~ 12min monoglyceride monomer 0.094 gram, 13.2 ~ 14.4min monoglyceride monomer 0.099 gram.
Embodiment 2
From Semen Coicis oil, a method for separation and Extraction Trace Components monoglyceride, comprises the steps:
(1) get the sherwood oil dilution doubly of 5mL Semen Coicis oil 5 volumes, press preparation system in passing through, at chromatographic column Silica flash post, moving phase: A is chromatographically pure sherwood oil, and B is chromatographically pure dehydrated alcohol, isocratic elution; Flow point detects with light scattering detector after shunting; The filler specification of Silica flash post is 20 ~ 35 μm,
spherical silica gel; Isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min 1;
(2)-(6) are with embodiment 1 (2)-(6);
10 ~ 12min monoglyceride monomer 0.045 gram, 13.2 ~ 14.4min monoglyceride monomer 0.047 gram.
Embodiment 3
From Semen Coicis oil, a method for separation and Extraction Trace Components monoglyceride, comprises the steps:
(1) get the sherwood oil dilution doubly of 25mL Semen Coicis oil 1 volume, press preparation system in passing through, at chromatographic column Silica flash post, moving phase: A is chromatographically pure sherwood oil, and B is chromatographically pure dehydrated alcohol, isocratic elution; Flow point detects with light scattering detector after shunting; The filler specification of Silica flash post is 20 ~ 35 μm,
spherical silica gel; Isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min 1;
(2)-(6) are with embodiment 1 (2)-(6);
10 ~ 12min monoglyceride monomer 0.221 gram, 13.2 ~ 14.4min monoglyceride monomer 0.223 gram.
Claims (5)
1. the method for separation and Extraction Trace Components monoglyceride from Semen Coicis oil, is characterized in that comprising the steps:
(1) get the sherwood oil dilution doubly of 5-25mL Semen Coicis oil 1-5 volume, press preparation system in passing through, at chromatographic column Silica flash post, moving phase: A is chromatographically pure sherwood oil, and B is chromatographically pure dehydrated alcohol, isocratic elution; Flow point detects with light scattering detector after shunting;
(2) by the target peak receiving liquid for preparing in Rotary Evaporators at 34 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa, obtain oily matter;
(3) oily matter TLC silica-gel plate, the sherwood oil of developping agent to be volume ratio be 85:14:1: acetone: formic acid detects; The Rf of target compound is 0.1;
(4) oily matter is used high pressure preparation system, in Innoval C18 chromatographic column, packing material size is 6 μm, and aperture is
moving phase: C is chromatographically pure acetonitrile, and D is chromatographically pure methylene dichloride, gradient elution; Flow point detects with light scattering detector after shunting, collects the receiving liquid of the target peak of retention time difference 11min and 14min;
(5) by the receiving liquid of each target peak that obtains respectively at Rotary Evaporators at 32 DEG C, be concentrated into solvent-free outflow under-0.9 ~-0.95Mpa.
(6) concentrated solution detects through reversed-phase liquid chromatography, and testing conditions is: Innoval C18 chromatographic column, light scattering detector, moving phase: A is chromatographically pure sherwood oil, B is chromatographically pure dehydrated alcohol, isocratic elution, and obtaining 2 kinds of purity is more than 95% monoglyceride monomer component.
2. a kind of method according to claim 1, it is characterized in that the filler specification of described Silica flash post be 20 ~ 35 μm,
spherical silica gel.
3. a kind of method according to claim 1, is characterized in that described step (1) described isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min.
4. a kind of method according to claim 1, is characterized in that described step (4) described gradient elution is: 0 ~ 16min, moving phase D keep 25%; 16 ~ 16.1min, moving phase D is from 25% to 60%; 16.1 ~ 23min, moving phase D keep 60%; 23.1 ~ 30min, moving phase D is from 60% to 25%.
5. a kind of method according to claim 1, is characterized in that described step (6) described isocratic elution is: the volume content of Mobile phase B is 28%, keeps 60min.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510332491.4A CN104892411B (en) | 2015-06-16 | 2015-06-16 | A kind of method of separation and Extraction Trace Components monoglyceride from Semen Coicis oil |
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| CN201510332491.4A CN104892411B (en) | 2015-06-16 | 2015-06-16 | A kind of method of separation and Extraction Trace Components monoglyceride from Semen Coicis oil |
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| CN104892411A true CN104892411A (en) | 2015-09-09 |
| CN104892411B CN104892411B (en) | 2016-08-17 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191134A (en) * | 2011-04-02 | 2011-09-21 | 大连理工大学 | Preparation method of partial glyceride |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102191134A (en) * | 2011-04-02 | 2011-09-21 | 大连理工大学 | Preparation method of partial glyceride |
Non-Patent Citations (2)
| Title |
|---|
| 李楠等: "HPLC法测定薏苡仁中甘油三油酸酯的含量", 《陕西科技大学学报》 * |
| 袁桂平等: "HPLC法测定薏苡仁饮片中甘油三油酸酯的含量", 《江西中医学院学报》 * |
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