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Novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel

A technology of silica gel column chromatography and natural products, applied in separation methods, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of qualitative analysis deviation and inability to obtain fatty acids, achieve a large range of carbon numbers, avoid losses, The effect of improving efficiency

Inactive Publication Date: 2015-05-27
LANZHOU CENT FOR OIL & GAS RESOURCES INST OF GEOLOGY & GEOPHYSICS CAS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Researchers usually use solvents of different polarities to elute the mixture in sequence according to the strength of polarity, so it can only meet the requirements of qualitative analysis, but can't do anything for quantitative analysis or more in-depth isotope research
In particular, column chromatography itself has a very serious problem: those medium and long-chain fatty acids that are trapped in the pores or gaps of the column packing can never be obtained by simply relying on solvent elution, resulting in serious deviations in the qualitative analysis of fatty acids

Method used

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  • Novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel
  • Novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel
  • Novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel

Examples

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Effect test

Embodiment 1

[0071] Example 1 A new method for extracting fatty acids in natural products by silica gel column chromatography, comprising the following steps:

[0072] (1) Crush the solid natural product to 100-200 mesh to obtain sample powder.

[0073] (2) After the sample powder was extracted with chloroform for 72 hours, it was concentrated using a rotary evaporator at a temperature of 30°C and a pressure of 0.04MPa for 5 minutes to obtain a concentrated solution of total lipid compounds. After constant weight, add erucic acid at 1 / 30 of the weight as an internal standard (the sample does not contain erucic acid after analysis).

[0074] Among them: the mass volume ratio of sample powder to chloroform is 1 g: 3 mL.

[0075] (3) Column packing: Put 4g of 100~200mesh silica gel particles in 50mL of dichloromethane, stir to remove air bubbles, let it stand for 1h to fully swell, then put it on a glass chromatography column (450mm×9mm I.D.) It is used for later use to obtain a silica...

Embodiment 2

[0081] Example 2 A new method for extracting fatty acids in natural products by silica gel column chromatography, comprising the following steps:

[0082] (1) Crush the solid natural product to 100-200 mesh to obtain sample powder.

[0083] (2) After the sample powder was extracted with chloroform for 72 hours, it was concentrated using a rotary evaporator at a temperature of 33° C. and a pressure of 0.06 MPa for 3 minutes to obtain a concentrated solution of total lipid compounds. After constant weight, add erucic acid at 1 / 30 of the weight as an internal standard (the sample does not contain erucic acid after analysis).

[0084] Among them: the mass volume ratio of sample powder to chloroform is 5 mL.

[0085] (3) Column packing: Put 4g of 100~200mesh silica gel particles in 50mL of dichloromethane, stir to remove air bubbles, let it stand for 1h to fully swell, then put it on a glass chromatography column (450mm×9mm I.D.) It is used for later use to obtain a silica ...

Embodiment 3

[0091] Example 3 A new method for extracting fatty acids in natural products by silica gel column chromatography, comprising the following steps:

[0092] (1) Crush the solid natural product to 100-200 mesh to obtain sample powder.

[0093] (2) After the sample powder was extracted with chloroform for 72 hours, it was concentrated using a rotary evaporator at a temperature of 31° C. and a pressure of 0.05 MPa for 4 minutes to obtain a concentrated solution of total lipid compounds. After constant weight, add erucic acid at 1 / 30 of the weight as an internal standard (the sample does not contain erucic acid after analysis).

[0094] Wherein: the mass volume ratio of sample powder and chloroform is 4mL.

[0095] (3) Column packing: Put 4g of 100~200mesh silica gel particles in 50mL of dichloromethane, stir to remove air bubbles, let it stand for 1h to fully swell, then put it on a glass chromatography column (450mm×9mm I.D.) It is used for later use to obtain a silica gel...

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Abstract

The invention relates to a novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel. The method comprises the following steps: (1) crushing solid natural products so as to obtain sample powder; (2) extracting and concentrating the sample powder so as to obtain a total lipid concentrate; (3) packing by dichloromethane by a wet method so as to obtain a silica gel chromatography column A; (4) adding the total lipid concentrate into the silica gel chromatography column A so as to obtain eluant; (5) pouring out all silica gel particles in the silica gel chromatography column A, adding hydrofluoric acid for multiple times until all the silica gel particles are completely corroded, extracting so as to obtain polar fractions, and concentrating the polar fractions to obtain a concentrate A; (6) adding boron trifluoride / methyl alcohol complex solutions in the concentrate A, carrying out methyl esterification so as to obtain an esterification liquid, and extracting and concentrating the esterification liquid to obtain a concentrate B; (7) packing by ethyl acetate by a wet method so as to obtain a silica gel chromatography column B; and (8) adding the concentrate B into the silica gel chromatography column B, eluting, and carrying out spin steaming so as to obtain the fatty acid component. The novel method for extracting fatty acid in natural products by utilizing column chromatography on silica gel, which is provided by the invention, is simple and convenient in process, and is easy to operate.

Description

technical field [0001] The invention relates to the technical field of separation and purification of natural products, in particular to a novel method for extracting fatty acids in natural products by silica gel column chromatography. Background technique [0002] Fatty acids are a class of organic compounds that widely exist in natural products. There are more than 200 natural fatty acids that have been discovered so far. Many modern products such as plants and seeds are rich in polyunsaturated fatty acids (such as ?-3, ?-6), which are indispensable to the human body but cannot be synthesized by themselves. plays an important balancing role. Therefore, accurate acquisition of fatty acid composition information is an important reference standard for the medical and pharmaceutical industries. In addition, fatty acids, as a class of biomarker compounds, also have important research value in the fields of environmental science and earth science. For example, in coal, peat, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/493C07C51/47C07C57/12C07C59/125C07C59/58B01D15/08B01D15/20B01D15/42
CPCB01D15/08B01D15/206B01D15/426C07C51/47C07C51/493C07C57/12C07C59/125C07C59/58
Inventor 常江夏燕青吴应琴马素萍雷天柱孙敏卓
Owner LANZHOU CENT FOR OIL & GAS RESOURCES INST OF GEOLOGY & GEOPHYSICS CAS