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A high-efficiency separation and analysis method for active components in Enteromorpha

A technology for separation and analysis of active ingredients, applied in material separation, analysis of materials, instruments, etc., can solve problems such as short service life, high organic residues, and wide particle size distribution

Active Publication Date: 2022-04-01
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantages of macroporous resin separation are: (1) high organic residues, difficult pretreatment; (2) poor strength, serious damage during use, and short service life; (3) wide particle size distribution, poor separation effect
The disadvantages of preparative liquid phase separation mainly include: low efficiency, low yield, and unsatisfactory purification effect for overly complex mixtures

Method used

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  • A high-efficiency separation and analysis method for active components in Enteromorpha
  • A high-efficiency separation and analysis method for active components in Enteromorpha
  • A high-efficiency separation and analysis method for active components in Enteromorpha

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Sample extraction:

[0035] The dried strips of Enteromorpha enteromorpha (1 kg) were completely pulverized into powder, extracted with 3 L of 60% ethanol for 3 times, each time for 3 days, and then the extract was filtered using a vacuum filter. All extracts were combined and concentrated to no alcohol smell, and then the concentrate was extracted with an equal amount of ethyl acetate. The ethyl acetate fraction was rotary evaporated to dryness at 55 °C to obtain 10 g of crude sample, which was stored in a refrigerator at 4 °C for further HSCCC purification.

[0036] Enrichment of polyphenolic compounds in Enteromorpha segmented by gradient countercurrent chromatography:

[0037] The two-phase solvent system tert-butyl methyl ether / n-butanol / acetonitrile / water (4:0:1:5, v / v) and tert-butyl methyl ether / n-butanol / acetonitrile / water (3:1:1:5, v / v) Prepare the solvent system according to the above solvent ratio respectively, put it in a separatory funnel, shake it up an...

Embodiment 2

[0048] The difference from Example 1 is that the upper phase is directly eluted and enriched using tert-butyl methyl ether / n-butanol / acetonitrile / water (3:1:1:5, v / v) solvent system, and the remaining steps are the same as in Example 1 same, the result is as image 3 shown.

[0049] Depend on image 3 It can be seen that if only a two-phase solvent system is used, the effective components cannot be separated.

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Abstract

The invention discloses a high-efficiency separation and analysis method for active components in Enteromorpha, which comprises performing ethyl acetate extraction on the alcohol extract of Enteromorpha to obtain the Enteromorpha extract, and separating and purifying the Enteromorpha extract by high-speed countercurrent chromatography Several components, each component is carried out liquid chromatography-mass spectrometry detection; The two-phase system that high-speed countercurrent chromatography adopts comprises two kinds, and the first two-phase system is that tert-butyl methyl ether, acetonitrile, water are 3.5~4.5 by volume: 1:4.5~5.5, the second two-phase system is tert-butyl methyl ether, n-butanol, acetonitrile, water, the volume ratio is 2.5~3.5:0.9~1.1:1:4.5~5.5, when using, the first two items The lower phase of the system is used as the stationary phase, and the upper phase of the first two-phase system and the upper phase of the second two-phase system are both used as mobile phases. The invention can separate and analyze the active ingredients of polyphenols in enteromorpha.

Description

technical field [0001] The invention relates to a high-efficiency analysis method for active components of Enteromorpha, in particular to a high-efficiency separation and analysis method for active components in Enteromorpha. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Enteromorpha belongs to Chlorophyta, Ulvales, and Ulvacae in taxonomy, mainly including Enteromorpha clathrata and E.intestinalis , Enteromorpha (E.compressa), Enteromorpha (E.prolifera), and Enteromorpha (E.linza), which grow in the intertidal zone. Enteromorpha is a kind of green tide algae, which is an algae resource with high utilization value. Studies have shown that Enteromorpha is rich in nutrie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/42
CPCG01N30/02G01N30/42
Inventor 杨文鸽王宸张进杰李超徐大伦王岱杰
Owner NINGBO UNIV