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Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof

A high-speed countercurrent chromatography and accelerated solvent technology, which is applied in solvent extraction, separation methods, chemical instruments and methods, etc., can solve the problem of low sample utilization, shorten extraction time, increase product yield, and achieve high purity.

Inactive Publication Date: 2010-02-03
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although accelerated solvent extraction and high-speed countercurrent chromatography are widely used in the fields of natural products, food, and medicine, the defect of accelerated solvent extraction is that the utilization rate of samples is low, and high-speed countercurrent chromatography alone also has certain defects. and both are still under independent research status

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  • Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof
  • Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof
  • Method for combined use of accelerated solvent extraction and high speed countercurrent chromatogram and device thereof

Examples

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Effect test

Embodiment 1

[0041] (Using ASE-preparative HSCCC to separate and purify isoferidin in Sargassum)

[0042]The specific operation is: Weigh 2.0g of 20-40mesh Sargassum sample into a 22mL ASE extraction tank, use HSCCC mobile phase as the extraction solution, extract at 100°C and 100bar pressure for 10min, cycle extraction twice, collect and extract liquid (for the high performance liquid chromatogram of Sargassum extract, please refer to image 3 shown), the extract is directly pumped into the preparative HSCCC for purification and preparation, and the waste liquid during the sampling process is collected into the waste liquid bottle 11. The conditions of preparative HSCCC: injection volume 10mL, solvent system is n-hexane: ethyl acetate: methanol: water=1:2:1:2 (volume ratio), column volume is 240mL, rotating speed 800rpm, above phase n-hexane / Ethyl acetate was used as the stationary phase, methanol / water as the lower phase was used as the mobile phase, and the flow rate was 2.0mL / min; ...

Embodiment 2

[0044] (Using ASE-analytical HSCCC to separate and purify Isoferidin in Sargassum)

[0045] The specific operation is: Weigh 2.0g of 20-40mesh Sargassum sample in a 22mL extraction tank, use HSCCC mobile phase as the extraction solution, extract at 100°C and 100bar pressure for 10min, cycle extraction twice, and collect the extraction solution (For the high-performance liquid chromatogram of Sargassum extract, please refer to image 3 shown), the extract is directly pumped into the analytical HSCCC for purification and separation, and the waste liquid during the sampling process is collected into the waste liquid bottle 11. Analytical high-speed countercurrent chromatography conditions: injection volume 2mL, solvent system is n-hexane: ethyl acetate: methanol: water = 1:2:1:2 (volume ratio), column volume is 43mL, rotation speed is 1600rpm, the above phase is n-hexane / ethyl acetate as the stationary phase, the lower phase methanol / water as the mobile phase, the flow rate ...

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Abstract

The invention discloses a method for the combined use of accelerated solvent extraction and high speed countercurrent chromatogram and a device thereof. An accelerated solvent extraction device extracts a material so as to obtain an extraction liquid which is collected by a liquid storage bottle. The extraction liquid is pumped by a peristaltic pump into a dosing ring. Stationary phase in the liquid storage bottle is pumped by a plunger pump into a high speed countercurrent chromatography. The high speed countercurrent chromatography is started, and simultaneously the plunger pump is used forpumping flowing phase in the liquid storage bottle into the high speed countercurrent chromatography for purpose of solvent system balance. Sample solution in the dosing ring is pumped into the high speed countercurrent chromatography. A preparing-type high speed countercurrent chromatogram is used for purification and preparation so as to obtain a target component, or an analysis-type high speedcountercurrent chromatogram is used for analyzing the target component in a natural product extract liquid. The above steps are integrated with the accelerated solvent extraction and the high speed countercurrent chromatogram by utilizing a switch valve, thereby realizing the online extraction, separation, purification and preparation of the natural product effective component and having the advantages of fastness, high efficiency and high automation. The method and the device have a wide application prospect in the fields such as food, medicine, biology and the like.

Description

technical field [0001] The invention relates to an accelerated solvent extraction-high-speed countercurrent chromatography (ASE-HSCCC) combined method, and an accelerated solvent extraction-high-speed countercurrent chromatography combined device for implementing the method, which is suitable for the detection of target components in the fields of food, medicine, biology, etc. Extraction separation, purification preparation or analysis. Background technique [0002] The traditional off-line natural product extraction, separation and purification preparation process is cumbersome and time-consuming, which easily leads to the loss of target components, and the extraction rate and recovery rate are low. Accelerated solvent extraction (ASE) is an extraction technique that increases the solubility of substances and the diffusion rate of solutes by increasing temperature and pressure, thereby improving extraction efficiency. It has the advantages of time saving, less solvent consu...

Claims

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Application Information

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IPC IPC(8): B01D11/00B01D15/04
Inventor 李攻科邓建朝肖小华
Owner SUN YAT SEN UNIV
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