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Supercritical selective dehydration extraction-pressure swing focusing supercritical fluid chromatography online analysis system and analysis method

A supercritical fluid and selective technology, applied in the analysis of materials, material separation, instruments, etc., can solve problems such as chromatographic peak broadening, impurity interference, etc., to overcome solvent effects, expand the application range, and facilitate extraction and separation.

Active Publication Date: 2021-10-08
SOUTH CHINA UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Based on this, the present invention provides a supercritical selective dehydration extraction-pressure swing focusing supercritical fluid chromatography on-line analysis system to solve the problem of impurity interference in the sample matrix, and at the same time solve the problem of existing supercritical fluid extraction-supercritical fluid chromatography When the system is used, the problem of chromatographic peak broadening caused by the unfocusing of a large amount of extract at the head of the chromatographic column improves the accuracy and precision of the analysis and expands the application range of the online supercritical fluid extraction-supercritical fluid chromatography technology

Method used

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  • Supercritical selective dehydration extraction-pressure swing focusing supercritical fluid chromatography online analysis system and analysis method
  • Supercritical selective dehydration extraction-pressure swing focusing supercritical fluid chromatography online analysis system and analysis method
  • Supercritical selective dehydration extraction-pressure swing focusing supercritical fluid chromatography online analysis system and analysis method

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Embodiment 1

[0089] Using the supercritical selective dehydration extraction-pressure swing focusing-chromatographic on-line analysis system and its analysis method of the present invention, the four compounds of p-hydroxybenzoic acid, vanillic acid, p-hydroxybenzaldehyde and vanillin in vanilla orchid are analyzed and detected .

[0090] In this embodiment, the selective adsorbent used in the supercritical fluid extraction device 4 is a reversed-phase adsorbent, and the chromatographic column 5 is a Shim-pack UC-X RP column (the specification is 250mm×4.6mm, 3.0μm) .

[0091] In step 1), sample injection is: 5mg sample is mixed with 5mg reverse-phase adsorbent and placed in the extraction tank of 5 milliliter specification in the supercritical fluid extraction device 4, and extraction tank is put into sample holder; The pressure of the pressure regulator 8 is set to 0 MPa, and the pressure of the second back pressure regulator 9 is set to 40 MPa; the first chromatographic pump 11 pushes th...

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Abstract

The invention relates to a supercritical selective dehydration extraction-pressure-swing focusing supercritical fluid chromatographic on-line analysis system, comprising a carbon dioxide pump, a first chromatographic pump, a second chromatographic pump, a first six-way switching valve for flow path switching and The second six-way switching valve, mixer, supercritical fluid extraction device using selective adsorbent, chromatographic column, ultraviolet detector, mass spectrometer detector, three-way connector A, three-way connector B, three-way connector C , a first back pressure regulator, a second back pressure regulator and connecting pipes for connecting various components. The invention also relates to the analytical method of said system. The invention solves the problem of impurity interference in the sample matrix, and also solves the problem of chromatographic peak broadening caused by a large amount of extract liquid not focusing at the head of the chromatographic column when the existing supercritical fluid extraction-supercritical fluid chromatography system is used.

Description

technical field [0001] The invention belongs to the field of analytical chemical sample pretreatment, and specifically relates to a supercritical selective dehydration extraction-pressure variable focusing supercritical fluid chromatography online analysis system and analysis method Background technique [0002] Supercritical fluid chromatography (SFC) is a powerful tool in modern separation science. It has advantages that liquid and gas chromatography do not have, and SFC can also be used to analyze chiral or unstable compounds that are difficult to analyze in liquid or gas chromatography. Supercritical carbon dioxide is the most commonly used mobile phase in SFC because it has a moderate critical pressure and temperature (7.3MPa, 31°C), has good safety performance, is non-flammable, non-corrosive, and has low toxicity. In addition, carbon dioxide is cheap and Miscibility with most organic solvents offers a wide range of possibilities for optimizing chromatographic separat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/14G01N30/20G01N30/32
CPCG01N30/06G01N30/14G01N30/20G01N30/32G01N30/88G01N2030/062G01N2030/201G01N2030/326G01N2030/8804G01N2030/884
Inventor 周婷金文彬
Owner SOUTH CHINA UNIV OF TECH
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