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Large-volume sample injection-variable temperature focusing supercritical fluid chromatography mass spectrometry analysis system and analysis method

A large-volume sample injection and chromatographic column technology, which is applied in the field of analytical chemistry chromatography analysis, can solve problems such as solvent incompatibility, achieve the effects of reducing solubility, ensuring stable response, and improving chromatographic peak broadening

Active Publication Date: 2021-11-19
SOUTH CHINA UNIV OF TECH
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Problems solved by technology

[0004] Based on this, the present invention provides a large-volume sampling-variable temperature focusing supercritical fluid chromatography mass spectrometry system, which intends to solve the problem of solvent incompatibility in supercritical fluid chromatography, thereby avoiding the problem of chromatographic peak broadening caused by large-volume sampling, Improve the chromatographic peak shape of the compound and increase the sensitivity of the analysis

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Embodiment 1

[0069] Using the large-volume sampling-variable temperature focusing supercritical fluid chromatography-mass spectrometry system and its analysis method of the present invention, 18 kinds of metabolites in the brain tissue of depressed rats were analyzed and detected. The 18 kinds of lipids are CE(20:4), TG(50:1), TG(52:1), TG(54:4), FA(17:1), AA, DHA, Cholesterol, DG(16 :1 / 22:5 / 0:0), DG(18:2 / 22:5 / 0:0), PC(32:2), MG, OEA, Cer(d18:1 / 16:0), Cer (42:2), PA(16:0 / 18:1), SM(d18:2 / 24:0), LPC(20:4), LPE(18:0), LPI(18:0).

[0070] In this embodiment, the volume of the quantitative loop 6 built into the column thermostat 7 is 20 μL, and the model of the chromatographic column 10 is Waters ACQUITY Torus TM DIOL column (3.0mm×100mm, 1.7μm, ).

[0071]The sample pretreatment method is as follows: Weigh 1 mg of freeze-dried brain tissue powder into a 1.5 mL centrifuge tube, add 400 μL of chloroform, shake at 1500 rpm for 30 minutes at 4°C; add 300 μL of pure water, vortex for 3 minutes...

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Abstract

The invention relates to a large-volume sample injection-variable temperature focusing supercritical fluid chromatography mass spectrometry analysis system. The system comprises a modifier pump, a carbon dioxide pump, a mixer, an automatic sample injector, a six-way valve for switching flow paths, a quantitative loop, a column oven, a trace preheater, a chromatographic column, a supplement pump, a three-way connector, a back pressure regulator, a mass spectrum detector and a connecting pipeline for connecting all the components, wherein the mixer, the trace preheater and the chromatographic column are arranged in the column oven. The invention also relates to an analysis method using the system. The analysis method comprises the following steps of (1) changing temperature; (2) loading a sample by an automatic sample injector; (3) performing large-volume sample injection-column head focusing; and (4) performing chromatographic separation and mass spectrometry. According to the method, a problem of solvent incompatibility in supercritical fluid chromatography is solved, so a problem of chromatographic peak broadening caused by large-volume sample introduction is avoided, the chromatographic peak shape of a compound is improved, and analysis sensitivity is improved.

Description

technical field [0001] The invention belongs to the field of analytical chemistry chromatographic analysis methods, in particular to a large-volume sampling-variable temperature focusing supercritical fluid chromatographic mass spectrometry analysis system and analysis method. Background technique [0002] Supercritical fluid chromatography (SFC), as a high-throughput chromatographic separation technique with fast analysis speed, high accuracy and high sensitivity, has been widely used in the separation of chiral enantiomers and the detection of biological metabolites in recent years. Food analysis, rapid quantification of active ingredients in natural products, lipidomics and metabolomics research and other fields. The most commonly used mobile phase in supercritical fluid chromatography is supercritical carbon dioxide. Compared with other supercritical fluids, the operating conditions of supercritical carbon dioxide are relatively simple (7.39MPa, 31.1°C). Compared with ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/24G01N30/30
CPCG01N30/02G01N30/72G01N30/24G01N30/30
Inventor 周婷冯洁清金文彬
Owner SOUTH CHINA UNIV OF TECH
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