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Liquid thin layer chromatography-mass spectrometry device, application and detection method

A technology of thin-layer chromatography and thin-layer chromatography plate, which is applied in the field of liquid-phase thin-layer chromatography-mass spectrometry, can solve problems that need to be improved, and achieve the effect of improving ionization efficiency and sensitivity

Active Publication Date: 2018-11-27
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the current thin-layer chromatography-mass spectrometry device, application and method of detecting samples still need to be improved

Method used

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  • Liquid thin layer chromatography-mass spectrometry device, application and detection method
  • Liquid thin layer chromatography-mass spectrometry device, application and detection method
  • Liquid thin layer chromatography-mass spectrometry device, application and detection method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] Embodiment 1 aminopyrine standard sample detection

[0062] The standard sample of aminopyrine (purchased from Sigma Company) was determined by using the liquid-phase thin-layer chromatography-mass spectrometry device according to the present invention.

[0063] Aminopyrine is made into 10 with ethanol as solvent -3 mol / L solution. Take about 0.5 μL of the prepared solution and spot it on a TLC plate that has been previously covered with a pencil substrate (a conventional 2B pencil is used to evenly coat the detection point). Then fix the top of the TLC plate closely to the adapter, and set the pencil matrix coating in the middle opposite to the laser entrance. The developer used here is a mixed solvent, that is, a mixed solvent with a volume ratio of carbon tetrachloride: ethyl acetate: methanol of 3:3:1. Draw up 500mL developer with a syringe, connect the corresponding pipeline, and fix it on the syringe pump. After everything is ready, turn on the argon auxiliary...

Embodiment 2

[0066] Embodiment 2, aminopyrine and 6-methylcoumarin mixed sample detection

[0067] The equimolar concentration and equal volume mixed samples of aminopyrine and 6-methylcoumarin were determined.

[0068] aminopyrine 10 -3 mol / L solution with 6-methylcoumarin 10 -3 mol / L ethanol solution was mixed 1:1, and 0.5 μL was spotted onto a TLC plate pre-coated with pencil matrix. All the other steps are the same as in Example 1.

[0069] Figure 4 a Overlay of ion chromatograms extracted from the mixture. It can be seen from the figure that the two chromatographic peaks have achieved baseline separation, which further proves the practical application ability of the method. Figure 4 b for Figure 4 The mass spectrum corresponding to the strongest signal in peak No. 1 in a, Figure 4 c for Figure 4 The mass spectrum corresponding to the strongest signal in a (after background subtraction).

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Abstract

The invention provides a liquid-phase thin-layer chromatography-mass spectrometry device, application and a detection method. The device comprises a thin-layer chromatographic sheet, a desorption chamber, a thin-layer chromatogram development unit and a mass spectrometry unit. The surface of the thin-layer chromatographic sheet is provided with a stationary phase; the desorption chamber is arranged on the upper surface of the thin-layer chromatographic sheet; the thin-layer chromatogram development unit is connected with the thin-layer chromatographic sheet; the mass spectrometry unit is connected with the desorption chamber. Therefore, a thin-layer chromatogram separation process and a mass spectrometry detection process can be carried out synchronously, detection time is saved, and a detection operation process is simplified.

Description

technical field [0001] The invention relates to the fields of analytical chemistry and instrument manufacturing, in particular to a liquid phase thin-layer chromatography-mass spectrometry device, application and detection method. Background technique [0002] Thin-layer chromatography (TLC), as one of the important members of the chromatographic family, is still widely used today due to its advantages of convenience, high throughput, low cost, and less solvent consumption. Thin-layer chromatography usually uses the ratio shift value of each component (R f ) for qualitative analysis, but the ratio shift value is easily disturbed by the external environment, and usually the chemical composition of the component cannot be determined, so it is difficult to use thin-layer chromatography to analyze samples qualitatively. As a powerful qualitative tool, mass spectrometry, combined with thin-layer chromatography, can alleviate the above problems. In recent years, with the rapid d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/90G01N30/94G01N30/95
CPCG01N30/90G01N30/94G01N30/95
Inventor 聂宗秀李亚峰陈素明熊彩侨侯剑张宁
Owner INST OF CHEM CHINESE ACAD OF SCI