Universal total-component quantitative analysis method of gas chromatography-mass spectrometry

A gas chromatography and quantitative analysis technology, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve problems that cannot be used to analyze GC-MS raw data

Active Publication Date: 2012-11-28
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In practice, some co-eluting peaks do not have characteristic ions, but the software will give all identified peaks a char

Method used

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  • Universal total-component quantitative analysis method of gas chromatography-mass spectrometry
  • Universal total-component quantitative analysis method of gas chromatography-mass spectrometry
  • Universal total-component quantitative analysis method of gas chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1. Sample

[0063] In this case, human serum is used as the sample. The serum samples were provided by Dalian Sixth People's Hospital.

[0064] 2. Analysis method

[0065] 2.1 Collection of sample total ion current chromatogram

[0066] (1) Sample pretreatment: After thawing 100μL of serum at room temperature, add 400μL methanol and 20μL internal standard solution (methanol solution of sorbic acid, tridecanoic acid and nonadenic acid, all 50μg / mL), vortex for 30s, Centrifuge (15000g) at 4°C for 15 min, and lyophilize 370 μL of the supernatant. 50μL of pyridine and 100μL of BSTFA (1% TMCS) were added to the lyophilized sample, and derivatized in a water bath at 80°C for 30 min. The derived samples were injected and analyzed within 24 hours.

[0067] (2) GC-MS analysis conditions: chromatography column: DB-5 (30m×250μm×0.25μm, J&W Scientific, Folsom, CA), carrier gas: helium (99.9995%), constant flow mode, flow rate 1.2mL / min. Injection volume: 2μL, injection port temperatur...

Embodiment 2

[0084] 1. Sample collection:

[0085] This example takes the flue-cured tobacco sample as an example. Collect tobacco leaf samples from the middle part of flue-cured tobacco, and bake them at 40°C to constant weight. The tobacco leaves were de-stemmed, crushed, passed through a 40-mesh sieve, sealed in a ziplock plastic bag, and stored in a refrigerator at 4°C.

[0086] 2. Analysis method

[0087] 2.1 Collection of sample total ion current chromatogram

[0088] (1) Extraction and concentration: accurately weigh 4.00g tobacco powder (passed through a 40-mesh sieve), add it to an 11mL stainless steel extraction tank, and add 200μL of internal standard solution (2-methylnaphthalene, 2mg / mL). Install the extraction cell and the receiving bottle on the accelerated solvent extraction cell. Extraction solvent, dichloromethane. The extraction temperature is 100°C, the extraction pressure is 1500 psi, the number of extraction cycles is 3, the static extraction time is 5 minutes, and the ex...

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Abstract

The invention discloses a universal total-component quantitative analysis method of gas chromatography-mass spectrometry. Firstly, the method employs a gas chromatography-mass spectrometry (GC-MS, full scan mode) method to obtain data information of to-be-analyzed samples, performs mass spectral de-convolution and peak identification on obtained full-scan information with an automated mass spectral deconvolution and identification system (AMDIS), extracts mass spectral information from an original data file according to results of peak identification, calculates characteristic values of compound ions, chooses characteristic ions of the compound, and finally establishes selected ion monitoring quantitative analysis method with the characteristic ions. A core of the method lies in choosing characteristic ions of the compound through the characteristic values of the compound ions. The method can give a plurality of characteristic ions and characteristic values to characteristic evaluation indexes thereof. The given characteristic ions can be used as quantitative ions and quantitative candidate ions.

Description

Technical field [0001] The invention relates to the fields of analytical chemistry and metabolomics, and is a method for quantitatively analyzing all identified compounds in a complex mixed system based on gas chromatography-mass spectrometry. Background technique [0002] Gas chromatography-mass spectrometry (GC-MS) combines the separation capabilities of chromatography with the qualitative functions of mass spectrometry, which can realize qualitative and quantitative analysis of complex mixtures. When using chromatographic mass spectrometry to quantitatively analyze complex mixtures, it is often necessary to identify characteristic ions. The characteristic ion of a compound in the full scan mode of GC-MS refers to the mass spectrum fragment ion of a target compound. This ion is only present in the compound and not in the other co-eluting (that is, the chromatographic retention time overlaps). Compound. If a compound does not have a co-eluting compound, each fragment ion of th...

Claims

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Application Information

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IPC IPC(8): G01N30/72
Inventor 许国旺李勇阮强路鑫林晓惠
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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