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A Universal Quantitative Analysis Method for All Components by Gas Chromatography-Mass Spectrometry

A gas chromatography mass spectrometry and gas chromatography technology, which is applied in the fields of analyzing materials, measuring devices, material separation, etc., and can solve the problems that cannot be used to analyze the original data of GC-MS.

Active Publication Date: 2014-10-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In practice, some co-eluting peaks do not have characteristic ions, but the software will give all identified peaks a characteristic ion
In addition, in general the software cannot be used to analyze GC-MS raw data generated by other workstations

Method used

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  • A Universal Quantitative Analysis Method for All Components by Gas Chromatography-Mass Spectrometry
  • A Universal Quantitative Analysis Method for All Components by Gas Chromatography-Mass Spectrometry
  • A Universal Quantitative Analysis Method for All Components by Gas Chromatography-Mass Spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] 1. Sample

[0063] In this example, human serum was used as the sample. 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 100 μL serum at room temperature, add 400 μL methanol and 20 μL internal standard solution (methanol solutions of sorbic acid, tridecanoic acid and nonadecanoic acid, all 50 μg / mL), vortex for 30 seconds, Centrifuge (15000g) at 4°C for 15 min, and take 370 μL of supernatant to lyophilize. Add 50 μL of pyridine and 100 μL of BSTFA (1% TMCS) to the lyophilized sample, and derivatize in a water bath at 80° C. for 30 minutes. Derivative samples were injected and analyzed within 24 hours.

[0067] (2) GC-MS analysis conditions: chromatographic 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: 2 μ...

Embodiment 2

[0084] 1. Sample collection:

[0085]This example takes flue-cured tobacco samples as an example. Tobacco leaf samples in the middle of the flue-cured tobacco were collected and cured at 40°C until constant weight. Tobacco leaves were destemmed and crushed, passed through a 40-mesh sieve, sealed in ziplock plastic bags, 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 of tobacco powder (through a 40-mesh sieve), add it to an 11mL stainless steel extraction cell, and add 200μL of internal standard solution (2-methylnaphthalene, 2mg / mL). Install the extraction cell and receiving bottle on the accelerated solvent extraction cell. Extraction solvent, dichloromethane. The extraction temperature is 100°C, the extraction pressure is 1500psi, the number of extraction cycles is 3 times, the static extraction time is 5 minutes, and the v...

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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 complex mixed systems based on gas chromatography-mass spectrometry. Background technique [0002] Gas chromatography-mass spectrometry (GC-MS) combines the separation ability of chromatography with the qualitative function of mass spectrometry, enabling qualitative and quantitative analysis of complex mixtures. In the quantitative analysis of complex mixtures by chromatography-mass spectrometry, it is often necessary to determine characteristic ions. The compound characteristic ion in GC-MS full-scan mode refers to the mass spectrum fragment ion of a certain target compound, which only exists in the compound and does not exist in other co-eluting (that is, overlapping in chromatographic retention time) compound. If there are no co-eluting compounds for a compound, each fragment ion of the compound can...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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