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Method for simultaneously detecting ketose and amino sugar by gas chromatography-mass spectrometry analysis method

A gas chromatography and mass spectrometry analysis technology, applied in the direction of analyzing materials, measuring devices, material separation, etc., can solve the problem of not using amino sugars, and achieve the effect of strong specificity, reliable results, and good separation.

Inactive Publication Date: 2018-02-02
夏永刚
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is currently not applied to amino sugars and ketoses

Method used

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  • Method for simultaneously detecting ketose and amino sugar by gas chromatography-mass spectrometry analysis method
  • Method for simultaneously detecting ketose and amino sugar by gas chromatography-mass spectrometry analysis method
  • Method for simultaneously detecting ketose and amino sugar by gas chromatography-mass spectrometry analysis method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 detects the establishment of the GC-MS method of sugar ketose and amino sugar

[0031] 1. Instruments and reagents

[0032] Agilent7890A-5975C GC / MS, equipped with DB-5 capillary column (60m×0.25mm×0.25μm); standard monosaccharides: fructose (Fru), glucosamine (GlcN), galactosamine (GalN), mannose ( ManN) (sigma company); Anemarrhena purified polysaccharide (extracted and purified in our laboratory); hexamethyldisilazane (Shanghai Shiyi Chemical Reagent Co., Ltd.); Trimethylchlorosilane (Shanghai Chemical Reagent Purchase and Supply Wulian Chemical plant); pyridine (Tianjin Guangfu Science and Technology Development Co., Ltd.); trifluoroacetic acid (Tianjin Guangfu Fine Chemical Research Institute); ethanethiol (Shijiazhuang Jishi Chemical Co., Ltd.); ).

[0033] 2. Experimental methods and results

[0034] 2.2 Optimization of experimental methods

[0035] 2.2.1 Preparation of solutions by literature method

[0036] Accurately weigh four standard monos...

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Abstract

The invention discloses a method for simultaneously detecting ketose and amino sugar by a gas chromatography-mass spectrometry analysis method. According to the method, thiolation and silicon etherification derivation of samples, ketose and amino sugar in mixed monosaccharide standard solution are performed by the aid of ethanethiol-trifluoroacetic acid and hexamethyldisilazane-trimethylsilane systems, reaction products are extracted by the aid of methylene dichloride or trichloromethane, organic layers are detected by the aid of a GC-MS (gas chromatography-mass spectrometer), the ratio of peak areas of the mixed monosaccharide standard solution with different concentrations to internal standard peak areas serves as a vertical coordinate, the concentration of each monosaccharide serves asa horizontal coordinate, so that a standard curve is built, and the content of monosaccharide in sample solution is quantified by an internal standard method. The method has the advantages of high specificity, good repeatability and separation degree, reliable result and the like, and ketose and amino sugar in traditional Chinese medicines can be detected and quantified. Besides, the method can also detect glucuronic acid, galacturonic acid, glucose, galactose, mannose, rhamnose, fucose, arabinose and xylose.

Description

technical field [0001] The invention relates to a method for detecting ketose and amino sugar, in particular to a method for simultaneously detecting ketose and amino sugar by using a gas chromatography-mass spectrometry analysis method. The invention belongs to the technical field of chemical analysis and detection. Background technique [0002] GC-MS (Gas Chromatograph-Mass Spectrometer) is a combination technology of gas chromatography and mass spectrometry. GC-MS uses gas chromatography as a mass spectrometer sampling system to separate complex chemical groups; mass spectrometers are used as detectors for qualitative and quantitative analysis. The test sample is separated into a single component by GC. According to its different retention time, it flows out of the chromatographic column at the same time as the carrier gas, and passes through the interface of the molecular separator to remove the carrier gas. The retained component enters the ion source of the MS instrum...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 夏永刚梁军王天龙孙慧敏
Owner 夏永刚
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