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Preparation method of gas chromatographic column for detection of chiral pesticide residues in food

A technology for pesticide residue detection and gas chromatographic columns, which is applied in the field of gas chromatographic column production, can solve the problems of stationary phase loss, the maximum allowable use temperature can not be too high, and achieve the effect of stable performance

Active Publication Date: 2017-07-14
ZHONGBIAO TESTING HENAN SERVICE +1
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

However, the traditional preparation method of chiral gas chromatography column is to coat the stationary phase on the inner wall of the capillary, and the loss of the stationary phase is serious at high temperature, so the maximum allowable use temperature of these chiral columns is often not very high

Method used

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  • Preparation method of gas chromatographic column for detection of chiral pesticide residues in food
  • Preparation method of gas chromatographic column for detection of chiral pesticide residues in food
  • Preparation method of gas chromatographic column for detection of chiral pesticide residues in food

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specific Embodiment

[0027] A specific embodiment according to the present invention is as follows:

[0028] (1) Synthetic stationary phase

[0029] 10 g of β-cyclodextrin was added to 150 g of chlorodimethyl ether (CH 3 (CH 2 ) 2 OCH 2 Cl), adding into aqueous sodium hydroxide solution, keeping pH = 10.5, reaction temperature at 80° C., reacting for 6 hours, stopping heating, and synthesizing a mixed solution containing cyclodextrin derivatives.

[0030] (2) Functionalization of stationary phase

[0031] Weigh 58g of 3-[(2,3)-glycidyloxy]propyltrimethoxysilane, dissolve it in 124g of ethanol, add the mixture obtained in (1) to the ethanol solution, and ultrasonicate while adding Stir and react for 2 hours; add 32.5g monomer tetramethoxysilane and catalyst hydrochloric acid solution, keep pH = 4.5, heat to 60°C, ultrasonically stir, react for 4 hours, then add sodium hydroxide solution to adjust to neutral; After centrifugation, the precipitate was filtered off to obtain a clear liquid.

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Abstract

A production method of a gas chromatography column for chiral pesticide residue detection in food comprises the following steps: (1) hydrogen of 2,6-site hydroxyl groups of cyclodextrin is substituted into ether for synthesis of a cyclodextrin derivative; (2) the synthesized cyclodextrin derivative is reacted with 3-[(2,3)-epoxy propoxy] propyl trimethoxysilane in an ethanol solution, monomer tetramethoxysilane and a catalyst hydrochloric solution are added, and a clear liquid is obtained by reaction separation; (3) quartz capillary inner surface is pre-treated for formation of silicon hydroxyl on the quartz capillary inner surface; and (4) the clear liquid is filled into a capillary column to prepare the gas chromatography column. The gas chromatography column prepared by the method can be applied to chiral pesticide residue detection in grains, vegetables and fruits and other a variety of foods.

Description

technical field [0001] The invention relates to a manufacturing method of a gas chromatographic column, in particular to a manufacturing method of a gas chromatographic column used for detection of chiral pesticide residues in food. Background technique [0002] Among the currently used pesticides, chiral pesticides account for about a quarter, and the detection of chiral pesticide residues in food is an important means to ensure food safety. This kind of analysis and detection work is generally realized by chromatographic methods, especially by direct separation on chromatographic chiral stationary phases. Among them, the gas chromatographic chiral stationary phase method is characterized by its fast, sensitive, good separation performance, accurate quantification, and does not use organic The advantages of solvents have attracted people's attention, and the fastest-growing and most widely used chiral stationary phases in the research of chiral separation in gas chromatogra...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/60
CPCG01N30/60G01N2030/025
Inventor 赵林萍苏永恒李梦雨贾松涛王继美康雪梅李小民
Owner ZHONGBIAO TESTING HENAN SERVICE