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Preparation method and application of a mercapto-bonded silver ion chromatographic column

A silver ion and chromatographic column technology, which is applied in the field of preparation of mercapto-bonded silver ion chromatographic columns, can solve the problems of complex preparation process of mercapto-bonded silver ion chromatographic columns, limitation of result accuracy and reproducibility, cumbersome manual operation, etc. , to achieve the effect of convenient laboratory preparation, large human influence factors, and short analysis time

Inactive Publication Date: 2016-05-25
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0017] The purpose of the present invention is to solve the complex preparation process of the above-mentioned thiol-bonded silver ion chromatographic column, harsh conditions, cumbersome manual operation, the accuracy and reproducibility of the obtained results are limited by experimental techniques, and the preparation of larger particle size fixed To solve the technical problems, a method for preparing a thiol-bonded silver ion chromatographic column is provided. The preparation method is easy to operate and can prepare a thiol-bonded silver ion chromatographic column with a small particle size stationary phase. The chromatographic column can be used for ultra-high performance liquid Separation of unsaturated organics, namely different types of triglycerides, in edible oils by phase chromatography or high performance liquid chromatography coupled to mass spectrometry

Method used

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  • Preparation method and application of a mercapto-bonded silver ion chromatographic column
  • Preparation method and application of a mercapto-bonded silver ion chromatographic column
  • Preparation method and application of a mercapto-bonded silver ion chromatographic column

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Embodiment 1

[0042] A preparation method for a mercapto-bonded silver ion chromatographic column, specifically comprising the following two steps:

[0043] (1) Silica gel column bonded mercaptopropyl group

[0044] Utilize the LC-30AD ultra-high performance liquid chromatograph of Shimadzu Corporation, use cyclohexane to wash the silica gel column at a flow rate of 0.5-1mL / min for 1h, take 4mL of mercaptopropyltrimethoxysilane and dissolve it in 100mL of cyclohexane, Rinse the silica gel column at a flow rate of 0.2-0.5mL / min at a column temperature of 40-80°C for 6-12h, and then wash the silica gel column with cyclohexane at a flow rate of 1mL / min at a column temperature of 40-80°C 1 -2h, then wash the silica gel column at a flow rate of 1mL / min at a column temperature of 40-80°C for 1-2h, and then maintain a constant column temperature of 40-80°C for 12-24h;

[0045] The silica gel column mentioned is the Ultimate UHPLC SIO of Yuexu Material Technology (Shanghai) Co., Ltd. 2 Silica gel...

Embodiment 2

[0060] A preparation method for a mercapto-bonded silver ion chromatographic column, specifically comprising the following two steps:

[0061] (1) Silica gel column bonded mercaptopropyl group

[0062] Using ultra-high performance liquid chromatography (Shimadzu), use cyclohexane to wash the silica gel column at a flow rate of 0.5-1mL / min for 1h, take 4mL of mercaptopropyltrimethoxysilane and dissolve it in 100mL of cyclohexane, at 40-80 Wash the silica gel column at a flow rate of 0.2-0.5mL / min for 6-12h at a column temperature of ℃, and then wash the silica gel column with cyclohexane at a flow rate of 1mL / min at a column temperature of 40-80°C for 1-2h, and then Wash the silica gel column with ethanol at a flow rate of 1mL / min at a column temperature of 40-80°C for 1-2h, then keep the column temperature at 40-80°C for 12-24h;

[0063] The silica gel column mentioned is the Ultimate UHPLC SIO of Yuexu Material Technology (Shanghai) Co., Ltd. 2 Silica gel column, the specif...

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Abstract

The invention discloses a mercapto-bonded silver ion chromatographic column and a preparation method thereof. The mercapto-bonded silver ion chromatographic column uses a liquid chromatograph and uses mercaptopropyltrimethoxysilane in the solvent cyclohexane In situ reaction with a blank silica gel chromatography column in the column to obtain a mercapto-bonded silica gel column, and then use a liquid chromatograph to directly bind silver ions to the mercapto-bonded silica gel column in situ to obtain a mercapto-bonded silver ion column. The preparation method of the mercapto-bonded silver ion chromatographic column is simple, and the particle size of the blank silica gel chromatographic column can be adjusted in the preparation process to finally obtain mercapto-bonded silver ion chromatographic columns with different small particle sizes. The column can be used for the separation and analysis of unsaturated organic matter in edible oil, especially corn oil and soybean oil, that is, different types of triglycerides in ultra-high performance liquid chromatography or liquid chromatography-mass chromatography.

Description

technical field [0001] The present invention relates to a preparation method of an effective chromatographic column, in particular to a preparation method of a mercapto-bonded silver ion chromatographic column, which is used in ultra-high performance liquid chromatography or its combination with mass spectrometry Different types of triglycerides in isolated edible oils. Background technique [0002] Silver ion chromatography is based on the unique properties of unsaturated organic compounds, that is, the ability to complex with transition metals. Unsaturated compounds act as electron donors, and silver ions act as electron acceptors to form ethylenic molecular complexes. Efficient separation of triglycerides containing different ethylenic bonds [1] . [0003] Silver ion columns are currently used to separate triglycerides containing different ethylenic bonds, mainly including the use of a single silver ion column [2] , or connect two silver ion columns in series [3] , or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30C11B7/00G01N30/60
Inventor 许旭何榕山晓琳董方圆
Owner SHANGHAI INST OF TECH
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