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Restricted access poly (styrene-co-divinyl benzene)-coated silica gel chromatographic packing and preparation method thereof

A technology of silica gel chromatography and divinylbenzene, applied in chemical instruments and methods, material separation, analysis of materials, etc., can solve the problem of high cost, achieve the effects of reducing loss, good exclusion effect, and reducing catalytic rate

Inactive Publication Date: 2012-02-01
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, restricted fillers have been reported in the literature (Anal.Bioanal.Chem., 2006, 384: 1462-1469; J.Chromatogr.B, 2004, 801: 141-156), but some methods in the literature require Introduce hydrophilic groups on the outer surface of silica gel by enzymatic hydrolysis, resulting in high cost, and there is no commercial limited-access chromatographic material in my country

Method used

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  • Restricted access poly (styrene-co-divinyl benzene)-coated silica gel chromatographic packing and preparation method thereof
  • Restricted access poly (styrene-co-divinyl benzene)-coated silica gel chromatographic packing and preparation method thereof
  • Restricted access poly (styrene-co-divinyl benzene)-coated silica gel chromatographic packing and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] 1. Preparation of ATRP initiator-immobilized silica gel

[0053] Weigh 15.0 g of activated silica gel microspheres, disperse them in 150 ml of dry toluene, and 2 Under protection, 18.0 ml of γ-aminopropyltrimethoxysilane reagent was added, stirred and refluxed at 110° C. for 12 hours. The reaction product was suction-filtered, washed with toluene, acetone, and in turn. Vacuum drying at 60°C, the product is marked as Sil-NH 2 .

[0054] Sil-NH 2 Transfer to a round-bottomed flask, add 120 ml of dry cyclohexanone, stir to disperse, and 2 Under protection, 30 ml of cyclohexanone solution containing 9.98 g of 4-chloromethylbenzoyl chloride was added dropwise in an ice-water bath, and 1.2 ml of pyridine was added, and the reaction was stirred at room temperature for 18 hours. After the reaction, the product was suction-filtered, and then Soxhlet extracted with acetone, and the obtained product was labeled as Sil-Cl. Dry in a vacuum oven at 60°C for later use.

[0055]...

Embodiment 2

[0061] The 2nd step in embodiment 1 adopts following experimental condition: pass N 2 Under gas conditions, add 2.5 grams of Si-Cl (initiator content is 1.3 mmol / g) in the there-necked flask after drying, 14 milliliters of toluene, mechanical stirring makes silica gel disperse, adds styrene 3.6 grams (34.6 mmol) successively , 0.34 g (3.4 mmol) of cuprous chloride and 1.07 g (6.9 mmol) of 2,2′-bipyridine, heated at 110° C. in an oil bath, and refluxed for 4 hours to obtain polystyrene-coated silica gel. The product is sequentially washed with ethanol and Na 2 Washing with saturated EDTA solution, then Soxhlet extraction with acetone for 12 hours, vacuum drying at 50°C for later use, to obtain polystyrene-coated silica gel, the carbon content was 25.4% as determined by elemental analysis.

Embodiment 3

[0063] The second step in Example 1 adopts the following experimental conditions: add 2.5 grams of Si-Cl (initiator content is 0.6 mmol / g) and 8 milliliters of toluene to the dried there-necked flask, mechanically stir to disperse the silica gel, and then add 0.73 g (7.02 mmol) of styrene, 0.83 g (6.38 mmol) of divinylbenzene, 0.4 g (2.56 mmol) of 2,2′-bipyridine, 0.125 g (1.26 mmol) of cuprous chloride, oil The bath was heated at 110° C. and refluxed for 2 hours to obtain poly(styrene-co-divinylbenzene)-coated silica gel. The product is sequentially washed with ethanol and Na 2 Wash with saturated EDTA solution, then Soxhlet extract with acetone for 12 hours, and vacuum-dry at 50°C for later use. The carbon content is 26% as measured by elemental analysis.

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Abstract

The invention relates to restricted access poly (styrene-co-divinyl benzene)-coated silica gel chromatographic packing and a preparation method thereof. The preparation method comprises the following steps of: introducing an atom transfer radical polymerization (ATRP) initiator into the surface of porous silica gel microspheres and coating poly (styrene-co-divinyl benzene) on the surface of silica gel through the grafting from method; then grafting polyglycidyl methacrylate on the surface of the coated layer; and further performing hydrolysis to get the hydrophilic surface so as to get the restricted access poly (glycidyl methacrylate-g-(styrene-co-divinyl benzene))-coated silica gel chromatographic packing. The polymer-coated silica gel chromatographic packing has the functions of combining with hydrophobic micromolecules and excluding biological macromolecules, and can perform effective separation on hydrophobic compounds in biological complex samples under the situation of eliminating the protein precipitation pretreatment process, be used as a chromatographic stationary phase or a solid-phase extraction agent, perform direct sample introduction, separation, extraction and determination on micromolecular compounds in biological or environmental samples and further realize the high-efficiency analysis and determination of micromolecular substances in a biological system.

Description

technical field [0001] The invention relates to a feed-limited poly(styrene-co-divinylbenzene)-coated silica gel chromatographic filler and a preparation method, belonging to the field of novel chromatographic separation materials. This limited-feed multifunctional separation material can be applied to the extraction of hydrophobic small molecular substances in biological or environmental samples and the direct injection chromatographic separation analysis, eliminating the need for pretreatment processes such as protein precipitation, and achieving the goal of analyzing small molecular substances in complex biological systems. The purpose of efficient analysis and determination. Background technique [0002] Biological and environmental samples have complex matrix components and low concentrations of analytes, requiring proper pretreatment before determination. Due to the advantages of high recovery, low reagent consumption and easy automation, solid-phase extraction has be...

Claims

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Application Information

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IPC IPC(8): G01N30/14B01J20/30B01J20/283
Inventor 董襄朝徐丹
Owner NANKAI UNIV
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