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Restricted access poly(3-sulfopropyl methacrylate (SPM)) modified silica gel chromatographic packing

A technology of glycerol methacrylate and ethylene glycol dimethacrylate, which is applied in the field of limited-entry poly(3-sulfopropyl methacrylate) modified silica gel chromatography packing, and can solve the problem of difficult grafting density and other problems, to achieve the effect of improving analysis efficiency and accuracy, reducing loss, and uniform grafting layer

Inactive Publication Date: 2014-03-12
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are limited types of chromatographic materials in the international market, but there are still problems that need to be improved. For example, the "grafting onto" method is used when grafting polymer chains, and this method is not easy to obtain uniform grafting density.

Method used

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  • Restricted access poly(3-sulfopropyl methacrylate (SPM)) modified silica gel chromatographic packing
  • Restricted access poly(3-sulfopropyl methacrylate (SPM)) modified silica gel chromatographic packing
  • Restricted access poly(3-sulfopropyl methacrylate (SPM)) modified silica gel chromatographic packing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] 1. Activation of Matrix Silica Gel

[0033] 10g of silica gel (particle size 10μm, pore size Specific surface area 380m 2 / g) was added to 100mL of hydrochloric acid / water (1:1, v / v) solution, stirred and refluxed at 105°C for 12 hours, filtered, washed with distilled water until neutral, vacuum-dried at 100°C, and stored in a desiccator for later use.

[0034] 2. ATRP initiator grafted on the surface of silica gel (the product is marked as Silica-In)

[0035] Take 10 g of activated and dried silica gel, add 60 ml of dry toluene, add 1.5 ml of (3-(2-bromoisobutyryl) propyl) triethoxysilane under stirring, and 2 Under protection, heat to reflux at 90°C and react for 15 hours. After the reaction is complete, the product is suction-filtered and washed three times with toluene and acetone respectively. Dry under vacuum. The silica gel (marked as Silica-In) with ATRP initiator grafted on the surface was obtained.

Embodiment 2

[0037] 1. Graft poly(3-sulfonate propyl methacrylate-co-ethylene glycol dimethacrylate) on the surface of silica gel by ATRP method Weigh the Silica-In (1.0 g) prepared in Example 1 and add it to the round bottom In the three-necked flask, add 0.62 g of 3-sulfopropyl methacrylate potassium salt (SPM), 0.26 mL of ethylene glycol dimethacrylate (EDMA), 0.15 g of 2,2'-bipyridine (BiPy), CuBr 2 0.028g and DMF / H 2 O (1 / 1, v / v) 24mL, after passing nitrogen for 10min, add CuBr0.036g, and stir the reaction at 30°C for 1 hour under the protection of nitrogen. After the reaction is completed, filter the reactant with suction, wash the product with a saturated aqueous solution of EDTA until it is colorless, then wash with water, extract it with ethanol / water (1 / 1, v / v) for 12 hours, and dry it in vacuum at 50°C for 12 hours , to obtain poly(3-sulfopropyl methacrylate-co-ethylene glycol dimethacrylate) modified silica gel material, labeled as Silica-g-p(SPM-co-EDMA). The content of sul...

Embodiment 3

[0043] The poly(methacrylic acid 3-sulfonate propyl ester-co-ethylene glycol dimethacrylate) modified silica gel material Silica-g-p (SPM-co-EDMA) synthesized in the embodiment 2, dry-loaded 50mm × In the 4.6mm i.d. stainless steel chromatographic column, the HPLC method was used to investigate the effect of this material on the inorganic cation Na + , NH 4 + 、K + , Mg 2+ and Ca 2+ separation ability. The chromatographic conditions and separation results are shown in Table 1, and the chromatographic separation diagram is shown in image 3 . Depend on image 3 It can be seen that the monovalent cations can basically be separated, and the peak shape is symmetrical; the divalent cations are well separated, which shows that the chromatographic stationary phase has good cation separation performance.

[0044] Table 1 Chromatographic selectivity and column efficiency of cross-linked poly(3-propyl methacrylate) modified silica gel for cations a

[0045]

[0046] a Chrom...

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Abstract

The invention relates to restricted access poly(3-sulfopropyl methacrylate (SPM)-co-ethylene glycol dimethacrylate (EDMA)) modified silica gel chromatographic packing (Silica-g-p(SPM-co-EDMA)-g-pGMMA ([poly(glycerol monomethacrylate)]) and a preparation method thereof. The silica gel chromatographic packing is a material formed by grafting a double-layer polymer onto the surface of silica gel, and adopts poly(3-SPM-co-EDMA) as an inner layer and pGMMA as an outer layer. The expression of the silica gel chromatographic packing is Silica-g-p(SPM-co-EDMA)-g-pGMMA, wherein Silica is porous silica gel, g indicates grafting, p(SPM-co-EDMA) indicates a cross-linked polymer of 3-SPM and EDMA, and pGMMA indicates poly(glycerol monomethacrylate). The silica gel chromatographic packing can serve as a chromatographic stationary phase or a solid phase extraction material for analyzing biological samples and environmental samples, directly samples and extracts cationic compounds, and improves the analysis efficiency and accuracy. A method for measuring melamine and cyromazine in milk by online solid phase extraction / high-performance liquid chromatography coupling technology is provided and has good accuracy and reproducibility.

Description

technical field [0001] The invention relates to a limited-advance poly(3-propyl methacrylate) modified silica gel chromatographic filler, in particular to a restricted-advance poly(3-propyl methacrylate-co-ethylene glycol dimethyl Acrylate) modified silica gel chromatographic filler (Silica-g-p(SPM-co-EDMA)-g-pGMMA) and its preparation method, the material is prepared by atom transfer radical polymerization and surface initiation method, using this material as a solid phase extraction agent, A solid-phase extraction (SPE) / liquid chromatography (HPLC) online method for the determination of melamine and cyromazine in milk was established. Background technique [0002] The chromatographic separation and determination of ionic or ionizable analytes play an important role in life sciences, medicine and other fields, and have a wide range of applications. However, in the analysis of small molecules in biological samples, due to the irreversible adsorption of biomacromolecules in ...

Claims

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Application Information

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IPC IPC(8): C08F285/00C08F8/12C08F292/00C08F220/32C08F220/58C08F222/14B01J20/286B01J20/30G01N30/02
Inventor 董襄朝姜萍张颖颖朱旭东
Owner NANKAI UNIV
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