A kind of preparation method and application of hydrophilic methacrylamide polymer monolithic column

A technology of methacrylamide and polymers, which is applied in the field of preparation of monolithic columns of hydrophilic methacrylamide polymers, achieving good application prospects, fast and efficient separation, and good selectivity

Inactive Publication Date: 2017-01-11
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, so far, there has been no report on the use of polymeric monolithic columns for the separation of nanoparticles. Therefore, it is of great academic and practical significance to develop a new method for the separation and enrichment of nanoparticles by monolithic column capillary microextraction.

Method used

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  • A kind of preparation method and application of hydrophilic methacrylamide polymer monolithic column
  • A kind of preparation method and application of hydrophilic methacrylamide polymer monolithic column
  • A kind of preparation method and application of hydrophilic methacrylamide polymer monolithic column

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Experimental program
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Effect test

Embodiment l

[0055] 1. Preparation of methacrylamide polymer capillary monolithic column

[0056] The synthesis steps of the methacrylamide polymer monolithic column are as follows:

[0057] (1) Activation process of the capillary: Rinse the glass capillary (10 cm×1 mm) with ultrapure water for 10 min, 1.0 mol L -1 Rinse with NaOH for 2h, rinse with ultrapure water for 30min, 1.0mol L -1 Rinse with HCl for 2 hours, rinse with ultrapure water to neutrality, and dry at 160°C for 5 hours under nitrogen protection; then inject ethanol / methacryloxytrimethoxysilane (γ-MAPS) with a volume ratio of 1:1 The solution bonds double bonds to the inner wall of the capillary.

[0058] (2) Preparation of hydrophilic methacrylamide polymer monolithic column by in situ synthesis: 110 mg of AA, 120 mg of Bis, 0.08 mL of 4-VP, 0.6 mL of dodecanol, AIBN were dissolved in 0.75 mL In DMSO, a mixed solution is formed, and the content of the AIBN in the mixed solution is 1wt%. After ultrasonication for 10 min,...

Embodiment 2

[0083] The synthesis steps of the methacrylamide polymer monolithic column are as follows:

[0084] (1) Activation process of the capillary: Rinse the glass capillary (10 cm×1 mm) with ultrapure water for 10 min, 1.0 mol L -1 Rinse with NaOH for 2h, rinse with ultrapure water for 30min, 1.0mol L -1 Rinse with HCl for 2 hours, rinse with ultrapure water to neutrality, and dry at 160°C for 5 hours under nitrogen protection; then inject ethanol / methacryloxytrimethoxysilane (γ-MAPS) with a volume ratio of 1:1 The solution bonds double bonds to the inner wall of the capillary.

[0085] (2) Preparation of hydrophilic methacrylamide polymer monolithic column by in situ synthesis: 110 mg of AA, 120 mg of Bis, 0.08 mL of 4-VP, 0.6 mL of dodecanol, AIBN were dissolved in 0.75 mL In DMSO, a mixed solution is formed, and the content of the AIBN in the mixed solution is 1wt%. After ultrasonication for 10 min, inject into the activated capillary in step (1), then seal both ends with a si...

Embodiment 3

[0087] The synthesis steps of the methacrylamide polymer monolithic column are as follows:

[0088] (1) Activation process of the capillary: Rinse the glass capillary (10 cm×1 mm) with ultrapure water for 10 min, 1.0 mol L -1 Rinse with NaOH for 2h, rinse with ultrapure water for 30min, 1.0mol L -1 Rinse with HCl for 2 hours, rinse with ultrapure water to neutrality, and dry at 160°C for 5 hours under nitrogen protection; then inject ethanol / methacryloxytrimethoxysilane (γ-MAPS) with a volume ratio of 1:1 The solution bonds double bonds to the inner wall of the capillary.

[0089] (2) Preparation of hydrophilic methacrylamide polymer monolithic column by in situ synthesis: 110 mg of AA, 120 mg of Bis, 0.08 mL of 4-VP, 0.6 mL of dodecanol, AIBN were dissolved in 0.75 mL In DMSO, a mixed solution is formed, and the content of the AIBN in the mixed solution is 1wt%. After ultrasonication for 10 min, inject into the activated capillary in step (1), then seal both ends with a si...

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Abstract

The invention discloses a preparation method and application of a hydrophilic methacrylamide polymer monolithic column. The preparation method comprises the following steps: (1) pretreating; (2) adding acrylamide, N, N'-methylene diacrylamide, 4-vinylpyridine, dodecanol and AIBN into dimethyl sulfoxide to form a mixed solution; and (3) carrying out ultrasonic treatment on the mixed solution, then pouring the mixed solution into a pretreated capillary tube, sealing the two ends of the capillary tube, and carrying out reaction for 12-24h at the temperature of 50-70 DEG C to obtain the hydrophilic methacrylamide polymer monolithic column. A method of utilizing the hydrophilic methacrylamide polymer monolithic column to detect nano-particles in a water sample comprises the following steps: enabling the water sample containing the nano-particles to flow through the hydrophilic methacrylamide polymer monolithic column, carrying out desorption, and determining the content of the nano-particles in a desorption solution by virtue of ICP-M. The preparation method has the advantages of rapidness, high efficiency, convenience, low cost and environmental protection. The method of utilizing the hydrophilic methacrylamide polymer monolithic column to detect the nano-particles in the water sample is capable of realizing online analysis, does not have the need for digesting the sample and is good in selectivity and strong in matrix interference-resistant ability.

Description

technical field [0001] The invention belongs to the technical field of separation, analysis and detection, and in particular relates to a preparation method and application of a monolithic column of a hydrophilic methacrylamide polymer. Background technique [0002] Nanoparticles refer to particles with a particle size of less than 100 nm (also known as ultrafine particles), which are located in the transition zone between atomic clusters and macroscopic objects, and have unique surface effects, small size effects, and macroscopic quantum tunneling effects. At present, nanoparticles have been widely used in the fields of industry, medicine and materials, especially gold nanoparticles (Au NPs). Combined with the advantages of not affecting its biological activity, it is used in photocatalysis, probes for optical microscopy, enhancement of Raman spectral signals, biosensing, cell imaging, delivery of targeted drugs, diagnosis and treatment of malignant tumors, etc. . However...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/281B01D15/20B01D15/22G01N1/34G01N1/40C08F222/38C08F220/56C08F226/06C08F2/44C08J9/28
CPCB01D15/20B01D15/22B01J20/281B01J2220/445B01J2220/4812C08F222/385G01N1/34G01N1/405C08F220/56C08F226/06
Inventor 胡斌张琳何蔓陈贝贝
Owner WUHAN UNIV
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