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Nanogold modified polymer monolithic column, and preparation method and application thereof

A monolithic column, polymer technology, applied in separation methods, chemical instruments and methods, other chemical processes, etc., can solve the problem of less application of inorganic metal ions, and achieve good preparation reproducibility, good adsorption performance, and adsorption capacity improvement. Effect

Inactive Publication Date: 2017-03-15
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, nano-gold modified monolithic columns have been used in the separation of biological macromolecules such as peptides and proteins in biological samples, but there are very few applications in the separation and detection of inorganic metal ions.

Method used

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  • Nanogold modified polymer monolithic column, and preparation method and application thereof
  • Nanogold modified polymer monolithic column, and preparation method and application thereof
  • Nanogold modified polymer monolithic column, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Preparation of nano-gold modified capillary monolithic column modified by mercaptosuccinic acid

[0035](1) Pre-activation process of capillary: choose fused silica capillary (20cm×530μm), rinse with ultrapure water for 10min, 1.0mol L -1 Rinse with NaOH solution for 2h, ultrapure water for 30min, 1.0mol L -1 Rinse with HCl solution for 2h and ultrapure water for 30min until neutral, then blow dry with nitrogen. Rinse the mixed solution of WD-70 and ethanol (volume ratio 1:1) into the capillary, seal both ends with silica gel pads, place it in an oven at 70°C for 12 hours, and then flush the unreacted reagent in the capillary with ethanol. out, and then dry the inside of the capillary with argon for later use.

[0036] (2) Preparation of poly(GMA-EDMA) monolithic column: a monolithic column was synthesized by thermally initiated in-situ polymerization, 140 mg of GMA, 120 mg of EDMA, 0.66 mL of cyclohexanol, 0.09 mL of dodecanol and 1% of AIBN was mixed, ul...

Embodiment 2

[0041] Example 2: Application of poly(GMA-EDMA-Au NPs-MSA) monolithic column in the detection of rare earth elements

[0042] Using the poly(GMA-EDMA-Au NPs-MSA) monolithic column prepared in Example 1 for the combination of capillary microextraction and ICP-MS to establish a method for detecting rare earth elements by monolithic CME-ICP-MS

[0043] 1) First optimize the conditions of capillary microextraction, such as Figure 6-Figure 9 As shown, the single variable method was used to optimize the conditions of capillary microextraction one by one, and the final optimal conditions were that the pH value of the sample solution was 5, and the sample loading flow rate was 0.1mL min -1 , the sample volume is 0.5 mL, and the eluent is HNO 3 , the eluent concentration and volume are 0.5mol L -1 , 0.02mL.

[0044] 2) Under optimal conditions, common interference ions (such as Table 1) and humic acid ( Figure 10 ) was investigated for the enrichment and detection of rare earth e...

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Abstract

The invention discloses a method for analyzing a rare earth element in seawater and human whole blood through online combination of ICP-MS (Inductively Coupled Plasma Mass Spectrometry) and capillary microextraction of a mercaptobutanedioic acid modified nanogold modified polymer monolithic column. Glycidyl methacrylate is taken as a monomer, ethylene glycol dimethacrylate is taken as a crosslinking agent, an in situ polymerization method is used to obtain the polymer monolithic column, then the surface of an epoxy group of the polymer monolithic column is subjected to a series of chemical reactions to enable the polymer monolithic column to be rich in sulfydryl, the nanogold is modified through a chemical bonding mode, and finally, the nanogold is taken as an intermediate ligand, and the mercaptobutanedioic acid having an affinity effect on the rare earth element is modified on the surface of the nanogold. The monolithic column is used to separate and enrich the rare earth element in a complex sample, the online analysis of the rare earth element in the seawater and whole human blood is realized, the adsorption capacity (3-6.5 times) of the monolithic column on the rare earth element is remarkably improved, and the method has the advantages of high sensitivity, high sample flux, low sample consumption, wider pH scope of application, higher capability of resisting matrix interference and the like.

Description

technical field [0001] The invention belongs to the technical field of separation, analysis and detection, and specifically relates to a monolithic column of nano-gold modified polymer modified by mercaptosuccinic acid and a preparation method thereof, and its use in capillary microextraction and inductively coupled plasma mass spectrometry for complex The rare earth elements in the sample are analyzed and detected on-line. Background technique [0002] Due to their special properties, rare earth elements are widely used in fields such as industry (magnetic materials, catalytic materials), agriculture (rare earth micro-fertilizers) and biomedicine (NMR contrast agents). Avoided release to the environment, significant effects on organisms through accumulation in the food chain. Studies have shown that long-term intake of low doses of rare earth elements can cause accumulation in the brain, induce toxic effects, frustrate nerves, and lower IQ; rare earth elements can also aff...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/22B01J20/285B01J20/30G01N27/62
CPCB01D15/22B01J20/285B01J2220/84G01N27/62
Inventor 胡斌蔡亚冰陈贝贝何蔓
Owner WUHAN UNIV
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