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Preparation method for molecularly imprinted monolithic column solid-phase microextraction fiber

A technology of molecular imprinting and fiber extraction, applied in chemical instruments and methods, other chemical processes, etc., can solve problems such as inability to selectively extract target compounds, non-selective graphene coating, etc., and achieve easy control of fiber diameter and high selectivity. the effect of increasing the specific surface area

Inactive Publication Date: 2013-10-09
DALIAN UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Jiang et al fixed graphene on the surface of silica gel particles to extract polybrominated diphenyl ethers (Q Liu, JB Shi, JT Sun, T Wang, LX Zeng, GB Jiang, Angew.Chem.Int.Ed., 2011, 50, 5913-5917), Li et al. (S.L.Zhang, Z.Du, G.K.Li.Anal.Chem.2011, 83, 7531-7541) bonded graphene to the outer wall of solid quartz capillary to prepare a graphene coating The SPME fiber has obtained good results for the extraction of polycyclic aromatic hydrocarbons, but the graphene coating has no selectivity and cannot be used for the selective extraction of target compounds in complex samples.

Method used

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  • Preparation method for molecularly imprinted monolithic column solid-phase microextraction fiber
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  • Preparation method for molecularly imprinted monolithic column solid-phase microextraction fiber

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Experimental program
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Embodiment 1

[0031] Take a quartz capillary with an inner diameter of 0.53mm and a length of 10cm, wash it with 0.1N sodium hydroxide and hydrochloric acid for 30 minutes, wash it with deionized water until neutral, and dry it with nitrogen.

[0032] Make up N,N-dimethylformaldehyde containing bisphenol A (0.15 mmol), methacrylic acid (102 μL), trimethylolpropane trimethacrylate (0.93 mL), and azoisobutyronitrile (21.35 mg). Amide (0.87mL) solution (solution A) and 2 mg / mL graphene in N,N-dimethylformamide solution (solution B); add 0.5mL solution A to solution B, sonicate for 10 minutes, nitrogen Oxygen for 5 minutes to form a prepolymer solution.

[0033] Insert the quartz capillary into the pre-polymer solution, and when the pre-polymer solution is full of the capillary, seal both ends of the capillary with a silicone rubber pad, and place it in a 65°C water bath for 24 hours; immerse the middle of the quartz capillary in 25% hydrofluoric acid for 2 hours , to obtain a polymer fiber wi...

Embodiment 2

[0035] Take a quartz capillary with an inner diameter of 0.25mm and a length of 10cm, wash it with 0.1N sodium hydroxide and hydrochloric acid for 30 minutes, wash it with deionized water until neutral, and dry it with nitrogen.

[0036] A configuration containing bisphenol A (0.15 mmol), methacrylic acid (102 μL), trimethylolpropane trimethacrylate (0.93 mL), azoisobutyronitrile (21.35 mg) and N,N-dimethylformaldehyde Amide (0.87mL) solution (solution A) and 2 mg / mL graphene N,N-dimethylformamide solution (solution B); add 0.5mL solution A to solution B, sonicate for 10 minutes, nitrogen deoxygenation 5min to form a prepolymer solution.

[0037] Insert the quartz capillary into the pre-polymer solution, and when the pre-polymer solution is full of the capillary, seal both ends of the capillary with a silicone rubber pad, and place it in a 65°C water bath for 24 hours; immerse the middle of the quartz capillary in 25% hydrofluoric acid for 2 hours , to obtain a polymer fiber ...

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Abstract

The invention relates to molecularly imprinted monolithic column solid-phase microextraction fiber and a preparation method, and belongs to the technical field of pretreatment of samples for analytical chemistry. The fiber is composed of graphene and a molecular imprinted polymer; one end of the fiber is fixed on a quartz capillary; and the other end of the fiber is exposed out of the quartz capillary. In preparation, a quartz capillary is inserted into a prepolymer solution containing graphene, template molecules, functional monomers, a cross-linking agent and an initiator, two ends of the quartz capillary are sealed when the quartz capillary is filled with the prepolymer solution; then the sealed quartz capillary is put into a water bath for reaction; the wall of the quartz tube at the middle of the quartz capillary is etched off by a hydrofluoric acid solution; the template molecules in the polymer are removed; and the quartz capillary is broken off from the middle, so that the molecularly imprinted monolithic column solid-phase microextraction fiber is obtained. The preparation method is simple and fast; and the prepared extraction fiber has good chemical stability, mechanical stability and heat stability, high extraction volume, good selectivity for the template molecules and long service life, and has wide application prospects in the fields of analytical chemistry and environmental analysis.

Description

technical field [0001] The invention discloses a preparation method of a solid-phase microextraction fiber of a molecularly imprinted monolithic column, which is mainly used for the separation and enrichment of target objects in complex aqueous solution samples, and belongs to the technical field of analytical chemical sample pretreatment. Background technique [0002] Pretreatment is an important step in the analysis of complex samples. Through pretreatment, the interfering substances in the sample are removed and the target substance is concentrated to make up for the lack of existing separation technology and instrument detection sensitivity. Solid phase microextraction (SPME) is a relatively new sample preparation technique. Compared with traditional sample pretreatment techniques such as liquid-liquid extraction, Soxhlet extraction, solid phase extraction, etc., SPME has the advantages of less sample consumption, short processing time, simple operation, no secondary po...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30
Inventor 谭峰王晓春李莲君全燮陈景文
Owner DALIAN UNIV OF TECH
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