Application of beta-cyclodextrin bonded silicone gel as solid phase extraction adsorption medium

A technology of bonded silica gel and adsorption medium, which is applied in chemical methods for reacting gases with non-granular solids, other chemical processes, chemical instruments and methods, etc., can solve the problem of difficult to obtain specific action site polymers, long synthesis and preparation process , difficult to obtain antibodies, etc., to achieve the effect of easy control, simple post-processing, and cheap raw materials

Inactive Publication Date: 2003-02-05
WUHAN UNIV
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Problems solved by technology

For immune-type fillers, it is difficult to obtain antibodies with higher purity and is generally more expensive, and there is currently a lack of antibodies against small molecule compounds; for molecularly imprinted polymers, the synthesis and preparation process is long, the operation is cumbersome, and it is difficult to obtain specific effects. Polymers with high site content have poor selectivity and slow mass transfer in aqueous solution

Method used

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Experimental program
Comparison scheme
Effect test

specific Embodiment approach 1

[0008] The specific embodiment 1. Synthesis of β-cyclodextrin bonded silica gel (CDS): get 5g of β-cyclodextrin through vacuum drying, take anhydrous dimethylformamide (DMF) as solvent, NaH as catalyst, in The reaction was stirred at room temperature for 1 h, and the unreacted solid matter was filtered off. Add 2 mL of KH-560 (γ-glycidylpropyltriethoxysilane) to the filtrate, react at 85-90°C for 5 hours under nitrogen protection, and then add 10 g of silica gel (20-30 μm). Raise the reaction temperature to 110-115°C and continue the reaction for 24 hours. After the reaction liquid is cooled to room temperature, it is filtered with suction. The product was washed successively with DMF, methanol, and secondary water, and finally washed with methanol again. After being filtered and dried, it was dried in an oven at 80-90°C for 1 hour, and then transferred to a desiccator for storage. 2. Solid phase extraction:

[0009] The obtained β-cyclodextrin bonded silica gel (CDS) was lo...

Embodiment 1

[0010] Before extraction, first activate CDS with 5mL methanol, 5mL secondary water or corresponding buffer solution, and then make the sample solution flow through the column under the negative pressure of the vacuum pump, and use an appropriate volume of cleaning solution to wash away impurities in the matrix. The eluent collected the analyte eluted into a test tube, concentrated with nitrogen in a water bath at 60-70°C, and then quantitatively analyzed after adding an internal standard. Embodiment 1: CDS is used for the selective solid phase extraction of 4-nitrophenol in water sample

[0011] 1. On-line evaluation of CDS (measurement of penetration volume): using the homogenization method, put 0.3137g CDS into a 50×4.6mm, I.D. stainless steel column, and make a 10mg / L solution of 4-nitrophenol as the mobile phase. The measured breakthrough volume was 136 mL, which corresponds to an adsorption capacity of 4.34 mg / 1 g CDS for 4-nitrophenol. The results show that CDS has a s...

Embodiment 2

[0021] Take 250mL of Wuhan East Lake water, after filtering, add the above 8 kinds of phenolic compounds, the concentration is 20μg / L, after extraction with the operation procedure of 2, the result is that the recovery rate of 4-nitrophenol is 63%, and the remaining phenolic compounds are almost No recycling. The results show that β-cyclodextrin bonded silica gel can be used in the analysis of actual water samples with good selectivity. The recovery rate of the column contaminated by humic acid in the water sample did not decrease significantly when re-extracted. Embodiment 2: CDS is used in the selective solid phase extraction of 2,4-dinitrophenol in water sample

[0022] Activation: Use a solid-phase extraction column filled with 500mg CDS, pass through the column with 5mL methanol and 5mL secondary water in sequence at a flow rate of 5mL / min.

[0023] Extraction: 250mL sample solution, containing 8 kinds of phenolic compounds: resorcinol, o-diphenol, phenol, 2,4-dinitroph...

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Abstract

The present invention relates to the application of beta-cyclodextrin bonded silica gel as solid-phase extraction adsorption medium. Said beta-cyclodextrin bonded silica gel features simple synthesis process and cheap raw material, when it is used for making solid-phase extraction, it features large penetration volume, high adsorption quantity, high selectivity, and can be regenerated and reused. It can be used for making selective extraction of nitrophenol compound in water sample, also can be used for pre-enrichment of medicine molecules in biological sample.

Description

technical field [0001] The invention relates to the application of β-cyclodextrin bonded silica gel as a solid-phase extraction adsorption medium. Background technique [0002] In the analysis of environmental water samples and biological samples, etc., the pre-enrichment of samples and the elimination of complex matrices are crucial. Traditional sample pretreatment usually adopts liquid-liquid extraction (LLE) method, but LLE method has the disadvantages of cumbersome operation, large consumption of organic solvent, and low extraction efficiency of polar compounds. The solid-phase extraction technology that appeared in the late 1970s and early 1980s is a method with high extraction efficiency, simple operation, and low consumption of organic solvents compared with liquid-liquid extraction. In recent years, both its offline (off-line) mode and online (on-line) mode have developed rapidly, and the offline mode has greater flexibility in its operation, which is suitable for e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J15/00B01J20/22
Inventor 冯钰锜范毅达世禄
Owner WUHAN UNIV
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