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Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof

A molecular imprinting and fiber membrane technology, applied in separation methods, solid adsorbent liquid separation, selective adsorption, etc., can solve the problems of cumbersome process and low recovery rate, and achieve the effect of high sensitivity

Inactive Publication Date: 2013-12-11
HENAN INST OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, in the offline extraction, the two-phase (non-polar organic solvent phase-polar solvent phase) liquid-liquid extraction is used, and then the MIP extraction column is used for extraction. However, there are still disadvantages such as the process is too cumbersome and the recovery rate is low.

Method used

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  • Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof
  • Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof
  • Hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Preparation method of molecularly imprinted monolithic adsorption rod coated with hollow fiber membrane

[0037] The inner surface of the capillary is pretreated prior to preparation of the monolithic column. It mainly has the following processes:

[0038](1) Rinse the capillary with 1mol / L NaOH solution for 30min; (2) Rinse with secondary water for 30min; (3) Rinse with 0.1mol / L HCL solution for 30min to remove sodium ions and other impurities; Rinse with water until pH = 7; (5) blow dry with nitrogen and set aside. Sonicate 0.50mmol (0.1111g) of the template molecule atrazine, 3.0mmol (0.127mL) of the functional monomer MAA, 5.380mmol (2.0mL) of the porogen toluene, and 14.278mmol (0.8mL) of dodecanol in a small vial for 10 minutes. , then add cross-linking agent EDMA 12.13mmol (0.280mL) and sonicate for 15min, after mixing, add initiator AIBN 0.030g and sonicate for 10min. Cut 30 cm of treated capillary tubes with inner diameters of 530 μm and 320 μm res...

Embodiment 2

[0043] The molecularly imprinted monolithic adsorption rod coated with the hollow fiber membrane prepared in Example 1 was used to extract atrazine and its structural analogues. The surface river water samples were collected from about 0.5m below the water surface of the East Lake of the school, filtered with filter paper and 0.45μm filter membrane to remove suspended solids, and then put them in the refrigerator for later use. The standard solutions of s-triazine, atrazine, terbuthine, ametrazine and the reference product metrizone were all prepared in series concentrations with water: acetonitrile (40:60, v / v) and stored in the refrigerator for later use.

[0044] Chromatographic conditions: ODS-C18 chromatographic column (200mm×4.6mm, ∮5μm,), the mobile phase is acetonitrile / water (v / v=60 / 40), the column temperature is room temperature, the flow rate is 0.8mL / min, and the detection wavelength is 220nm, for sample liquid phase analysis and detection, each injection volume is...

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Abstract

The invention claims a hollow-fiber-film-coated molecular imprinting integral adsorption rod, as well as a preparation method and an application thereof. According to the invention, an atrazine molecular imprinting capillary integral extraction head is prepared by using a way of in-situ microwave polymerization in a capillary; the imprinting integral extraction head is coated by using a hollow fiber film and then is used as a solid phase micro-extraction head; by combining a hollow fiver film extraction technology and a high performance liquid chromatography, parameters affecting the extracting efficiency are optimized, such as extraction and analysis solvents, salt concentrations and pH values, extraction and analyzing time, stirring speed and the like; two analysis methods capable of directly extracting triazine herbicides in an environmental water sample are established. The standard recovery rates of detected four triazine herbicide substances are greater than 80% under the optimized experiment conditions. According to the invention, a detection method in which hollow-fiber-film-coated molecular imprinting polymer integral column micro-extraction and an HPLC (High Performance Liquid Chromatography) are combined is established; the detection method has the advantages of simplicity, rapidity, high sensitivity and the like and is suitable for the routine analysis of the water samples.

Description

technical field [0001] The invention relates to a molecularly imprinted monolithic adsorption rod coated with a hollow fiber membrane and its preparation method and application, in particular to an imprinted solid-phase microextraction monolithic column using atrazine as a template molecule and a preparation method thereof. For the extraction of atrazine and its triazine herbicides. Background technique [0002] Solid-phase microextraction (Solid-phase microextraction, SPME) was first proposed by the research group of Professor Pawliszyn of the University of Waterloo, Canada in 1989, and then in 1990, the research group used the Hamilton 7000 syringe to convert it into the first SPME extraction and sampling device. Because of its simplicity, rapidity and sensitivity, it soon attracted great attention from people. SPME technology integrates sampling, extraction and energy enrichment simultaneously, and when combined with gas chromatography and liquid chromatography, it can m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/08B01D15/22G01N30/08
Inventor 陈军张裕平柏连阳周小毛张毅军陈娜刘润强刘坤峰
Owner HENAN INST OF SCI & TECH
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