▎ 摘　　要

NOVELTY - Chlorophenol graphene-based molecular imprinted solid phase extraction column comprises an empty column, frits and fillers. The filler comprises chlorophenol graphene molecularly imprinted nanoparticles and traditional solid phase extraction filler in a mass ratio of 1:1-10. The chlorophenol graphene molecularly imprinted nanoparticles are prepared by loading graphene magnetic iron(II,III) oxide polymer material as a functional unit, and allowing target chlorophenols to be absorbed as a template molecule. USE - The chlorophenol graphene-based molecular imprinted solid phase extraction column is useful in enrichment and purification of trace chlorophenols in environmental water samples (claimed). ADVANTAGE - The chlorophenol graphene-based molecular imprinted solid phase extraction column has large specific surface area and adsorption sites, high specific selectivity, good accumulation effect. The method reduces matrix effects, is simple and economical; has stable process conditions. DETAILED DESCRIPTION - An INDEPENDENT CLAIM is also included for preparing chlorophenol graphene-based molecular imprinted solid phase extraction column, comprising (i) preparing chlorophenol graphene-based molecular imprinted nanoparticles by (a) preparing high magnetic response of monodisperse core-shell magnetic polymer microspheres by carrying out solvothermal method of 1-3.5 g iron(III) chloride hexahydrate, 70-100 g ethylene glycol, 5-6.5 g sodium acetate and 1-2 g polyethylene glycol, mixing, stirring to dissolve at 50 degrees C for 0.5-1 hour, to obtain mixed solution, adding to a polyfluortetraethylene high pressure kettle at 200 degrees C, reacting for 4-10 hours, to obtain magnetic iron oxide microspheres, adding 50-100 mg magnetic iron oxide microspheres with 80-120 ml acetonitrile, carrying out ultrasonic dispersion for 0.5-1 hour, adding 0.2-0.8 g divinylbenzene (DVB), 0.2-0.8 g glycidyl methacrylate (GMA) as a polymerization monomer and 0.01-0.1 g azobisisobutyronitrile (ABIN) as an initiator, carrying out precipitation- polymerization reaction at 60-100 degrees C for 0.5-5 hours, (b) activating carboxy group of graphene oxide by adding 100-150 mg graphene oxide with water, added ultrasonic dispersion for 3-4 hours, adding 100-150 mg 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and 80-90 mg N-hydroxysuccinimide, and mechanically stirring at room temperature for 30-40 minutes, (c) carrying out molecular self-assembly by mixing 20-50 ml to be adsorbed target chlorophenols (10-50 mmol/l) and 50-100 ml ethylenediamine solution (100-200mmol/l), and carrying out ultrasonic agitation at 50 degrees C for 1-2 hours, and (d) mixing all the above mentioned raw materials by adding into a three-necked flask at 80-85 degrees C, carrying out ultrasonic agitation for 2.5-3 hours, eluting using acetate/methanol mixtures surface template molecule thrice, and drying under vacuum; (ii) adding 10-100 mg chlorophenol graphene-based molecular imprinted nanoparticles with 10-30 ml organic solvent, carrying out ultrasonic agitation for 10-30 minutes, mixing, transferring to empty solid phase extraction column after filling uniformly sieve with sealing ends; (iii) adding conventional solid-phase extraction filler material with 10-30 ml organic solvent, carrying out ultrasonic agitation for 10-30 minutes, mixing, transferring to chlorophenol containing graphene molecules of step (ii) to obtain imprinted nanoparticles SPE small columns, uniformly filling, closing the top portion with sieve, washing column with 10-20 ml acidic organic solvent, and cleaning with 10-20 ml organic solvent; and (iv) introducing nitrogen to remove the solid phase extraction column residual organic solvent, carrying out vacuum drying at 20-60 degrees C for 1-12 hours.