▎ 摘　　要

NOVELTY - Preparing solid phase micro extraction tube composite column involves preparing titanium dioxide-graphene oxide composite. The certain concentration of graphene oxide is added dropwise to an aqueous solution of methacrylatoethyl trimethyl ammonium chloride. The obtained solution is centrifuged, washed and then dispersed in ultrapure water. The certain concentration of titanium dioxide slurry is added dropwise and then stirred for 7-14 hours, after centrifugation, washing and drying. USE - Method for preparing solid phase micro extraction tube composite column used for detecting enrichment of trace amounts of phosphopeptide (claimed). ADVANTAGE - The method enables to prepare solid phase micro extraction tube composite column, which solves problem of extraction, simple, flexible, selective extraction of complex phosphopeptide, analyzes protein group in phosphopeptide and has chemical application prospect. DETAILED DESCRIPTION - Preparing solid phase micro extraction tube composite column involves preparing titanium dioxide-graphene oxide composite. The certain concentration of graphene oxide is added dropwise to an aqueous solution of methacrylatoethyl trimethyl ammonium chloride. The obtained solution is centrifuged, washed and then dispersed in ultrapure water. The certain concentration of titanium dioxide slurry is added dropwise and then stirred for 7-14 hours, after centrifugation, washing and drying. The solid phase micro extraction column is prepared by adding monomer, crosslinking agent, initiator and agent in the obtained titanium dioxide-graphene oxide composite. The solution is injected into capillary and then placed into polymerization reaction tank for 5-30 minutes, under ultraviolet light. The monomer is methyl acrylate, the crosslinking agent is ethylene glycol dimethacrylate and the initiator is 2,2-dimethoxy-phenylacetophenone from normal propanol, 1,4-butanediol and water. The capillary has silylating agent, which is 3-(Trimethoxysilyl)propyl methacrylate. An INDEPENDENT CLAIM is included for a method for extracting and analysis of phosphopeptide, which involves: (A) extracting phosphopeptide from solid phase within sample tube, where pressure is 200-500psi and the solid phase extraction column has acetic acid solution, which flows through the peptide sample, where an analyte extracted is left in the extraction column; and (B) performing centrifugation and collecting column end solution and using phosphopeptide samples with a pressure of 200-500psi, which flow through the extraction column and the extracts are eluted from extraction phase, collecting the centrifugation tube for extraction of column end solution, where the pH of the acetic acid solution (0.1vol.%) is 3-4 and pH of the analytical solution is 9-11 and concentration of aqueous ammonia is 0.01-1% (v/v).