Preparation Of Phosphate Diester Quaernary Ammonium Salt Within The Monolitthic Column And Study Of Its Application In μ-HPLC Systom

Microflow or nanoflow chromatographic methods have attracted strong interest. While there is a lot of problems when comes to the particulate-packed capillary columns which are the traditional columns used in HPLC. The appearance of capillary monolithic columns put forward a completely significantly alternative for traditional packed capillary column. But its development is still in the very beginning step. Therefore, novel monolithic columns were developed and their applications have been studied.1,Phosphate diester quaternary ammonium salt as the matrix within the capillary monolithic column is one kind of polymeric monoliths, and also get more and more attractive within the hydrophilic monolithic column chromatography. In this paper, based on the previous studies, we study on the catalytic synthesis of 2,3-epoxypropyl trimethyl chloride as the basis for further synthesis of phosphate diester quaternary ammonium salts of gender within the monomer, for the conduct of the phosphate diester quaternary ammonium salt class gender monolithic column preparation and design of experiments, a new type of monolithic column prepared by the physical and chromatographic characterization, expansion the application of the monolithic capillary column in the analysis science. Research papers and the main conclusions are as follows. 2,2,3-Epoxypropyl trimethyl ammonium chloride(GTA) was synthesized at normal temperature using epichlorohydrin and trim ethylamine as raw materials and potassium iodide as catalyst in the presence of ethanol. Varied factors influencing the yield were investigated by orthogonal experiment. The optimum reaction conditions are as follows :nEPIC:nTMA∶nKI=1:0.3:0.02,reaction temperature 20℃,total reaction time 4h. Ethanol and excess epichlorohydrin and the composition of the media in favor of the trimethylamine nucleophilic substitution reaction, meanwhile, at a low temperature in polar solvents in the reaction system by adding a small amount of inhibitor (hydroquinone) may reduce the polymerization reaction, so there are fewer side effects, the product of high purity.3,Discussion the issue of combination for the column bed and the wall is not fully close-knit.and found that if we increasing the time of sodium hydroxide's corrosion, may facilitate the integration of the column bed and the wall'tightness.4,During the experiment, overall the chromatography performance of Phosphate diester quaternary ammonium salt as the monomer within the capillary monolithic column, the relationship between mobile phase velocity and the column pressure were investigated, relationship between theoretical plate height and mobile phase linear velocity, the chromatography efficiency of the performance with the different column diameter, the overall separation impedance of the column performance etc. The experimental results showed that when the phosphate diester quaternary ammonium salt within the new monolithic capillary column at a higher pressure and higher velocity, the velocity and pressure between the stigma still maintain a good linear relationship, a higher the column efficiency, high tolerance, and good mechanical stability. Second, with the increasing of the capillary diameter , column efficiency got a increase, but the porosity of the column decreased, permeability decreased either. Again, the method of power flow can eliminate the efficiency on the column theoretical plate number and other chromatographic parameters from the remaining surface of the column stationary phase layer.