A novel, simple sample pretreatment method to simultaneously separate and analysis different polarity, compounds, phthalate esters and its metabolites, was developed. Using activated carbon fiber and carbon fiber made a sample prereatment mini-column. This technique can simultaneous separate polar and non polar group in complex biological sample. The various parameters affecting separation efficiency such as composition of elution solvent, elution solvent volume and elution solvent flow rate were optimized. Using the pre-column system combined GC-MS or MS/MS determined phthalate esters and its metabolites within short time of 25 min, respectively. Recovery of phthalate esters and its metabolites were between 75.4 and 85.1%, and reproducibility were between 3.4 and 7.7%, and detection limit were between 5 to10 ng mL-1 for urine biological sample. Analytical characteristics of the method was compared with SPE and SPME methods. Finally, this technique was applied to determine phthalate esters and its metabolites in urine samples. The experimental results demonstrated which is favor to treatment of urine sample using only single injection, and it can simultaneously obtain both phthalates and its metabolites with fast speed and high accuracy. |