Present thesis has been focused on the synthesis of new sorbents and their application as solid sorbents in solid phase microextraction and thin film microextraction technique. In the first study, polysiloxane nanofibers were fabricated on the stainless steel wire and used as an extracting phase in solid phase microextraction technique. Chlorobenzenes were selected as model compounds. Analysis of compounds was done with gas chromatography and electron capture detection. The prepared fiber had better extraction efficiency compared to commercial fiber (PDMS) and nonfibrous polysiloxane fiber. The limits of detections were in the range of 0.15-75 ng L - 1 and relative standard deviations (RSDs) were less than 6%. Besides, the capability of the method for the analysis of chlorobenzenes in river water, river sediment, wastewater and activated sludge was investigated. In the second study, molecularly imprinted nanofibers were coated on a stainless steel wire and used for the selective solid phase microextraction of simazine. Analysis of simazine was done with gas chromatography- mass spectrometry detection. The influence of important parameters were studied and optimized. The capability of prepared fiber in selective extraction of simazine was also investigated. In this study, the limit of detection of 5 ng L - 1 was obtained for simazine. River water, well water and tap water were used for the evaluation of the method and the relative recoveries were calculated for these samples. In the third study, mesoporous carbon- ZrO 2 nanocomposite was synthesized and used as a sorbent for solid phase microextraction of benzene, toluene, ethylbenzene and m, p - xylenes. The mesoporous carbon- ZrO 2 nanocomposite was synthesized from carbonization of Zr- based metal organic framework. Gas chromatography with flame ionization detector was used for the analysis of compounds. The limit of detections were in the range of 0.05 to 0.56 µg/L and relative standard deviations were in the range of 3-4%. Besides, the method was applied for the analysis of compounds in different water and wastewater samples. In the fourth study, phenyl carbamate functionalized zinc oxide nanorods were fabricated on a cellulose filter paper and used as a novel sorbent in thin film microextraction (TFME) of phenylurea compounds. Analysis of compounds was done with High-performance liquid chromatography with UV–Vis diode array detector (HPLC-DAD). The influence of critical parameters in TFME method were investigated and optimized. Under the optimized conditions, detection limits in the range of 0.04 to 0.13 µg/L were achieved for studied compounds. Finally, the proposed method was applied for the analysis of compounds in river, well and tap water and the relative recoveries were obtained for these samples. In the final work, polyacrylonitrile/zeolite imidazolate-8 was prepared with electrospinning method and introduced for thin film microextraction. Bisphenol A was selected as model compound. High-performance liquid chromatography with UV–Vis detector was used for the analysis of bisphenol A in different samples. The influences of important parameters in extraction and desorption of bisphenol A were studied and optimized. Under optimal conditions, limit of detection was 0.03 µg/L and the relative standard deviation of the method was less than 6%. Finally, the capability of the method for real sample analysis was investigated using river, well, waste water and baby bottle samples.