Preparation of a New Solid-Phase Microextraction Fiber by Coating Silylated Nanoporous Silica on a Copper Wire

• Published in: Journal of the Chinese Chemical Society (Taipei) 2012-06, Vol.59 (6), p.727-732
• Main Authors: Hashemi, Payman, Badiei, Alireza, Shamizadeh, Mohammad, Ziarani, Ghodsi Mohammadi, Ghiasvand, Ali Reza
• Format: Article
• Language: English
• Subjects: Copper wire; New solid phase microextraction fiber; Phenolic compounds; Silylated nanoporous silica
• ISSN: 0009-4536; 2192-6549
• DOI: 10.1002/jccs.201100429

LUS‐1 typed nanoporous silica particles were synthesized and silylated with hexamethyldisilazane and investigated as a highly porous fiber coating for solid‐phase microextraction (SPME). The pore size distribution of the prepared Sil‐LUS‐1 was still typical of MCM‐41 and centered at 3 nm with a specific surface area of 720 m2g−1. The SPME fiber was prepared by liming the material on a copper wire. The extraction efficiency of the new fiber was compared with a commercial PDMS fiber for headspace extraction and GC‐MS analysis of phenol, 4‐nitrophenol, 2,4‐dichlorophenol and 4‐chlorophenol in water samples. Due to the high porosity of the prepared fiber it showed a higher sensitivity and better selectivity for the extraction of the target compounds. For optimization of different factors affecting the extraction efficiency, a simplex optimization method was used. The relative standard deviation for the measurements by one fiber was better than 7% for five replicates and the fiber‐to‐fiber reproducibility was about 10% for five fabricated fibers. Detection limits in the range of 0.002 to 0.026 μg mL−1 were obtained for the phenolic compounds. The fiber was successfully applied for the determination of phenolic compounds in natural water samples. LUS‐1 nanoporous silica particles were synthesized, silylated and limed on a copper wire to be used as a new SPME fiber. Due to the high porosity of the fiber it showed a higher sensitivity and better selectivity for the extraction of phenolic compouned compared to a commercial PDMS fiber.