Abstract: A solgelderived poly（methylphenylvinylsiloxane)(PMPVS)/hydroxy terminated silicone oil (OHTSO) solidphase microextraction fiber coupled with gas chromatography (GC) was developed to determine methylphosphonates and phosphates in air samples. The extraction and desorption parameters influencing on solidphase microextraction (SPME) process were optimized. Compared with three comme rcial SPME stationary phases, this fiber shows the best selectivity and sensitivity towards these compounds. The detection limits of this method varied from 27.2 to 28.3 μg／L, and the relative standard deviations (n=5) for these compounds were found to be from 4.7% to 6.8%. The linearity range was one order of magnitude. For blank air samples, standard additional experiment was used, the recoveries of three compounds, dimethy methyl phosphonate, trimethyl phosphate, tributyl phosphate were 94.7%,89.3% and 93.2%, respectively.

Key words: solgel technology, poly（methylphenylvinylsiloxane)/hydroxyterminated silicone oil, solidphase microextraction, methylphosphonates, phosphates