固相微萃取/气相色谱法检测甲基膦酸酯和磷酸酯

采用溶胶 凝胶方法制备的聚甲基苯基乙烯基硅氧烷/羟基硅油固相微萃取探头联用气相色谱对空气中的甲基膦酸酯和磷酸酯进行分析. 优化了固相微萃取的过程和热解析过程. 该探头的萃取能力强于3种商用固相微萃取探头. SPME GC方法的检出限低（27.2~28.3 μg／L），重现性好（4.7~6.8%）， 线性范围为0.029 2~0.292 mg／L.对空白的空气样品进行标准加入回收实验，3种化合物甲基膦酸二甲酯、 磷酸三甲酯和磷酸三丁酯的回收率分别为94.7%, 89.3%和 93.2%.

Determination of Methylphosphonates and Phosphates in Air Samples Using Solid-phase Microextraction Coupled with Gas Chromatography

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.