以羟基硅油和二乙烯基苯为涂层材料,采用溶胶-凝胶技术和自由基引发交联的方法制备了一种新型的固相微萃取探头.采用顶空固相微萃取与气相色谱联用的方法模拟检测了水中磷酸酯和甲基磷酸酯类化合物.与商品化固相微萃取探头相比,该新型涂层可获得高的萃取效率.甲基膦酸二甲酯、磷酸三甲酯和磷酸三丁酯的最低检测限分别为0.34,2.20 和0.01 mg/L,相对标准偏差为3.67%～6.44%,线性范围为1～2个数量级,方法重现性好,回收率为89.46%～90.88%.
Copoly (hydroxy-terminated silicone oil/divinylbenzene) (OH-TSO/DVB) was synthesized as a stationary phase coating with vinyltriethoxylsilane (VTEOS) as the bridge using the sol-gel coating method and cross-linking technology. This stationary phase was applied for solid-phase microextraction (SPME) of phosphates and methylphosphonates. Compared with commercial SPME fibers, the novel coatings showed better selectivity and sensitivity in analysis of phosphates and methylphosphonates. Some important parameters, such as extraction time, extraction temperature, effect of salt and desorption time, were optimized. The limits of detection for dimethyl methylphosphonate (DMMP), trimethyl phosphate (TMP) and tributyl phosphate (TBP) in water were 0.34, 2.20 and 0.01 mg/L, respectively. Relative standard deviations from 3.67% to 6.44%(n=6) can be achieved depending on the compounds. The linear ranges were about 1-2 orders of magnitude. The recoveries of spiked water samples were 89.46% to 90.88%.
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