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 2 0和 0 0 1mg/L,相对标准偏差为 3 6 7%～ 6 4 4 % ,线性范围为 1～ 2个数量级 ,方法重现性好 ,回收率为 89 4 6 %～ 90 88%。 Hydroxysilicone and divinylbenzene were used as coating materials to prepare a new type of SPME probe by sol-gel technique and radical-initiated cross-linking method. The method of headspace solid-phase microextraction and gas chromatography was used to simulate the detection of phosphate and methylphosphate in water. The new coating achieves high extraction efficiencies compared to commercial solid-phase microextraction probes. The detection limits of methyl methylphosphonate, trimethyl phosphate and tributyl phosphate were 0 34,2 2 0 and 0 0 1 mg / L, respectively. The relative standard deviations (RSDs) ranged from 36.7% to 64.4% The linear range of 1 ~ 2 orders of magnitude, good reproducibility, recovery of 89 4 6% ~ 90 88%.