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采用溶胶-凝胶方法制备了PEG-20M涂层的固相微萃取（SPME）探头并研究了它的特性。该探头具有耐高温，抗溶剂冲洗,使用寿命长的特点。由于PEG-20M的极性比较强，因此它对极性化合物如酚等有很好的萃取能力。用该探头测定了酚类物质，检出限达0.78～4.2 ng/mL，线性范围为0.1～10 μg/mL，相对标准偏差RSD＜6%。“,”A solid-phase microextraction (SPME) fiber coated with PEG-20M layer was prepared by sol-gel coating technology. It has high thermal stability (to 320℃) and solvent stability (with CH2Cl2 and H2O). Efficient analysis of phenols with headspace SPME-GC was achieved using sol-gel-derived PEG-20M fiber with a precision better than 6% and limits of detection at the ng/mL level. Analysis of phenol and 2,4-dimethylphenol in paper mill was reported.