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A fast silyl derivatization technique for simultaneous GC/ MS analysis of alkylphenols, chlorophenols, and bisphenol A was developed. The analytes were silylized with an excess amount of bis(trimethylsilyl)trifluoroacetamide (BSTFA) followed by hydrolysis of excess silyl reagent with water. Reaction rates of derivatization were studied in various solvents and found to be fastest in acetone. Derivatization reaction in acetone was completed quantitatively within 15 s at room temperature while it took more than 1 h in other solvents studied. Similar results were obtained in mixed solvents with acetone if the content of acetone was higher than 60% (v/v). Since water-immiscible solvents such as dichloromethane or hexane are frequently used in the extraction of phenolic analytes in various sample matrixes, acetone can be added to the extracts in order to accelerate the reaction rate of derivatization. Stability of the derivatives in sample for long-term storage was ensured by hydrolyzing excess derivatizing reagent, BSTFA, with a spike of water followed by dehydration using anhydrous sodium sulfate. On the basis of the above results, a derivatizing treatment kit was designed to improve the convenience of analysis. It was possible to treat sample within several minutes successfully by using the kit. So fast simultaneous determination of those anlaytes by GC/MS was possible with improved convenience as well as sensitivity and reproducibility.