A method has been developed for the trace analysis of 27 compounds from a diverse group of pharmaceuticals, steroids, pesticides, and personal care products. The method employs solid-phase extraction (SPE) and liquid chromatography/tandem mass spectrometry (LC/MS/ MS), using electrospray ionization (ESI) in both positive and negative modes and atmospheric pressure chemical ionization in positive mode. Unlike many previous methods, a single SPE procedure using 1 L of water coupled to a simple LC method is used for all ionization modes. Instrument detection limits for most compounds were below 1.0 pg on column with reporting limits of 1.0 ng/L in water. Recoveries for most compounds in deionized water were greater than 80%. Sulfuric acid was found to be the preferred sample preservative, and structures of all MS/MS product ions are proposed. Matrix effects from waters with a high content of treated municipal effluent were observed in both ESI modes and are discussed in the paper.In recent years, reports have shown that certain contaminants at trace concentrations in surface waters can have dramatic effects on the endocrine systems of aquatic organisms. 1-3 These compounds are collectively known as endocrine-disrupting compounds (EDCs). Pharmaceuticals, steroids, and personal care products have also been detected in the aquatic environment and may act as EDCs. [4][5][6] As environmental contaminants continue to be discovered, the need for comprehensive methods for their sensitive and selective identification has also increased. Traditional gas chromatography is of limited value without time-consuming and labor-intensive derivatization because many environmental contaminants are polar, have low volatility, and are thermally labile. This has led to the increased use of liquid chromatography/mass spectrometry (LC/MS) due to its ability to effectively analyze these types of molecules.LC/MS methods for the analysis of pharmaceuticals, steroids, and personal care products in water have been developed for a number of different mass spectrometers using diverse extraction procedures and elution protocols. A complete review of methods for the analysis of these compounds in water using LC/MS is beyond the scope of this paper, and thorough reviews have previously been published. [7][8][9] The majority of concentration techniques involve solid-phase extraction (SPE) in which many solid phases, eluent schemes, and final solvents with and without ionpairing reagents, buffers, and modifiers were used. 10-20 Additionally, both single quadrupole 11,15,16

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