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On-line solid-phase extraction (SPE) was interfaced to liquid chromatography with atmospheric pressure chemical ionization mass spectrometry (HPLC-APCI-MS) for the determination of US Environmental Protection Agency (EPA) phenols. The system, allowing fully automated operation, was used to evaluate different SPE cartridge materials and dimensions. Six different SPE materials (C-18 HD, Polymer Labs PLRP-s, Hamilton PRP-1, Hysphere GP, Hysphere SH and Waters Oasis) were tested. Criteria for their comparison were first the recovery for the different phenols and its reproducibility, but also chromatographically relevant items like peakshape in the on-line elution mode. High recoveries and good relative standard deviations were obtained particularly for the newer, strongly retaining SPE materials that have become commercially available recently (the Hysphere materials and Waters Oasis) compared to the well known silica-based and weaker polymeric adsorbents like PLRP-s and PRP-1. These advantages are, however, traded in for good chromatographic peahshape, since the stronger adsorbents give rise to notable peak broadening in on-line elution. This is particularly true when using APCI-MS detection which on the one hand offers excellent selectivity and sensitivity, but imposes additional restrictions on the mobile phase composition in order not to suppress the response significantly. The influence of these parameters on the on-line-SPE-HPLC-MS determination of EPA phenols is discussed and present limitations are pointed out. (C) 2000 Elsevier Science B.V. All rights reserved.