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Anal Chem. 2009 Sep 1;81(17):7373-8. doi: 10.1021/ac9008995.

Single-step LC/MS method for the simultaneous determination of GC-amenable organochlorine and LC-amenable phenoxy acidic pesticides.

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Dipartimento di Scienze Geologiche, Tecnologie Chimiche e Ambientali, Università degli Studi di Urbino Carlo Bo, Piazza Rinascimento 6, 61029 Urbino, Italy.


Water pollution by organochlorine pesticides (OCPs) is considered as an analytical challenge, since these persistent and nonbiodegradable pollutants are not amenable by liquid chromatography coupled to atmospheric pressure ionization mass spectrometry (LC/API-MS). This represents a significant constraint in multiresidue analysis of real samples, when high polar, poorly volatile compounds are present as well. This paper reports the development of an innovative single-step method for the simultaneous determination of OCPs and polar pesticides belonging to the class of phenoxy acids in water samples. The method is based on an off-line solid-phase extraction (SPE) procedure with Carbograph 4 followed by liquid chromatography coupled to a direct electron ionization mass spectrometer (LC/direct-EI-MS). The direct-EI capability of acquiring high-quality EI spectra and operation in selected ion monitoring mode allowed a precise quantification of OCPs and phenoxy acids in a single chromatographic run without derivatization. The instrumental response was characterized by excellent sensitivity, linearity, and precision. The SPE recovery rates in river water gave values equal or better than 80% for most of the compounds. The method limits of detection (LODs) span from 0.002 to 0.052 microg/L, allowing the detection of the selected pesticides at the limits required by the European Union (EU) legislation for drinking water.

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