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Trace analysis of parabens, triclosan and related chlorophenols in water by headspace solid-phase microextraction with in situ derivatization and gas chromatography-tandem mass spectrometry.

Journal of chromatography. A (2009-05-06)
Jorge Regueiro, Elias Becerril, Carmen Garcia-Jares, Maria Llompart
ABSTRACT

An in situ derivatization solid-phase microextraction method has been developed for the determination of parabens, triclosan and related chlorophenols in water. Acetylated derivatives are selectively determined using gas chromatography with tandem mass spectrometry. Parameters affecting both derivatization and SPME procedures, such as fiber coating, extraction mode, temperature, volume of derivatizating reagent and ionic strength, are studied and optimized through a multifactorial experimental design. The performance of the method is studied in terms of accuracy, linearity, precision and limits of detection. Quantitative recoveries (> or =82%) and satisfactory precision (RSD< or =12%) are obtained. Limits of detection at the low picogram per millilitre level are achieved for all target compounds. Linearity is studied in a wide range of concentrations and an analysis of variance with a lack-of-fit test is run to validate the calibration data. Extraction time profiles are also obtained. Finally, the applicability of the proposed method is demonstrated for several real samples including river water, wastewaters and swimming pool water. Since no matrix effects are observed, quantification can readily be carried out by external calibration with ultrapure water standards.

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Ethyl 4-hydroxybenzoate, ReagentPlus®, 99%