Simultaneous determination of a variety of endocrine disrupting compounds in carrot, lettuce and amended soil by means of focused ultrasonic solid–liquid extraction and dispersive solid-phase extraction as simplified clean-up strategy

• Published in: Journal of Chromatography A 2015-04, Vol.1389, p.8-18
• Main Authors: Mijangos, L., Bizkarguenaga, E., Prieto, A., Fernández, L.A., Zuloaga, O.
• Format: Article
• Language: English
• Subjects: Analytical chemistry; Bisphenol A; Carrots; Chromatography; Cleaning; Compost amended soil; Daucus; Dispersive solid-phase extraction; Endocrine-disrupting compound; Extraction; Focused ultrasonic solid–liquid extraction; Lettuces; Liquid chromatography–tandem mass spectrometry; Soil (material); Vegetables
• ISSN: 0021-9673
• DOI: 10.1016/j.chroma.2015.02.036

•Development of a FUSLE-dSPE-LC–(ESI)-MS/MS method for the analysis of EDCs.•An exhaustive evaluation of liquid chromatography–tandem mass spectrometry.•Through optimisation of focused ultrasound extraction variables.•Dispersive solid phase extraction as simplified clean-up strategy. The present study is focused on the development of an analytical method based on focused ultrasonic solid–liquid extraction (FUSLE) followed by dispersive solid-phase extraction (dSPE) clean-up and liquid chromatography–triple quadrupole tandem mass spectrometry (LC–MS/MS) optimised for the simultaneous analysis of certain endocrine disrupting compounds (EDCs), including alkylphenols (APs), bisphenol A (BPA), triclosan (TCS) and several hormones and sterols in vegetables (lettuce and carrot) and amended soil samples. Different variables affecting the chromatographic separation, the electrospray ionisation and mass spectrometric detection were optimised in order to improve the sensitivity of the separation and detection steps. Under the optimised extraction conditions (sonication of 5min at 33% of power with pulse times on of 0.8s and pulse times off of 0.2s in 10mL of n-hexane:acetone (30:70, v:v) mixture using an ice bath), different dSPE clean-up sorbents, such as Florisil, Envi-Carb, primary-secondary amine bonded silica (PSA) and C18, or combinations of them were evaluated for FUSLE extracts before LC–MS/MS. Apparent recoveries and precision in terms of relative standard deviation (RSDs %) of the method were determined at two different fortification levels (according to the matrix and the analyte) and values in the 70–130% and 2–27% ranges, respectively, were obtained for most of the target analytes and matrices. Matrix-matched calibration approach and the use of labelled standards as surrogates were needed for the properly quantification of most analytes and matrices. Method detection limits (MDLs), estimated with fortified samples, in the ranges of 0.1–100ng/g for carrot, 0.2–152ng/g for lettuce and 0.9–31ng/g for amended soil were obtained. The developed methodology was applied to the analysis of 11 EDCs in both real vegetable bought in a local market and in compost (from a local wastewater treatment plant, WWTP) amended soil samples.