Determination of selected organic contaminants in soil by pressurized liquid extraction and gas chromatography tandem mass spectrometry with in situ derivatization

• Published in: Journal of Chromatography A Vol. 1248; pp. 9 - 17
• Main Authors: Albero, Beatriz, Sánchez-Brunete, Consuelo, Miguel, Esther, Pérez, Rosa A., Tadeo, José L.
• Format: Journal Article
• Language: English
• Published: Netherlands Elsevier B.V 27.07.2012
• Subjects: derivatization; gas chromatography; Gas Chromatography-Mass Spectrometry - methods; Gas chromatography–tandem mass spectrometry; In situ derivatization; Limit of Detection; Linear Models; Liquid-Liquid Extraction - methods; Organic contaminants; Parabens - analysis; Parabens - isolation & purification; physicochemical properties; polybrominated diphenyl ethers; polychlorinated biphenyls; Polychlorinated Biphenyls - analysis; Polychlorinated Biphenyls - isolation & purification; polycyclic aromatic hydrocarbons; Pressure; Pressurized liquid extraction; Salicylates - analysis; Salicylates - isolation & purification; Soil; Soil - analysis; Soil Pollutants - analysis; Soil Pollutants - isolation & purification; soil pollution; soil sampling; Tandem Mass Spectrometry; Pressurized liquid extraction; Soil; Gas chromatography–tandem mass spectrometry; Organic contaminants; In situ derivatization
• ISSN: 0021-9673; 1873-3778
• DOI: 10.1016/j.chroma.2012.05.078

► Simultaneous analysis of forty organic contaminants in soil. ► In situ derivatization by means of sandwich injection. ► GC–MS/MS analysis after pressurized liquid extraction. ► Determination of organic contaminants in Spanish agricultural fields. The determination of organic contaminants in soil is a real challenge due to the large number of these compounds with quite different physico-chemical properties. In the present work, an analytical method was developed for the simultaneous determination in soil of 40 organic contaminants belonging to different chemical classes: polycyclic aromatic hydrocarbons, polychlorinated biphenyls, polybrominated diphenyl ethers, UV filters, parabens, bisphenols and triclosan. Soil was extracted by pressurized liquid extraction and the extracts, without the need of a clean-up step, were analyzed by gas chromatography–tandem mass spectrometry after in situ derivatization in the gas chromatographic system. In the pressurized liquid extraction step, two extraction cycles were performed with a mixture of ethyl acetate–methanol (90:10, v/v) at 80°C. Recovery of these contaminants from soil samples spiked at levels ranging from 30 to 120ngg−1 was satisfactory for most of the compounds. The developed procedure provided detection method limits from 0.1 to 2.5ngg−1. The analysis of soil samples collected in different agricultural fields confirmed the presence of some of the studied contaminants. Polycyclic aromatic hydrocarbons were the main contaminants detected, parabens and polychlorinated biphenyls were also found but at relatively low concentration levels, 2-ethylhexyl salicylate was the UV filter that appeared most frequently at levels ranging from 17.2 to 43.4ngg−1 and triclosan was found in eight out of fourteen samples, at relatively low concentration levels (0.8–28.6ngg−1).