Chromatographic Methods for the Determination of Emerging Contaminants in Natural Water and Wastewater Samples: A Review.

This review is devoted to analytical methods published in the scientific literature in the last 10 years for the determination of emerging contaminants in aquatic media. The article is mainly focused on sample preparation and on instrumental techniques most used for the detection and quantification of the analytes of interest. The sample preparation techniques include classical liquid-liquid extraction and solid-phase extraction, but also recent microextraction techniques such as solid-phase microextraction, stir-bar sorptive extraction, dispersive liquid-liquid microextraction, ultrasound-assisted emulsification microextraction, or microextraction by packed sorbent. Most studies focus on minimizing the number of analysis steps and on the use of the lowest amount of solvents in the sample treatment step. Liquid chromatography and gas chromatography mainly coupled to tandem mass spectrometry are usually the employed analytical techniques. A large number of multiresidue methods are being developed for the determination of several families of these compounds with only one extraction step to minimize sample handling and treatment.

Determination of bisphenols with estrogenic activity in plastic packaged baby food samples using solid-liquid extraction and clean-up with dispersive sorbents followed by gas chromatography tandem mass spectrometry analysis.

Bisphenols (BPs) are a family of chemicals with known endocrine disrupting activity. Bisphenol A (BPA) is the most representative prototype of this group of chemicals. Recently, the use of BPA, a prototype of endocrine disruptors, has been reduced and replaced with structural analogs due to its negative effects on both the environment and consumers. In this work, a new method is presented for the determination of seven BPs, with estrogenic activity in ready-to-eat plastic packaged baby foods. The procedure involves the isolation of the analytes using solid-liquid phase extraction with acetonitrile followed by a clean-up step with a mixture of dispersive-SPE sorbents (C18 and PSA) and magnesium sulphate, to reduce matrix effect from proteins, sugars and lipids. Extraction parameters were optimized using multivariate optimization methods. The compounds were detected and quantified by gas chromatography tandem mass spectrometry (GC-MS/MS). The limits of quantification were between 0.1 and 1.2ngg-1 for the studied analytes. The method was validated using matrix-matched calibration and recovery assays with spiked samples. Recovery rates were between 91% and 110% and % RSD was lower than 13% in all cases. The method has been successfully applied for the determination of these endocrine disrupting chemicals (EDCs) in samples of a novel type of food consumed by pre-schoolers. This is the first study to analyze EDCs in plastic packaged foods consumed by this target group.