Multiclass determination of 66 organic micropollutants in environmental water samples by fast gas chromatography–mass spectrometry

A multiresidue method has been developed for quantification and identification of 66 multiclass priority organic pollutants in water by fast gas chromatography (GC) coupled to mass spectrometry (MS). Capabilities and limitations of single quadrupole mass spectrometer as detector in fast GC were studied evaluating the chromatographic responses in terms of sensitivity and chromatographic peak shapes, as they were influenced by scan time. The number of monitored ions in a selected ion monitoring (SIM) group strongly conditioned the scan time and subsequently the number of data points per peak. A compromise between peak shape and scan time was adopted in order to reach the proper conditions for quantitative analysis. An average of 10–15 points per peak was attained for most compounds, involving scan times between 0.1 and 0.22 s. The method was validated for mineral, surface, and groundwater. A solid-phase extraction pre-concentration step using C18 cartridges was applied. Four isotopically labeled standards were added to the samples before extraction and used as surrogates to ensure a reliable quantification. Analyses were performed by GC–MS in electron ionization mode, monitoring the three most abundant and/or specific ions for each compound and using the intensity ratios as a confirmatory parameter. With a chromatographic run of less than 10 min, SIM mode provided excellent sensitivity and identification capability due to the monitoring of three ions and the evaluation of their intensity ratio. Limits of detection below 10 ng/L were reached for most of the 66 compounds in the three matrices studied. Accuracy and precision of the method were evaluated by means of recovery experiments at two fortification levels (10 and 100 ng/L), obtaining recoveries between 70% and 120% in most cases and relative standard deviations below 20%. The possibilities of a simultaneous SIM scan method have also been explored for non-target qualitative analysis. The developed method has been applied to the analysis of surface water samples collected from the Mediterranean region of Spain.