A multi-residue method for determination of 70 organic micropollutants in surface waters by solid-phase extraction followed by gas chromatography coupled to tandem mass spectrometry

Abstract

A multi-residue method, based on gas chromatography coupled to tandem mass spectrometry (GC-MS/MS), has been developed for the determination of 70 organic micropollutants from various chemical classes (organochlorinated, organophosphorous, triazines, carbamate and urea, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, pharmaceuticals, phenols, etc.) in surface waters. A single-step SPE extraction using OASIS HLB cartridges was employed for the recovery of target micropollutants. The method has been validated according to monitoring performance criteria of the Water Framework Directive, taking into account the approved guidelines on quality assurance and quality control. The recoveries ranged from 60 to 110 %, the coefficient of variation from 0.84 to 27.4 %, and the uncertainty from 6 to 37 %. The LOD varied from 6.0 to 40 ng/L. The limits of quantification for the priority pollutants anthracene, alachlor, atrazine, benzo(a)pyrene, chlorfenvinphos, diuron, isoproturon, nonylphenol, simazine, and terbutryn fulfill the criterion of <30 % of the relevant environmental standards. The method was employed to investigate the water quality in the basin of a transboundary river, Strymonas, in NE Greece during three sampling campaigns conducted in the year 2013. Thirty-nine compounds were detected in the river water. Metolachlor, diuron, isoproturon, salicylic acid, chlorfenvinphos, 1,2-benzanthracene, pyrene, diflubenzuron, and carbaryl exhibited the highest detection frequencies.

Pesticides in the surface waters of Lake Vistonis Basin, Greece: Occurrence and environmental risk assessment

“…Lindane has been detected in the rivers Axios, Evros and Ardas in Greece in similar concentrations in the past years and its presence was attributed to transboundary pollution (Vryzas et al, 2009). In more recent studies, lindane was either not detected (Terzopoulou et al, 2015) or detected up to 0.062 μg/L in Strymon River, Greece (Litskas et al, 2012).…”

Simultaneous determination of alachlor and its metabolites in beef muscle, liver, milk, and egg by liquid chromatography–tandem mass spectrometry

“…ALA and possible metabolites such as 2‐chloro‐ N ‐(2,6‐diethylphenyl) acetamide (CDA), 2,6‐diethylaniline (DEA), and 2‐ethyl‐6‐(1‐hydroxyethyl) aniline (HEEA; Figure 1), which can diffuse into groundwater and disperse in the environment, cause serious ecological and physiological problems [20–22]. GC techniques have been considered for multiresidue monitoring methodology of herbicides [23–27]. On the other hand, recent studies showed that LC–MS or tandem mass spectrometry (LC–MS/MS) was used for the determination of ALA and its metabolites [10,28–31].…”

Determination of Ten Macrolide Drugs in Environmental Water Using Molecularly Imprinted Solid-Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry

“…Liquid chromatography-tandem mass spectrometry (LC-MS/MS), which has the advantages of unambiguous identification and accurate quantification, is the preferred strategy to detect MALs in water [ 10 , 11 , 12 ]. Besides, a pre-concentration step such as solid-phase extraction (SPE) or lyophilization is indispensable for the analysis of water samples [ 13 , 14 , 15 ]. However, the lyophilization procedure is time-consuming (more than 24 h for lyophilization) and the quantification of target compounds would be affected by the impurities.…”