Determination of triazine herbicides in aqueous samples by dispersive liquid–liquid microextraction with gas chromatography–ion trap mass spectrometry

A simple and rapid new dispersive liquid–liquid microextraction technique (DLLME) coupled with gas chromatography–ion trap mass spectrometric detection (GC–MS) was developed for the extraction and analysis of triazine herbicides from water samples. In this method, a mixture of 12.0 μL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected by syringe into the 5.00 mL water sample containing 4% (w/v) sodium chloride. In this process, triazines in the water sample are extracted into the fine droplets of chlorobenzene. After centrifuging for 5 min at 6000 rpm, the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (8.0 ± 0.3 μL). The settled phase (2.0 μL) is collected and injected into the GC–MS for separation and determination of triazines. Some important parameters, viz, type of extraction solvent, identity and volume of disperser solvent, extraction time, and salt effect, which affect on DLLME were studied. Under optimum conditions the enrichment factors and extraction recoveries were high and ranged between 151–722 and 24.2–115.6%, respectively. The linear range was wide (0.2–200 μg L−1) and the limits of detection were between 0.021 and 0.12 μg L−1 for most of the analytes. The relative standard deviations (RSDs) for 5.00 μg L−1 of triazines in water were in the range of 1.36–8.67%. The performance of the method was checked by analysis of river and tap water samples, and the relative recoveries of triazines from river and tap water at a spiking level of 5.0 μg L−1 were 85.2–114.5% and 87.8–119.4%, respectively. This method was also compared with solid-phase microextraction (SPME) and hollow fiber protected liquid-phase microextraction (HFP-LPME) methods. DLLME is a very simple and rapid method, requiring less than 3 min. It also has high enrichment factors and recoveries for the extraction of triazines from water.