A modified micro-solid phase extraction device for in-port elution and injection into portable liquid chromatography: A proof-of-concept study.

A micro-solid phase extraction (micro-SPE) device packed with a C18 sorbent (10 mg) has been developed for the enrichment and purification of organic water pollutants prior to their analysis using a portable liquid chromatograph with a dual UV detector. To this end, the sorbent was immobilized at the inlet of a 4 mm syringe filter (0.20 µm), which was modified to reduce its internal volume. The filter was coupled to the needle of the chromatograph. After loading the sample and cleaning the sorbent for analyte purification, the device was installed into the injection port of the chromatograph, and the target compounds were desorbed and transferred directly to the chromatographic column with a small volume of organic solvent. Under optimized conditions, sample volumes as large as 50 mL could be processed with the micro-SPE device, while the analytes were desorbed with only 60 µL of methanol. As a result, efficient preconcentration could be reached, as demonstrated for different water contaminants, namely aclonifen, bifenox, tritosulfuron, triflusulfuron-methyl and caffeine. The proposed micro-SPE device was applied to the analysis of different types of water (river, well, sea, ditch and wastewater). The recoveries of the target compounds in samples ranged from 76 % to 109 %, which allowed their detection at low to sub µg/L levels. All operations were carried out manually, and thus, no additional laboratory instruments such as centrifuges, stirrers or evaporators were required. This proof-of-concept study shows that the proposed micro-SPE approach can be considered a reliable and effective option for the on-site analysis of pollutants in environmental water samples by portable liquid chromatography.