BACKGROUND: Alkylphenols are water contaminants of strong endocrine disruptive potential. Sample preparation is generally imperative to improve sensitivity and minimize matrix effects. Dispersive solid phase extraction is a powerful alternative to cartridge-based sorbent extraction omitting backpressure problems and reducing procedural time. Herein, solvent-dissolvable sorbents offer the advantages of easy and cost-efficient production, efficiency, and full analyte recovery, while eluates can be directly submitted to instrumental determination. Despite the potential to reduce environmental impact and enhance reproducibility, there is a lack of automation attempts. RESULTS: A fully automated solvent-assisted dispersive solid phase extraction method was developed for selected alkylphenols based on the technique Lab-In-Syringe. The void of automatic bidirectional syringe pump was used as mixing and extraction vessel. The iron(III) thenoyltrifluoroacetonate complex was used as novel dissolvable sorbent. 40 μL complex solution was dispersed in the sample, leading to the precipitation of 0.4 mg sorbent. Extraction occurred within 40 s and was accelerated by in-syringe magnetic stirring. The sorbent was retained on a melamine foam packing in the syringe inlet, dissolved in a methanolic solution of ascorbic acid, and injected into online-coupled HPLC. Linear working ranges were achieved from 1 to 1000 μg/L with sub-ppb detection limits and accuracies ranging from 98.3 to 110 %. SIGNIFICANCE: In this work, we explored for the first time automated in-syringe automated dispersive SPE based on a dissolvable sorbent. Parallel operation of sample pretreatment and separation enabled throughputs of 4.5/h with typically <5 % RSD and preconcentrations of 16.4-21.2. AGREE greenness evaluation yielded a score of 0.59.

Department of Analytical Chemistry Faculty of Pharmacy in Hradec Králové Charles University Akademika Heyrovského 1203 500 03 Hradec Králové Czech Republic

Karadeniz Technical University Faculty of Pharmacy Department of Analytical Chemistry Farabi Street 61080 Trabzon Türkiye

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