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.

• Klíčová slova
• Alkylphenols, High performance liquid chromatography, Iron(III) thenoyltrifluoroacetonate complex, Lab-in-syringe automation, Solvent-assisted dispersive solid phase Extraction,
• MeSH
• automatizace MeSH
• chemické látky znečišťující vodu analýza   izolace a purifikace   MeSH
• chromatografie kapalinová metody   MeSH
• fenoly * izolace a purifikace   analýza   chemie   MeSH
• injekční stříkačky * MeSH
• limita detekce MeSH
• mikroextrakce na pevné fázi * metody   MeSH
• vysokoúčinná kapalinová chromatografie MeSH
• železité sloučeniny chemie   MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• chemické látky znečišťující vodu MeSH
• fenoly * MeSH
• železité sloučeniny MeSH

In this work, we describe for the first time the use of iron(III) thenoyltrifluoroacetonate complex (Fe(TTA)3) as a novel sorbent for solvent-assisted dispersive micro-solid phase extraction (SA-dμSPE) of bisphenols from water samples. The extraction procedure is based on the formation of nanoparticles in situ following the rapid injection of a methanolic solution of Fe(TTA)3 into the stirred aqueous sample. Herein, the synthesis of Fe(TTA)3 and study of the essential parameters of the preparative procedure are described. The optimized procedure allowed for efficient enrichment of bisphenols from various water samples, chosen as model contaminants and matrix, within 2.5 min. The sorbent was collected by centrifugation, dissolved in methanol, and injected to perform HPLC with spectrophotometric detection. The limits of detection and quantification obtained ranged from 1.0-3.1 and 3.1-7.5 μg L-1, respectively. Intraday and interday precisions of <7% relative standard deviation (RSD) and <8% RSD with analyte recoveries ranging between 70-117% (103.8% on average) were obtained for the analysis of river water, wastewater treatment plant effluent, and bottled water.

• Publikační typ
• časopisecké články MeSH