Lab-In-Syringe automation of deep eutectic solvent-based direct immersion single drop microextraction coupled online to high-performance liquid chromatography for the determination of fluoroquinolones

YILDIRIM S., Cocovi-Solberg D. J., USLU B., Solich P., Horstkotte B.

TALANTA, vol.246, 2022 (SCI-Expanded) identifier identifier identifier

  • Publication Type: Article / Article
  • Volume: 246
  • Publication Date: 2022
  • Doi Number: 10.1016/j.talanta.2022.123476
  • Journal Name: TALANTA
  • Journal Indexes: Science Citation Index Expanded (SCI-EXPANDED), Scopus, Academic Search Premier, L'Année philologique, Aerospace Database, Analytical Abstracts, Aqualine, Aquatic Science & Fisheries Abstracts (ASFA), BIOSIS, CAB Abstracts, Chemical Abstracts Core, Communication Abstracts, EMBASE, Food Science & Technology Abstracts, MEDLINE, Metadex, Pollution Abstracts, Veterinary Science Database, Civil Engineering Abstracts
  • Keywords: Automation of sample preparation, Natural deep eutectic solvent, Fluoroquinolone antibiotics, Lab-in-syringe, Directly immersed single drop microextraction, Online coupling to HPLC, SOLID-PHASE EXTRACTION, SEQUENTIAL-INJECTION, ENVIRONMENTAL WATER, FLOW-BATCH, SAMPLES, QUANTIFICATION, OPTIMIZATION, ANTIBIOTICS, OFLOXACIN
  • Karadeniz Technical University Affiliated: Yes


Lab-In-Syringe direct immersion single drop microextraction is proposed as an automated sample pretreatment methodology and coupled online to HPLC with fluorescence detection for the determination of fluoroquinolones in environmental waters. For the first time, a drop of a natural deep eutectic solvent (NADES), synthesized from hexanoic acid and thymol, has been used as an extractant in automated single-drop microextraction. The extraction procedure was carried out within the 5 mL void of an automatic syringe pump. A 9-position head valve served the aspiration of all required solutions, air, waste disposal, and hyphenation with the HPLC instrument. Sample mixing during extraction was done by a magnetic stirring bar placed inside the syringe. Only 60 mu L of NADES were required omitting toxic classical solvents and improving the greenness of the proposed methodology. By direct injection, linear working ranges between 0.1 and 5 mu g L-1 were achieved for all fluoroquinolones. The limit of quantification values and enrichment factors ranged from 20 ng L-1 to 30 ng L-1 and 35 to 45, respectively. Accuracies obtained from the analysis of spiked surface water and wastewater treatment plant effluent analysis at two concentration levels (0.5 and 4 mu g L-1) ranged from 84.6% to 119.7%, with RSD values typically <3%.