Kochale, Kjell; Lang, Björn; Cunha, Ricardo; Teutenberg, Thorsten; Schmidt, Torsten C.:
Online coupling of miniaturized HPLC and high performance thin layer chromatography by a fractionation unit for effect directed analysis
In: Advances in Sample Preparation, Band 9 (2024), Artikel 100102
2024Artikel/Aufsatz in ZeitschriftOA Gold
ChemieFakultät für Chemie » Analytische Chemie
Damit verbunden: 1 Publikation(en)
Titel in Englisch:
Online coupling of miniaturized HPLC and high performance thin layer chromatography by a fractionation unit for effect directed analysis
Autor*in:
Kochale, Kjell
;
Lang, Björn
;
Cunha, Ricardo
;
Teutenberg, Thorsten
Sonstiges
korrespondierende*r Autor*in
;
Schmidt, Torsten C.UDE
GND
1074278453
LSF ID
14592
ORCID
0000-0003-1107-4403ORCID iD
Sonstiges
der Hochschule zugeordnete*r Autor*in
Erscheinungsjahr:
2024
Open Access?:
OA Gold
Web of Science ID
Scopus ID
Notiz:
CA extern
Sprache des Textes:
Englisch
Schlagwort, Thema:
Acetylcholinesterase ; Automation ; Effect-directed analysis ; Fractionation ; Miniaturized HPLC ; Thin-layer chromatography
Ressourcentyp:
Text

Abstract in Englisch:

The rising discharge of anthropogenic chemicals into aquatic environments poses a significant threat, necessitating effective monitoring strategies. This study introduces an innovative approach to effect-directed analysis (EDA) by coupling liquid chromatography (LC) with high-performance thin-layer chromatography (HPTLC), utilizing a modified MALDI spotter. The objective is to optimize fractionation parameters for sample application and assess the method's viability in identifying acetylcholinesterase (AChE) inhibitors, specifically malathion, parathion, and chlorfenvinphos. The optimization process involves controlling sample volume, spot shape, and spot distances on HPTLC plates. Successful application is demonstrated by a miniaturized LC system coupled to the HPTLC plate via spotter, allowing effective separation and identification of AChE inhibitors. The study further explores the method's application to water samples from a river with predominantly agricultural drainage area. Spiked samples reveal distinct active spots, identified through extraction and subsequent high-resolution mass spectrometry (HRMS) measurements. However, results indicate the absence of AChE inhibitors in non-spiked water samples, affirming the efficacy of the EU ban on most organophosphate pesticides. The usefulness of HPTLC in separation of coeluting substances from HPLC is emphasized, demonstrating its suitability for the effect-directed analysis of complex samples. This work shows the integration of HPTLC with liquid chromatography for EDA, offering a powerful tool for identifying and monitoring AChE inhibitors in water samples. The approach addresses limitations in current monitoring strategies and provides insights into the presence and impact of chemicals in aquatic ecosystems. The study contributes to ongoing efforts to enhance water quality monitoring, aligning with the principles of the EU Water Framework Directive.