Thermally condensed humic acids onto silica as SPE for effective enrichment of glucocorticoids from environmental waters followed by HPLC-HESI-MS/MS.
J Chromatogr A
; 1540: 38-46, 2018 Mar 09.
Article
en En
| MEDLINE
| ID: mdl-29429744
ABSTRACT
Pristine humic acids (HAs) were thermally condensed onto silica microparticles by a one-pot, inexpensive and green preparation route obtaining a mixed-mode sorbent (HA-C@silica) with good sorption affinity for glucocorticoids (GCs). The carbon-based material, characterized by various techniques, was indeed applied as the sorbent for fixed-bed solid-phase extraction of eight GCs from river water and wastewater treatment plant effluent, spiked at different concentration levels in the range 1-400â¯ngâ¯L-1. After sample extraction, the target analytes were simultaneously and quantitatively eluted in a single fraction of methanol, achieving enrichment factor 4000 and 1000 in river water and wastewater effluent, respectively. Full recovery for all compounds, was gained in the real matrices studied (80-125% in river water, 79-126% in wastewater effluent), with inter-day precision showing relative standard deviations (RSD) below 15% and 18% (nâ¯=â¯3), for river and wastewater effluent, correspondingly. The high enrichment factors coupled with high-performance liquid chromatography tandem mass spectrometry quantification (MRM mode) provided method quantification limits of 0.009-0.48â¯ngâ¯L-1 in river water and 0.06-3â¯ngâ¯L-1 in wastewater effluent and, at the same time, secure identification of the selected drugs. As also evidenced by comparison with literature, HA-C@silica proved to be a valid alternative to the current commercial sorbents, in terms of extraction capability, enrichment factor, ease of preparation and cost. The batch-to-batch reproducibility was assessed by recovery tests on three independently prepared HA-C@silica powders (RSD lower than 7%).
Palabras clave
Texto completo:
1
Colección:
01-internacional
Base de datos:
MEDLINE
Contexto en salud:
2_ODS3
Problema de salud:
2_quimicos_contaminacion
Asunto principal:
Monitoreo del Ambiente
/
Cromatografía Líquida de Alta Presión
/
Dióxido de Silicio
/
Espectrometría de Masas en Tándem
/
Extracción en Fase Sólida
/
Glucocorticoides
/
Sustancias Húmicas
Tipo de estudio:
Prognostic_studies
Idioma:
En
Revista:
J Chromatogr A
Año:
2018
Tipo del documento:
Article