RT Journal Article
T1 Supercritical fluid chromatography time-of-flight mass spectrometry enantiomeric determination of basic drugs in sewage samples
A1 Cobo Golpe, Miguel
A1 Ramil Criado, María
A1 Cela Torrijos, Rafael
A1 Rodríguez Pereiro, Isaac
K1 Supercritical fluid chromatography
K1 Chiral separations
K1 Mass spectrometry
K1 Basic pharmaceuticals
K1 Wastewater
K1 Sludge
AB Many pharmacologically active compounds are chiral species, and their therapeutic or toxicological effects might differ between isomers. Herein, we develop a fast and sensitive chiral analysis methodology for the determination of eight pharmaceuticals, considered as emerging environmental pollutants and belonging to two different chemical classes, in wastewater and sludge samples. Compounds were separated using supercritical fluid chromatography (SFC) combined with time-of-flight mass spectrometry (TOF-MS) detection. The stationary phase, the modifier and the additive combined with supercritical carbon dioxide (CO2), in the SFC mobile phase, played a major effect in the enantiomeric resolution of selected compounds. Moreover, the composition of the mobile phase affected their ionization efficiency in the electrospray ionization source. Methanol (MeOH), containing a 0.1% of ammonia, was used as CO2 modifier for the separation of compounds in a polysaccharide-type column. Total analysis time was 15.5 min, achieving resolution factors between 1.03 and 2.49 for the eight pairs of enantiomers. In combination with mixed-mode solid-phase extraction and matrix solid-phase dispersion protocols, compounds were determined in wastewater and sludge samples, with limits of quantification in the range of 0.010–0.020 µg L−1 and 3.7–11.1 ng g−1, for aqueous and solid samples, respectively. The amine-type drugs (tramadol, propranolol and venlafaxine) were mostly found in wastewater samples, whilst azolic antimycotics were mainly quantified in sludge. The first group of compounds showed enantiomeric fractions significantly different to those existing in the commercial counterpart pharmaceuticals
PB Elsevier
YR 2022
FD 2022
LK http://hdl.handle.net/10347/29050
UL http://hdl.handle.net/10347/29050
LA eng
NO Journal of Chromatography A Volume 1673 (2022) 463088. https://doi.org/10.1016/j.chroma.2022.463088
NO This study was supported through grants PGC2018-094613-B-I00 and ED431C 2021/06, funded by Spanish Government and Xunta de Galicia, respectively. Both projects are co-funded by the EU FEDER program. M.C.G. thanks a FPI fellowship to the Ministry of Science and Education (Spain)
DS Minerva
RD 27 abr 2026