RT Journal Article
T1 Development and application of an in-house library and workflow for gas chromatography–electron ionization–accurate-mass/high-resolution mass spectrometry screening of environmental samples
A1 Castro Bustelo, Verónica
A1 Quintana Álvarez, José Benito
A1 López Vázquez, Javier
A1 Carro Mariño, Nieves
A1 Cobas Sáenz, Julio César
A1 Bilbao Alemany, Denís
A1 Cela Torrijos, Rafael
A1 Rodil Rodríguez, María del Rosario
K1 Gas chromatography–quadrupole time of flight (GC-QTOF)
K1 Contaminants of emerging concern (CECs)
K1 Persistent organic pollutants (POPs)
K1 Kovats retention index
K1 Matrix solid-phase dispersion (MSPD)
AB This work presents an optimized gas chromatography–electron ionization–high-resolution mass spectrometry (GC-EI-HRMS) screening method. Different method parameters affecting data processing with the Agilent Unknowns Analysis SureMass deconvolution software were optimized in order to achieve the best compromise between false positives and false negatives. To this end, an accurate-mass library of 26 model compounds was created. Then, five replicates of mussel extracts were spiked with a mixture of these 26 compounds at two concentration levels (10 and 100 ng/g dry weight in mussel, 50 and 500 ng/mL in extract) and injected in the GC-EI-HRMS system. The results of these experiments showed that accurate mass tolerance and pure weight factor (combination of reverse-forward library search) are the most critical factors. The validation of the developed method afforded screening detection limits in the 2.5–5 ng range for passive sampler extracts and 1–2 ng/g for mussel sample extracts, and limits of quantification in the 0.6–3.2 ng and 0.1–1.8 ng/g range, for the same type of samples, respectively, for 17 model analytes. Once the method was optimized, an accurate-mass HRMS library, containing retention indexes, with ca. 355 spectra of derivatized and non-derivatized compounds was generated. This library (freely available at https://doi.org/10.5281/zenodo.5647960), together with a modified Agilent Pesticides Library of over 800 compounds, was applied to the screening of passive samplers, both of polydimethylsiloxane and polar chemical integrative samplers (POCIS), and mussel samples collected in Galicia (NW Spain), where a total of 75 chemicals could be identified
PB Springer
SN 1618-2642
YR 2021
FD 2021
LK http://hdl.handle.net/10347/28994
UL http://hdl.handle.net/10347/28994
LA eng
NO Castro, V., Quintana, J.B., López-Vázquez, J. et al. Development and application of an in-house library and workflow for gas chromatography–electron ionization–accurate-mass/high-resolution mass spectrometry screening of environmental samples. Anal Bioanal Chem (2021). https://doi.org/10.1007/s00216-021-03810-w
NO Open Access funding provided thanks to the CRUE-CSIC agreement with Springer Nature. This research was funded by Xunta de Galicia (ED431C 2021/06 and V.C. predoctoral contract: ED481A-2017/156), the Spanish Agencia Estatal de Investigación—MCIN/AEI/10.13039/501100011033 (ref. CTM2017-84763-C3-R-2 and PID2020-117686RB-C32), and FEDER/ERDF funds
DS Minerva
RD 25 abr 2026