2024-03-28T15:07:30Zhttp://digital.csic.es/dspace-oai/requestoai:digital.csic.es:10261/1504962017-12-18T14:33:07Zcom_10261_31891com_10261_2col_10261_31892
DIGITAL.CSIC
author
Pérez-Ortega, Patricia
author
Gilbert-López, Bienvenida
author
Molina-Díaz, Antonio
author
García-Reyes, Juan F.
funder
Universidad de Jaén
funder
Junta de Andalucía
funder
Ministerio de Economía y Competitividad (España)
funder
European Commission
funder
Ministry of Education and Culture (Hungary)
2017-05-26T10:43:06Z
2017-05-26T10:43:06Z
2016
Analytical and Bioanalytical Chemistry 408(18): 4857-4869 (2016)
http://hdl.handle.net/10261/150496
10.1007/s00216-016-9589-6
http://dx.doi.org/10.13039/501100007064http://dx.doi.org/10.13039/501100003329http://dx.doi.org/10.13039/501100000780http://dx.doi.org/10.13039/501100011011
The aim of the study was to evaluate the performance of different chromatographic approaches for the liquid chromatography/mass spectrometry (LC-MS(/MS)) determination of 24 highly polar pesticides. The studied compounds, which are in most cases unsuitable for conventional LC-MS(/MS) multiresidue methods were tested with nine different chromatographic conditions, including two different hydrophilic interaction liquid chromatography (HILIC) columns, two zwitterionic-type mixed-mode columns, three normal-phase columns operated in HILIC-mode (bare silica and two silica-based chemically bonded columns (cyano and amino)), and two standard reversed-phase C columns. Different sets of chromatographic parameters in positive (for 17 analytes) and negative ionization modes (for nine analytes) were examined. In order to compare the different approaches, a semi-quantitative classification was proposed, calculated as the percentage of an empirical performance value, which consisted of three main features: (i) capacity factor (k) to characterize analyte separation from the void, (ii) relative response factor, and (iii) peak shape based on analytes’ peak width. While no single method was able to provide appropriate detection of all the 24 studied species in a single run, the best suited approach for the compounds ionized in positive mode was based on a UHPLC HILIC column with 1.8 μm particle size, providing appropriate results for 22 out of the 24 species tested. In contrast, the detection of glyphosate and aminomethylphosphonic acid could only be achieved with a zwitterionic-type mixed-mode column, which proved to be suitable only for the pesticides detected in negative ion mode. Finally, the selected approach (UHPLC HILIC) was found to be useful for the determination of multiple pesticides in oranges using HILIC-ESI-MS/MS, with limits of quantitation in the low microgram per kilogram in most cases.
eng
closedAccess
HILIC
Food
Pesticide testing
LC-MS
Mixed mode
Polar pesticides
Study of different HILIC, mixed-mode, and other aqueous normal-phase approaches for the liquid chromatography/mass spectrometry-based determination of challenging polar pesticides
artículo
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URL
https://digital.csic.es/bitstream/10261/150496/1/accesoRestringido.pdf
File
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42637ae8545636bc41605c1740a9a84e
15753
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accesoRestringido.pdf