| Title: | Simultaneous analysis of highly polar and multi-residue-type pesticides by heart-cutting 2D-LC-MS |
| Author(s): | Cano-Carrillo I; Martinez-Piernas AB; Gilbert-Lopez B; Molina-Diaz A; Garcia-Reyes JF; |
| Address: | "Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaen, Campus Las Lagunillas, 23071, Jaen, Spain. Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaen, Campus Las Lagunillas, 23071, Jaen, Spain; University Research Institute for Olives Grove and Olive Oil, University of Jaen, Campus Las Lagunillas, 23071, Jaen, Spain. Analytical Chemistry Research Group, Department of Physical and Analytical Chemistry, University of Jaen, Campus Las Lagunillas, 23071, Jaen, Spain; University Research Institute for Olives Grove and Olive Oil, University of Jaen, Campus Las Lagunillas, 23071, Jaen, Spain. Electronic address: jfgreyes@ujaen.es" |
| DOI: | 10.1016/j.talanta.2023.124918 |
| ISSN/ISBN: | 1873-3573 (Electronic) 0039-9140 (Linking) |
| Abstract: | "Liquid chromatography-mass spectrometry (LC-MS) is currently the gold-standard technique for the analysis of non-volatile small organic molecules. However, one-dimensional liquid chromatography (1D-LC) cannot efficiently deal with mixtures of analytes with different physicochemical properties and, thus, specific chromatographic behaviour. As an alternative, this work proposes a two-dimensional liquid chromatography/high-resolution mass spectrometry (2D-LC-HRMS) approach for the simultaneous analysis of compounds with different polarities. It is based on the combination of hydrophilic interaction liquid chromatography (HILIC) in the first dimension ((1)D) and reversed-phase chromatography (RPLC) in the second dimension ((2)D), employing the heart-cutting methodology. The coupling between (1)D and (2)D was performed by a multiple heart-cutting (MHC) interface equipped with an active solvent modulation (ASM) valve. The aim of the study was the development of a 2D-LC methodology able to (i) acquire the (1)D and (2)D content by MS in a single analytical run, avoiding the loss of information caused by the MHC algorithm for filling the sampling loops; (ii) overcome the breakthrough problem caused by solvent incompatibility, modifying the (2)D gradient during the ASM phase for this purpose. To evaluate the 2D-LC approach, pesticide residue analysis was proposed, selecting 20 pesticides covering a wide range of polarities (log K(ow) from -3.2 to 4.3) and including some of the so-called single residue method pesticides because of the difficulty of including them in 1D-LC multi-residue methods with satisfactory chromatographic resolution. The proposed strategy was to transfer in a single cut the void volume from the HILIC separation (consisting of the nonpolar pesticides) to the (2)D for analysis under RPLC conditions. The developed assembly was assessed in a vegetable matrix (tomato) employing a hybrid QuEChERS/QuPPe sample treatment based on acetonitrile and methanol extraction. The proposed setup may be extended for 2D-LC applications where it is essential to acquire the entire content of both dimensions in a single data file just by coupling a selection valve to the MHC interface" |
| Keywords: | Active solvent modulation Breakthrough Heart-cutting Pesticide Selection valve Two-dimensional liquid chromatography; |
| Notes: | "PubMed-not-MEDLINECano-Carrillo, Irene Martinez-Piernas, Ana B Gilbert-Lopez, Bienvenida Molina-Diaz, Antonio Garcia-Reyes, Juan F eng Netherlands 2023/07/17 Talanta. 2024 Jan 1; 266(Pt 1):124918. doi: 10.1016/j.talanta.2023.124918. Epub 2023 Jul 11" |
