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Improving the simultaneous target and non-target analysis LC-amenable pesticide residues using high speed Orbitrap mass spectrometry with combined multiple acquisition modes

Łukasz Rajskia, Styliani Petromelidoub, Francisco José Díaz-Galianoa, Carmen Ferrera, Amadeo Rodríguez Fernandez-Albaa 

aEuropean Union Reference Laboratory for Pesticide Residues in Fruits & Vegetables, University of Almeria, Agrifood Campus of International Excellence (ceiA3) Department of Hydrogeology and Analytical Chemistry, Ctra. Sacramento S/N, La Cañada de San Urbano, 04120, Almería, Spain

bLaboratory of Environmental Pollution Control, Department of Chemistry, Aristotle University of Thessaloniki, Thessaloniki, GR–541 24, Greece

Talanta 228 (2021) 122241



The use of high-resolution mass spectrometry (HRMS) for the simultaneous target and non-target analysis of pesticide residues in food control is a subject that has been studied over the last decade. However, proving its efficacy compared to the more established triple quadrupole mass spectrometers (QQQ-MS2) is challenging. Various HRMS platforms have been evaluated, seemingly showing this approach not to be as effective as QQQMS2 for quantitative analysis, especially in routine food testing laboratories. The two main reasons are (i) the lower sensitivity especially in the case of the fragment ions produced and (ii) the lack of familiarity and an understanding of the most appropriate combination of HRMS acquisition modes to use. In fact, the number of different acquisition modes can appear as a puzzle to inexperienced users. This work was therefore focused on obtaining experimental data to gain a better understanding of the extended acquisition capabilities of a new QOrbitrap platform. Experimental data were obtained for 244 pesticides and their degradation products in commodities of varying matrix complexity (tomato, onion, avocado, and orange) using various combinations of acquisition modes. The best results for targeted analysis were obtained with a combination of full scan (FS), allions fragmentation (AIF) and target MS2 (tMS2) modes, and for non-target analysis using full scan (FS) and datadependent MS2 (ddMS2) modes. All these acquisition modes (FS, AIF, tMS2, and ddMS2) could be applied simultaneously with cycle times ≤ 1 s. The tMS2 especially, proved to be a very powerful approach to increase sensitivity for MS2 fragments and identification rates. Overall, the results for the various pesticide-commodity combinations were fully satisfactory in terms of limit of quantitation (LOQ) repeatability and identification when considered against the SANTE EU Guideline criteria. In addition, the screening capabilities were evaluated for a non-target survey with the use of spectral libraries, the presence of non-target compounds was detected, thus proving the efficacy of the proposed approach. Another issue often overlooked is the optimization of use of spectral libraries, but in our experiments the compounds present in these libraries were not blindly sought in the screening analyses. To minimize the potential for false positives detects in our study, the extractability of the compounds present in the libraries, was also taken into account. The extractability of compounds using a QuEChERS acetonitrile procedure was estimated based on the physicochemical properties of target compounds. By removing compounds that will not be extracted, reduces the occurrences of false detects, reducing the time required for data processing and thus improving the efficiency of the overall screening workflow. 


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Last modified 11-03-2021, 12:41:09

Published 11-03-2021, 12:40:52

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