Analytical and Bioanalytical Chemistry

, Volume 407, Issue 21, pp 6317–6326 | Cite as

Liquid chromatography Orbitrap mass spectrometry with simultaneous full scan and tandem MS/MS for highly selective pesticide residue analysis

  • María del Mar Gómez-Ramos
  • Łukasz Rajski
  • Horacio Heinzen
  • Amadeo R. Fernández-AlbaEmail author
Paper in Forefront
Part of the following topical collections:
  1. High-Resolution Mass Spectrometry in Food and Environmental Analysis


This paper describes the application of LC/Q-Orbitrap MS for the analysis of pesticide residues in fruit and vegetable commodities. LC/Q-Orbitrap MS working in full scan simultaneously with a single MS/MS scan was used to analyse 139 pesticide residues in QuEChERS extracts of tomato, pepper, orange and green tea. Full scan data were obtained at a resolution of 70,000 whereas MS/MS data were obtained at a resolution of 17,500. Quantitation and detection was carried out using full scan data while MS/MS data were used only for identification. MS/MS scans did not have a negative influence on quantitation under the applied conditions. Some peak area reproducibility problems were the consequence of the low sensitivity for some compounds (aldicarb, chlorpyriphos methyl, fenitrothion and fipronil) under the applied conditions. The relation between the operational parameters (viz. automatic gain control (AGC) target, maximum injection time (IT), underfill ratio, isolation window and apex trigger) and the number of automatically identified compounds was investigated. Mass error and minimal intensity of selected fragment ions were also studied. Various working modes were compared, such as full scan with single MS/MS scan and full scan with multiple MS/MS scans. In both cases, the number of automatically reported pesticides was the same. However full scan with single MS/MS scan ensured more points per peak in full scan mode and better peak area reproducibility. The evaluation of the identification and quantitation capabilities of the instrument was performed through the analysis of 100 real samples. The samples were also analysed by LC–QqQ MS/MS and the results of both analytical systems were compared. The comparison revealed that the two instruments were consistent with each other. They found the same pesticides and neither false positive nor false negatives were reported. Nevertheless the Q-Orbitrap MS allowed one to work in high resolution mass spectrometry, increasing the selectivity and, in full scan mode, permitting the retrospective analysis of the data feature that cannot be achieved with QqQ.


Mass spectrometry Pesticides Orbitrap Q-Orbitrap 



The authors acknowledge funding support from The European Commission, DG SANCO (Specific Agreement No. 2007/1 to Framework Partnership Agreement No. SANCO/2007/FOOD SAFETY/025-Pesticides in Fruit and vegetables). The authors also would like to thank Michal Godula from Thermo Fisher Scientific for providing LC/Q-Orbitrap MS and constant support of the work.

Supplementary material

216_2015_8709_MOESM1_ESM.pdf (176 kb)
ESM 1 (PDF 176 kb)


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Copyright information

© Springer-Verlag Berlin Heidelberg 2015

Authors and Affiliations

  • María del Mar Gómez-Ramos
    • 1
  • Łukasz Rajski
    • 1
  • Horacio Heinzen
    • 2
  • Amadeo R. Fernández-Alba
    • 1
    Email author
  1. 1.European Union Reference Laboratory for Pesticide Residues in Fruit & Vegetables, Agrifood Campus of International Excellence (ceiA3) Department of Hydrogeology and Analytical ChemistryUniversity of AlmeriaAlmeríaSpain
  2. 2.Pharmacognosy & Natural ProductsFacultad de Quimica UdelaRMontevideoUruguay

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