, Volume 81, Issue 5, pp 759–768 | Cite as

Multi-pesticide Residues Determination in Samples of Fruits and Vegetables Using Chemometrics Approach to QuEChERS-dSPE Coupled with Ionic Liquid-Based DLLME and LC–MS/MS

  • Abubakar Lawal
  • Richard Chee Seng Wong
  • Guan Huat Tan
  • Lukman Bola Abdulra’uf
  • Ali Mohamed Ali Alsharif


Pesticides play vital roles in agricultural practices, but the nature and mishandling of the chemicals have led to their accumulation in moist soil, vegetables and fruits. Thus, development of efficient methods for pesticides determination is one of the most important ways to address such challenges. Multivariate response surface methodology optimisation using Placket–Burman and Box–Behnken designs were respectively used for screening and optimisation of significant factors of quick, easy, cheap, effective, rugged and safe (QuEChERS) with dispersive solid-phase extraction (SPE). Consequently, the optimised QuEChERS-dSPE technique coupled with modified ionic liquid-based (IL-based) dispersive liquid–liquid microextraction was used for sample preparation before LC–MS/MS. The developed method was validated (SANTE 11831-2017) for multi-pesticide residues determination in samples of bananas, cabbages, tomatoes, oranges and onions. The precision results were satisfactory in terms of relative standard deviation (≤ 20%) as recommended. The results of accuracy for relative recoveries (82–137%) were satisfactory because 92.5% of results were within the recommended range (70–120%). The matrix effects in all the samples were very weak (less effective) (≤ − 80%). The linearity of the evaluated results was 5–400 µg kg−1 and regression coefficients (R2) were > 0.99. The resulting limits of detection and quantitation were 0.02–0.32 and 0.07–1.06 µg kg−1, respectively, and therefore satisfactory. Certifiably, the estimated measurement uncertainties range (1–16%) was acceptable (≤ 50%). Thus, the developed method could be reliable and suitable for routine determination of multiple pesticide residues in various vegetable and fruit samples.


Chemometrics DOE and RSM QuEChERS-dSPE and DLLME cleanups Ionic liquid-based Pesticide residues Liquid chromatography–mass spectrometry Fruits and vegetables 



The authors acknowledge the Postgraduate Research Project (IPPP) for supporting this research under the Grant no. PG 174-2014B, University of Malaya Kuala Lumpur, Malaysia.

Compliance with Ethical Standards

Conflict of interest

The authors of this research agreed with no conflicts of interest.


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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Abubakar Lawal
    • 1
    • 2
  • Richard Chee Seng Wong
    • 1
  • Guan Huat Tan
    • 1
  • Lukman Bola Abdulra’uf
    • 3
  • Ali Mohamed Ali Alsharif
    • 1
  1. 1.Department of Chemistry, Faculty of ScienceUniversity of MalayaKuala LumpurMalaysia
  2. 2.Department of Pure and Industrial ChemistryUmaru Musa Yar’adua UniversityKatsinaNigeria
  3. 3.Department of Chemistry, College of Pure and Applied SciencesKwara State UniversityMaleteNigeria

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