Comparison of Different d-SPE Sorbent Performances Based on Quick,Easy, Cheap,Effective, Rugged,and Safe (QuEChERS) Methodology for Multiresidue Pesticide Analyses in Rapeseeds |
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Authors: | Saida Belarbi Martin Vivier Wafa Zaghouani Aude De Sloovere Valerie Agasse Pascal Cardinael |
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Institution: | 1.Laboratoire SMS-EA3233, Normandie University, FR3038 INC3M, Unirouen, Place Emile Blondel, F-76821 Mont-Saint-Aignan, France;2.SGS France Laboratoire de Rouen, Technopôle du Madrillet, 65 Avenue Ettore Bugatti, BP 90014, F-76801 Saint Etienne du Rouvray, France; (M.V.); (W.Z.); (A.D.S.) |
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Abstract: | Pesticide extraction in rapeseed samples remains a great analytical challenge due to the complexity of the matrix, which contains proteins, fatty acids, high amounts of triglycerides and cellulosic fibers. An HPLC-MS/MS method was developed for the quantification of 179 pesticides in rapeseeds. The performances of the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method were evaluated using different dispersive solid-phase extraction (d-SPE) sorbents containing common octadecylsilane silica/primary–secondary amine adsorbent (PSA/C18) and new commercialized d-SPE materials dedicated to fatty matrices (Z-Sep, Z-Sep+, and EMR-Lipid). The analytical performances of these different sorbents were compared according to the SANTE/12682/2019 document. The best results were obtained using EMR-Lipid in terms of pesticide average recoveries (103 and 70 of the 179 targeted pesticides exhibited recoveries within 70–120% and 30–70%, respectively, with low RSD values). Moreover, the limits of quantification (LOQ) range from 1.72 µg/kg to 6.39 µg/kg for 173 of the pesticides. Only the recovery for tralkoxydim at 10 μg/kg level was not satisfactory (29%). The matrix effect was evaluated and proved to be limited between −50% and 50% for 169 pesticides with this EMR-Lipid and freezing. GC-Orbitrap analyses confirmed the best efficiency of the EMR-Lipid sorbent for the purification of rapeseeds. |
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Keywords: | multiresidue pesticide analyses rapeseeds QuEChERS extraction dispersive solid-phase extraction HPLC-MS/MS |
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