PMID- 28720218 OWN - NLM STAT- MEDLINE DCOM- 20171016 LR - 20191210 IS - 1873-3778 (Electronic) IS - 0021-9673 (Linking) VI - 1512 DP - 2017 Aug 25 TI - Pesticide analysis in coffee leaves using a quick, easy, cheap, effective, rugged and safe approach and liquid chromatography tandem mass spectrometry: Optimization of the clean-up step. PG - 98-106 LID - S0021-9673(17)31016-6 [pii] LID - 10.1016/j.chroma.2017.07.033 [doi] AB - An analytical method using a quick, easy, cheap, effective, rugged and safe (QuEChERS) procedure for multi-residue determination of 52 pesticides in coffee leaf extractshas been developed and validated according to SANTE/11945/2015 guidelines. Different sorbent combinations for dispersive solid phase extraction (d-SPE) clean-up as well as dispersive liquid-liquid microextraction (DLLME) were tested. The relative standard deviations (RSDs) for the recovery of 87-94% of pesticides added to coffee leaf extracts,was 20% for most pesticides when d-SPE was carried out adding Supelclean ENVI-Carb 120/400. To explain this fact,the secondary metabolic profile was analyzed in all the extraction and clean-up procedures. Only in the clean-up procedure with the addition of Supel QuE Z-Sep+, does caffeine show a constant adsorption between blank and spiked samples. In other clean-up procedures, the amount of caffeine was higher in those samples spiked with pesticides. This indicates competition between caffeine and pesticides for adsorption to the sorbent. Addition of Supel QuE Z-Sep+ to the procedure revealed only a 32% matrix effect, whereas using PSA+ C18 the matrix effect was close to 97%. The process efficiency is up to 54% with the addition of Supel QuE Z-Sep+ and just up to 7% for the other clean-up procedures. The method was successfully tested in coffee leaves from different types of cultivars. Pesticides were not detected in organic coffee leaf extracts, but thiametoxan was clearly detected in 50% of coffee leaf extracts harvested from coffee trees grown under traditional conditions as determined by UHPLC-TOFMSLC/QqTOF-MS/MS. CI - Copyright (c) 2017 Elsevier B.V. All rights reserved. FAU - Trevisan, Maria Teresa Salles AU - Trevisan MTS AD - Food and Environmental Safety Research Group, Facultat de Farmacia, Universitat de Valencia, Av. Vicent Andres Estelles, s/n, 46100, Burjassot, Valencia, Spain; Departamento de Quimica Organica e Inorganica, Universidade Federal do Ceara, CP 12200, 60451-970, Fortaleza, Brazil; Division of Preventive Oncology, National Center for Tumor Diseases, Im Neuenheimer Feld 460, Heidelberg, Germany; Cancer Research Center (DKFZ), Im Neuenheimer Feld 581, Heidelberg, Germany. Electronic address: mariattre@hotmail.com. FAU - Owen, Robert Wyn AU - Owen RW AD - Division of Preventive Oncology, National Center for Tumor Diseases, Im Neuenheimer Feld 460, Heidelberg, Germany; Cancer Research Center (DKFZ), Im Neuenheimer Feld 581, Heidelberg, Germany. FAU - Calatayud-Vernich, Pau AU - Calatayud-Vernich P AD - Food and Environmental Safety Research Group, Facultat de Farmacia, Universitat de Valencia, Av. Vicent Andres Estelles, s/n, 46100, Burjassot, Valencia, Spain. FAU - Breuer, Andrea AU - Breuer A AD - Division of Preventive Oncology, National Center for Tumor Diseases, Im Neuenheimer Feld 460, Heidelberg, Germany; Cancer Research Center (DKFZ), Im Neuenheimer Feld 581, Heidelberg, Germany. FAU - Pico, Yolanda AU - Pico Y AD - Food and Environmental Safety Research Group, Facultat de Farmacia, Universitat de Valencia, Av. Vicent Andres Estelles, s/n, 46100, Burjassot, Valencia, Spain. LA - eng PT - Evaluation Study PT - Journal Article DEP - 20170711 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Coffee) RN - 0 (Pesticide Residues) SB - IM MH - Adsorption MH - Chromatography, Liquid/methods MH - Coffea/*chemistry MH - Coffee/*chemistry MH - Food Contamination/*analysis MH - Pesticide Residues/chemistry/*isolation & purification MH - Plant Leaves/*chemistry MH - Solid Phase Extraction/*methods MH - Tandem Mass Spectrometry/methods OTO - NOTNLM OT - Coffee leaves OT - Dispersive solid-phase clean-up OT - Liquid chromatography-mass spectrometry OT - Matrix co-extractives OT - Pesticides OT - QuEChERS EDAT- 2017/07/20 06:00 MHDA- 2017/10/17 06:00 CRDT- 2017/07/20 06:00 PHST- 2017/04/03 00:00 [received] PHST- 2017/06/26 00:00 [revised] PHST- 2017/07/10 00:00 [accepted] PHST- 2017/07/20 06:00 [pubmed] PHST- 2017/10/17 06:00 [medline] PHST- 2017/07/20 06:00 [entrez] AID - S0021-9673(17)31016-6 [pii] AID - 10.1016/j.chroma.2017.07.033 [doi] PST - ppublish SO - J Chromatogr A. 2017 Aug 25;1512:98-106. doi: 10.1016/j.chroma.2017.07.033. Epub 2017 Jul 11.