PMID- 26695310 OWN - NLM STAT- MEDLINE DCOM- 20160929 LR - 20231213 IS - 1873-3573 (Electronic) IS - 0039-9140 (Linking) VI - 146 DP - 2016 Jan 1 TI - Analysis of glyphosate and aminomethylphosphonic acid in leaves from Coffea arabica using high performance liquid chromatography with quadrupole mass spectrometry detection. PG - 609-20 LID - S0039-9140(15)30186-7 [pii] LID - 10.1016/j.talanta.2015.07.059 [doi] AB - Glyphosate is a commonly applied herbicide in coffee plantations. Because of its non-selective mode of action it can damage the crop exposed through spray drift. Therefore, it is of interest to study glyphosate fate in coffee plants. The aim of this study was to develop an analytical method for accurate and precise quantification of glyphosate and its main metabolite aminomethylphosphonic acid (AMPA) at trace levels in coffee leaves using liquid chromatography with single-quadrupole mass spectrometry detection. The method is based on a two-step solid phase extraction (SPE) with an intermediate derivatization reaction using 9-fluorenylmethylchloroformate (FMOC). An isotope dilution method was used to account for matrix effects and to enhance the confidence in analyte identification. The limit of quantification (LOQ) for glyphosate and AMPA in coffee leaves was 41 and 111 mug kg(-1) dry weight, respectively. For the method optimization a design of experiments (DOE) approach was used. The sample clean-up procedure can be simplified for the analysis of less challenging matrices, for laboratories having a tandem mass spectrometry detector and for cases in which quantification limits above 0.1 mg kg(-1) are acceptable, which is often the case for glyphosate. The method is robust, possesses high identification confidence, while being suitable for most commercial and academic laboratories. All leaf samples from five coffee fields analyzed (n=21) contained glyphosate, while AMPA was absent. The simplified clean-up procedure was successfully validated for coffee leaves, rice, black beans and river water. CI - Copyright (c) 2015 Elsevier B.V. All rights reserved. FAU - Schrubbers, Lars C AU - Schrubbers LC AD - Department of Plant and Environmental Sciences, Faculty of Science, University of Copenhagen, Frederiksberg C, Denmark. Electronic address: schruebbers@plen.ku.dk. FAU - Masis-Mora, Mario AU - Masis-Mora M AD - Centro de Investigacion en Contaminacion Ambiental, Universidad de Costa Rica, San Jose, Costa Rica. FAU - Rojas, Elizabeth Carazo AU - Rojas EC AD - Centro de Investigacion en Contaminacion Ambiental, Universidad de Costa Rica, San Jose, Costa Rica. FAU - Valverde, Bernal E AU - Valverde BE AD - Department of Plant and Environmental Sciences, Faculty of Science, University of Copenhagen, Frederiksberg C, Denmark; Investigacion y Desarrollo en Agricultura Tropical S.A. (IDEA Tropical), Alajuela, Costa Rica. FAU - Christensen, Jan H AU - Christensen JH AD - Department of Plant and Environmental Sciences, Faculty of Science, University of Copenhagen, Frederiksberg C, Denmark. FAU - Cedergreen, Nina AU - Cedergreen N AD - Department of Plant and Environmental Sciences, Faculty of Science, University of Copenhagen, Frederiksberg C, Denmark. LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20150720 PL - Netherlands TA - Talanta JT - Talanta JID - 2984816R RN - 0 (Isoxazoles) RN - 0 (Organophosphonates) RN - 0 (Tetrazoles) RN - J090588E6X (2-amino-3-(3-hydrox-5(2-methyl-2H-tetrazol-5-yl)isoxazol-4-yl)propionic acid) RN - TE7660XO1C (Glycine) SB - IM MH - Chromatography, High Pressure Liquid/*methods MH - Coffea/*chemistry MH - Environment, Controlled MH - Glycine/*analogs & derivatives/analysis/chemistry/isolation & purification/metabolism MH - Isoxazoles MH - Limit of Detection MH - Mass Spectrometry/*methods MH - Organophosphonates/*analysis/chemistry/isolation & purification/metabolism MH - Plant Leaves/*chemistry MH - Solid Phase Extraction MH - Tetrazoles MH - Glyphosate OTO - NOTNLM OT - Coffea arabica OT - Coffee OT - Glyphosate analysis OT - Liquid chromatography mass spectrometry OT - Single quadrupole EDAT- 2015/12/24 06:00 MHDA- 2016/09/30 06:00 CRDT- 2015/12/24 06:00 PHST- 2015/04/14 00:00 [received] PHST- 2015/07/13 00:00 [revised] PHST- 2015/07/19 00:00 [accepted] PHST- 2015/12/24 06:00 [entrez] PHST- 2015/12/24 06:00 [pubmed] PHST- 2016/09/30 06:00 [medline] AID - S0039-9140(15)30186-7 [pii] AID - 10.1016/j.talanta.2015.07.059 [doi] PST - ppublish SO - Talanta. 2016 Jan 1;146:609-20. doi: 10.1016/j.talanta.2015.07.059. Epub 2015 Jul 20.