title: Simultaneous determination of atropine and scopolamine in buckwheat and related products using modified QuEChERS and liquid chromatography tandem mass spectrometry.
abstract: A method was developed for the determination of atropine and scopolamine in buckwheat and related products. A modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) extraction procedure was evaluated. Dispersive solid phase extraction (d-SPE) was studied as clean-up step, using graphitized black carbon (GBC) and primary secondary amine (PSA). The extract was diluted with water (50:50, v/v) prior to chromatographic analysis. The method was validated and recoveries (except chia samples spiked at 10μg/kg) ranged from 75% to 92%. Intra and inter-day precision was lower than or equal to 17%. The limit of quantification of atropine and scopolamine was 0.4 and 2μg/kg, respectively. Eight types of samples (buckwheat, wheat, soy, buckwheat flour, buckwheat noodle, amaranth grain, chia seeds and peeled millet) were analyzed. Target compounds were not found above the detection limits of the method, but three transformation products of scopolamine (norscopine, hydroscopolamine and dihydroxyscopolamine) were putative identified in the tested samples using high resolution mass spectrometry (Exactive-Orbitrap).
authors.affiliation: Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain; Tea Research Institute, Chinese Academy of Agricultural Sciences (TRICAAS), 9 South Meiling Road, 310008 Hangzhou, China.
authors.forename: Hongping
authors.initials: H
authors.lastname: Chen
authors.affiliation: Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
authors.forename: Jesús
authors.initials: J
authors.lastname: Marín-Sáez
authors.affiliation: Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain.
authors.forename: Roberto
authors.initials: R
authors.lastname: Romero-González
authors.affiliation: Department of Chemistry and Physics, Analytical Chemistry Area, University of Almería, Research Centre for Agricultural and Food Biotechnology (BITAL), Agrifood Campus of International Excellence ceiA3, Carretera de Sacramento s/n, E-04120 Almería, Spain. Electronic address: agarrido@ual.es.
authors.forename: Antonia
authors.initials: A
authors.lastname: Garrido Frenich
mesh_terms: D001285:Atropine / Q000032:analysis* / Q000302:isolation & purification; D002853:Chromatography, Liquid / Q000379:methods*; D019612:Fagopyrum / Q000254:growth & development / Q000378:metabolism*; D012601:Scopolamine / Q000032:analysis* / Q000302:isolation & purification; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry
chemical_list: D014867:Water; D001285:Atropine; D012601:Scopolamine
keywords: Atropine; Buckwheat and related food; Liquid chromatography tandem mass spectrometry; Modified QuEChERS; Scopolamine; Transformation products