4.6 Article

Simultaneous determination of oxathiapiprolin and two metabolites in fruits, vegetables and cereal using a modified quick, easy, cheap, effective, rugged, and safe method and liquid chromatography coupled to tandem mass spectrometry

Journal

JOURNAL OF CHROMATOGRAPHY A
Volume 1329, Issue -, Pages 30-37

Publisher

ELSEVIER
DOI: 10.1016/j.chroma.2013.12.087

Keywords

Oxathiapiprolin; Metabolites; Residue; Modified QuEChERS; UPLC-MS/MS

Funding

  1. Nature Science Foundation of China (NSFC) [31171879, 31000863]
  2. Public service sector R D Project [201203098]

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An effective and rapid analytical method for the simultaneous determination of a new fungicide oxathiapiprolin and its metabolites (IN-E8S72 and IN-WR791) residues in fruits (grape, watermelon, watermelon peel), vegetables (cucumber, tomato, potato) and cereal (wheat) was developed by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) using the modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction concept. Three target compounds were extracted from all matrices with 1% (V/V) formic acid aqueous solution and acetonitrile then cleaned by dispersive solid phase extraction (dSPE) with octadecylsilane (C-18) and graphitized carbon black (GCB). The determination of the target compounds was achieved within a 5.1 min run time by using an UPLC HSS T3 column connected to an electrospray ionization source (ESI, positive ion mode) for oxathiapiprolin and the negative mode for the two metabolites. The method showed excellent linearity (R-2 > 0.9904) for target compounds. The limit of detection (LOD) for the three compounds ranged from 0.5 mu g kg(-1) to 7.5 mu g kg(-1) and the limits of quantitation (LOQ) were 1 mu g kg(-1) and 10 mu g kg(-1) for oxathiapiprolin and the metabolites, respectively. The mean recoveries from seven matrices ranged from 81.5 to 110.7%, with intra-day relative standard deviations (RSDr) in the range of 0.8-12.0% for all three test compounds. The inter-day RSDR were less than 14.5% for all of the recovery tests. The method was successfully applied for simultaneous analysis of oxathiapiprolin and its metabolites in actual trial samples, indicating its effectiveness in investigating oxathiapiprolin and its metabolites in the food. (C) 2014 Elsevier B.V. All rights reserved.

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