Simultaneous Determination of Multiclass Pesticides and Antibiotics in Honey Samples Based on Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

被引:2
作者
Débora Orso
Luana Floriano
Lucila C. Ribeiro
Nelson M. G. Bandeira
Osmar D. Prestes
Renato Zanella
机构
[1] Universidade Federal de Santa Maria,Laboratório de Análise de Resíduos de Pesticidas (LARP), Departamento de Química
来源
Food Analytical Methods | 2016年 / 9卷
关键词
Honey; Pesticides; Antibiotics; UHPLC-MS/MS;
D O I
暂无
中图分类号
学科分类号
摘要
A simple, fast, and efficient method was developed for simultaneous determination of 79 pesticides and 13 antibiotics compounds of different chemical classes of pesticides and antibiotics in honey samples by ultra-high performance liquid chromatography with tandem mass spectrometry (UHPLC-MS/MS). The sample preparation procedure includes homogenization with McIlvaine buffer 0.1 mol L−1 (pH 4), followed by extraction with acetonitrile and cleanup with florisil, using dispersive solid phase extraction (d-SPE). The proposed method was validated with good results, such as linearity (r2 > 0.9901), normality, and independence of the evaluated data, as well as recoveries between 70 and 120 % with relative standard deviation (RSD) <20 % for most of the compounds spiked from 0.1 to 200 μg kg−1. The experimental method limits of detection and quantification were from 0.03 to 1.51 μg kg−1 and from 0.1 to 5 μg kg−1, respectively, for the pesticides. For the antibiotics, the decision limits (0.1 to 2 μg g−1) and the detection capacity (0.12 to 2.81 μg g−1) were below the maximum residue limits (MRLs) established for honey by the Brazilian and European legislation. The method was successfully applied to real samples from different botanical and geographic origins. From them, 44 % presented residues from 0.12 to 10 μg kg−1 of one or more analytes. The proposed method combines the advantages of a quick sample preparation step with the selectivity and sensitivity of the UHPLC-MS/MS and proved to be suitable for routine analyses.
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页码:1638 / 1653
页数:15
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  • [1] Anastassiades M(2003)Fast and easy multiresidue method employing acetonitrile extraction/partitioning and dispersive solid-phase extraction for the determination of pesticide residues in produce J AOAC Int 83 412-431
  • [2] Lehotay SJ(2013)Pesticide residues levels in honey from apiaries located of Northern Poland Food Control 31 196-201
  • [3] Stajnbaher D(2010)A simple hollow fiber renewal liquid membrane extraction method for analysis of sulfonamides in honey samples with determination by liquid chromatography–tandem mass spectrometry J Chromatogr A 1217 6449-6454
  • [4] Schenck FJ(2014)Screening of volatile compounds in honey using a new sampling strategy combining multiple extraction temperatures in a single assay by HS-SPME–GC–MS Food Chem 145 1061-1065
  • [5] Barganska Z(2003)Assessment of pesticide residues in honey samples from Portugal and Spain J Agric Food Chem 51 8132-8138
  • [6] Slebioda M(2006)Solid-phase microextraction and gas chromatography with atomic emission detection for multiresidue determination of pesticide in honey Anal Chim Acta 562 9-15
  • [7] Namiesnik J(2013)Comparative study of the physicochemical and palynological characteristics of honey from Melipona subnitida and Apis mellifera Int J Food Sci Technol 48 1698-1706
  • [8] Bedendo GC(2014)Confirmation of 13 sulfonamides in honey by liquid chromatography-tandem mass spectrometry for monitoring plans: validation according to European Union Decision 2002/657/EC J Chromatogr A 1339 128-136
  • [9] Jardim ICSF(2011)Overcoming matrix effects using the dilution approach in multiresidue methods for fruits and vegetables J Chromatogr A 1218 7634-7639
  • [10] Carasek E(2010)Comparison of several extraction techniques for multiclass analysis of veterinary drugs in eggs using ultra-high pressure liquid chromatography-tandem mass spectrometry Anal Chim Acta 661 150-160