Within-laboratory validation of a multiresidue method for the analysis of 98 pesticides in mango by liquid chromatography-tandem mass spectrometry. 2012

N Fleury Filho, and C A Nascimento, and E O Faria, and A R Cruvinel, and J M Oliveira
Residues and Contaminants Laboratory - LANAGRO-GO, Ministry of Agriculture, Livestock and Food Supply, Goiânia, Goiás, CEP 74674-025, Brazil. nelio.fleury@agricultura.gov.br

A within-laboratory validation procedure for a selective and sensitive method for the simultaneous determination of 98 pesticide residues in mango is presented. QuEChERS extraction was adapted to laboratory conditions. Mango samples (10 g) mixed with sodium sulfate (4 g) and sodium acetate (1 g) were extracted with acetonitrile/acetic acid (99/1 v/v), cleaned using dispersive solids, and subsequently identified and quantified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Pesticides were separated on a reversed-phase column using a gradient elution in conjunction with positive-mode electrospray ionisation. The analytical performance of the method was demonstrated by analysis of spiked mango samples at three concentration levels (0.01, 0.05 and 0.1 mg kg(-1)) for 3 different days, and the analysis was performed by three analysts. Calibration curves were statistically acceptable by the ordinary last-square method (OLSM), with a regression coefficient above 0.98 for all analytes. The method accuracy (n = 18) was between 80% and 110%, and precisions were below 20% for 95% of the analytes. The method uncertainty at the LOQ was evaluated considering the uncertainty associated with the calibration curve and the uncertainty associated with the method precision. The validation data for all pesticides were in accordance with Brazilian and European guidelines for pesticide residue analysis.

UI MeSH Term Description Entries
D010573 Pesticide Residues Pesticides or their breakdown products remaining in the environment following their normal use or accidental contamination. Pesticide Residue,Residue, Pesticide,Residues, Pesticide
D001938 Brazil A country located on the eastern coast of South America, located between Colombia and Peru, that borders the Atlantic Ocean. It is bordered on the north by Venezuela, Guyana, Suriname, and French Guiana, on the south by Uruguay, and on the west by Argentina. The capital is Brasilia.
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D005504 Food Analysis Measurement and evaluation of the components of substances to be taken as FOOD. Analysis, Food,Analyses, Food,Food Analyses
D005506 Food Contamination The presence in food of harmful, unpalatable, or otherwise objectionable foreign substances, e.g. chemicals, microorganisms or diluents, before, during, or after processing or storage. Food Adulteration,Adulteration, Food,Adulterations, Food,Contamination, Food,Contaminations, Food,Food Adulterations,Food Contaminations
D053719 Tandem Mass Spectrometry A mass spectrometry technique using two (MS/MS) or more mass analyzers. With two in tandem, the precursor ions are mass-selected by a first mass analyzer, and focused into a collision region where they are then fragmented into product ions which are then characterized by a second mass analyzer. A variety of techniques are used to separate the compounds, ionize them, and introduce them to the first mass analyzer. For example, for in GC-MS/MS, GAS CHROMATOGRAPHY-MASS SPECTROMETRY is involved in separating relatively small compounds by GAS CHROMATOGRAPHY prior to injecting them into an ionization chamber for the mass selection. Mass Spectrometry-Mass Spectrometry,Mass Spectrometry Mass Spectrometry,Mass Spectrometry, Tandem
D057230 Limit of Detection Concentration or quantity that is derived from the smallest measure that can be detected with reasonable certainty for a given analytical procedure. Limits of Detection,Detection Limit,Detection Limits
D021241 Spectrometry, Mass, Electrospray Ionization A mass spectrometry technique used for analysis of nonvolatile compounds such as proteins and macromolecules. The technique involves preparing electrically charged droplets from analyte molecules dissolved in solvent. The electrically charged droplets enter a vacuum chamber where the solvent is evaporated. Evaporation of solvent reduces the droplet size, thereby increasing the coulombic repulsion within the droplet. As the charged droplets get smaller, the excess charge within them causes them to disintegrate and release analyte molecules. The volatilized analyte molecules are then analyzed by mass spectrometry. ESI Mass Spectrometry,Electrospray Ionization Mass Spectrometry,Mass Spectrometry, ESI,Spectrometry, ESI Mass
D031022 Mangifera A plant genus of the family ANACARDIACEAE best known for the edible fruit. Mango,Mangifera indica,Mangifera indicas,Mangiferas,Mangos,indicas, Mangifera

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