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

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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.
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Keywords: LC/MS; chromatography – LC/MS; fruit; in-house validation; method validation; pesticide residues; residues; vegetables

Document Type: Research Article

Affiliations: Residues and Contaminants Laboratory – LANAGRO-GO,Ministry of Agriculture, Livestock and Food Supply, Goiânia,Goiás, CEP 74674-025, Brazil

Publication date: April 1, 2012

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