Development and Validation of a Multiresidue Method for the Determination of Pesticides in Dry Samples (Rice and Wheat Flour) Using Liquid Chromatography/Triple Quadrupole Tandem Mass Spectrometry
| Autor: | F. J. Arrebola, José Luis Martínez Vidal, Ángel Grande-Martínez, Laura Díaz Moreno, Antonia Garrido Frenich |
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| Rok vydání: | 2015 |
| Předmět: |
Acetonitriles
Flour Wheat flour Food Contamination Acetates Quechers High-performance liquid chromatography Specimen Handling Analytical Chemistry Limit of Detection Tandem Mass Spectrometry Humans Environmental Chemistry Sample preparation Solid phase extraction Triticum Observer Variation Pharmacology Chromatography Pesticide residue Chemistry Solid Phase Extraction Extraction (chemistry) Pesticide Residues Water Oryza Triple quadrupole mass spectrometer Solvents Adsorption Agronomy and Crop Science Food Analysis Chromatography Liquid Food Science |
| Zdroj: | Journal of AOAC INTERNATIONAL. 98:1186-1198 |
| ISSN: | 1944-7922 1060-3271 |
| DOI: | 10.5740/jaoacint.sge4-grande-martinez |
| Popis: | A rapid and sensitive multiresidue method was developed and validated for the determination of around 100 pesticides in dry samples (rice and wheat flour) by ultra-performance LC coupled to a triple quadrupole mass analyzer working in tandem mode (UPLC/QqQ-MS/MS). The sample preparation step was optimized for both matrixes. Pesticides were extracted from rice samples using aqueous ethyl acetate, while aqueous acetonitrile extraction [modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method] was used for wheat flour matrixes. In both cases the extracts were then cleaned up by dispersive solid phase extraction with MgSO4 and primary secondary amine + C18 sorbents. A further cleanup step with Florisil was necessary to remove fat in wheat flour. The method was validated at two conc compounds), obtaining recoveries ranging from 70 to 120%, intraday and interday precision values ≤20% expressed as RSDs, and expanded uncertainty values ≤50%. The LOQ values ranged between 3.6 and 20 μg/kg, although it was set at 3.6 μg/kg for the majority of the pesticides. The method was applied to the analysis of 20 real samples, and no pesticides were detected. |
| Databáze: | OpenAIRE |
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