TY - JOUR

T1 - Development and Validation of an Analytical Methodology To Determine Deltamethrin Residues and Its Metabolites in Pine Products Using GC-QTOF-MS

AU - Jano, Ana

AU - Fuente-Ballesteros, Adrián

AU - Bernal, José

AU - Ares, Ana M.

AU - Valverde, Silvia

N1 - Publisher Copyright: © 2025 American Chemical Society.

PY - 2025/4/21

Y1 - 2025/4/21

N2 - A new analytical methodology has been proposed to determine deltamethrin and two of its main metabolites (3-phenoxybenzoic acid and 3-(2,2-dibromoethenyl)-2,2-dimethylcyclopropanecarboxylic acid) in pine needle and pine nut samples, using gas chromatography coupled to quadrupole time-of-flight mass spectrometry. Two sample treatments were developed consisting of a solvent extraction for pine needles and a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology for pine nuts, both followed by an additional cleanup step. The eco-friendliness and practicality of the methods were assessed using modified green analytical procedure index and blue applicability grade index, respectively. The method was validated in terms of selectivity, limits of detection (0.2-26 μg kg-1) and quantification (0.6-79 μg kg-1), linearity, matrix effect (< ±20%), trueness (recoveries 82-102%), and precision (relative standard deviation <9%). An analysis of 20 Spanish samples revealed that no residues were found in any of them.

AB - A new analytical methodology has been proposed to determine deltamethrin and two of its main metabolites (3-phenoxybenzoic acid and 3-(2,2-dibromoethenyl)-2,2-dimethylcyclopropanecarboxylic acid) in pine needle and pine nut samples, using gas chromatography coupled to quadrupole time-of-flight mass spectrometry. Two sample treatments were developed consisting of a solvent extraction for pine needles and a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) methodology for pine nuts, both followed by an additional cleanup step. The eco-friendliness and practicality of the methods were assessed using modified green analytical procedure index and blue applicability grade index, respectively. The method was validated in terms of selectivity, limits of detection (0.2-26 μg kg-1) and quantification (0.6-79 μg kg-1), linearity, matrix effect (< ±20%), trueness (recoveries 82-102%), and precision (relative standard deviation <9%). An analysis of 20 Spanish samples revealed that no residues were found in any of them.

KW - deltamethrin

KW - GC-QTOF-MS

KW - metabolites

KW - method validation

KW - pine needle

KW - pine nut

KW - sample treatment

KW - Chemistry

UR - https://www.scopus.com/pages/publications/105003022429

U2 - 10.1021/acsagscitech.5c00044

DO - 10.1021/acsagscitech.5c00044

M3 - Journal articles

AN - SCOPUS:105003022429

VL - 5

SP - 656

EP - 666

JO - ACS Agricultural Science and Technology

JF - ACS Agricultural Science and Technology

SN - 2692-1952

IS - 4

ER -