Determination of flonicamid and its metabolites in bell pepper using ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (Orbitrap).
The development and validation of a method to determine flonicamid and its metabolites as TFNA (4-trifluoromethylnicotinic acid), TFNG (N-(4-trifluoromethylnicotinoyl) glycine) and TFNA-AM (4-trifluoromethylnicotinamide) in bell pepper samples by ultra-high-performance liquid chromatography coupled to Orbitrap mass spectrometry (UHPLC-Orbitrap-MS) was performed. A fast and simple extraction procedure with acidified acetonitrile and salts (magnesium sulfate and sodium chloride) was used. The methodology was validated, checking for specificity, recovery, precision, limits of detection (LODs) and limits of quantification (LOQs). The recoveries ranged from 84% to 98%, and precisions were lower than 17%. Finally, LODs ranged from 1 µg kg-1(flonicamid) to 6 µg kg-1(TFNA-AM), while LOQs ranged from 10 µg kg-1(flonicamid) to 30 µg kg-1(TFNA-AM). Bell pepper samples were analysed and concentrations up to 98 µg kg-1(flonicamid) were detected, although the sum of flonicamid and metabolites did not exceed the maximum residue limit (MRL) set by the European Union.
a Research Group 'Analytical Chemistry of Contaminants', Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almeria, Agrifood Campus of International Excellence, ceiA3 , Almeria , Spain.
Rosalía
R
López-Ruiz
a Research Group 'Analytical Chemistry of Contaminants', Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almeria, Agrifood Campus of International Excellence, ceiA3 , Almeria , Spain.
Roberto
R
Romero-González
a Research Group 'Analytical Chemistry of Contaminants', Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almeria, Agrifood Campus of International Excellence, ceiA3 , Almeria , Spain.
José Luis
JL
Martínez Vidal
a Research Group 'Analytical Chemistry of Contaminants', Department of Chemistry and Physics, Research Centre for Agricultural and Food Biotechnology (BITAL) , University of Almeria, Agrifood Campus of International Excellence, ceiA3 , Almeria , Spain.
Antonia
A
Garrido Frenich
D002212:Capsicum / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid; D013058:Mass Spectrometry; D009536:Niacinamide / Q000031:analogs & derivatives* / Q000032:analysis / Q000378:metabolism
D009536:Niacinamide; C524822:flonicamid
Flonicamid; HRMS; Orbitrap; QuEChERS; TFNA; TFNA-AM; TFNG; UHPLC; metabolites