Optimisation and validation of a specific analytical method for the determination of thiram residues in fruits and vegetables by LC–MS/MS

► Specific analytical methodology is developed for determination of dithiocarbamate fungicide thiram in fruits and vegetables. ► The method is based on LC coupled to tandem MS. ► Thiram degradation along sample treatment is minimised, adding specific reagents and operating at around 5°C. ► The excel...

Ausführliche Beschreibung

Gespeichert in:
Bibliographische Detailangaben
Veröffentlicht in:Food chemistry Jg. 135; H. 1; S. 186 - 192
Hauptverfasser: Peruga, Aranzazu, Grimalt, Susana, López, Francisco J., Sancho, Juan V., Hernández, Félix
Format: Journal Article
Sprache:Englisch
Veröffentlicht: Kidlington Elsevier Ltd 01.11.2012
Elsevier
Schlagworte:
apples
Biological and medical sciences
detection limit
dithiocarbamate fungicides
EDTA (chelating agent)
eggplants
enzyme activity
field experimentation
Food industries
Fruit and vegetable industries
fruits
Fruits and vegetables
Fundamental and applied biological sciences. Psychology
lettuce
Liquid chromatography
mass spectrometry
Residues
strawberries
Tandem mass spectrometry
Thiram
Tandem mass spectrometry
Residues
Liquid chromatography
Fruits and vegetables
Thiram
Validation
Residue
Fruit vegetable
Method
Mass spectrometry
ISSN:0308-8146, 1873-7072
Online-Zugang:Volltext
Tags: Tag hinzufügen
Keine Tags, Fügen Sie den ersten Tag hinzu!
Beschreibung
Zusammenfassung:► Specific analytical methodology is developed for determination of dithiocarbamate fungicide thiram in fruits and vegetables. ► The method is based on LC coupled to tandem MS. ► Thiram degradation along sample treatment is minimised, adding specific reagents and operating at around 5°C. ► The excellent sensitivity and selectivity of the method allows monitoring for compliance of MRLs, with LOQ of 0.01mg/kg. ► The acquisition of several SRM transitions allows the reliable confirmation of thiram in the samples at very low levels. Thiram is a non-systemic dithiocarbamate fungicide, which is easily degraded during sample preparation since it is affected by pH, matrix components and temperature. In this work, specific methodology for thiram analysis in vegetable (eggplant and lettuce) and fruit (strawberry) samples has been developed based on liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS). Minimising thiram degradation during standards storage and sample preparation was carefully studied. The effect of low temperature (about 5°C), addition of a dehydrating agent (Na2SO4 anhydrous), pH regulator (NaHCO3), and enzymatic activity reduction (EDTA) during extraction was evaluated. The optimised procedure was validated for eggplants, lettuces, and strawberries. Satisfactory recoveries, between 80% and 106%, and relative standard deviations below 10% were obtained at 0.1 and 0.01mg/kg fortification levels (n=5). Limits of detection below 0.0012mg/kg were achieved. The validated method has been applied to eggplant and lettuce samples collected from different field trials as well as several strawberry and apple samples.
Bibliographie:ObjectType-Article-1
SourceType-Scholarly Journals-1
ObjectType-Feature-2
content type line 23
ISSN:0308-8146
1873-7072
DOI:10.1016/j.foodchem.2012.04.064