Validation of the Method for Determination
of Pesticide Residues by Gas Chromatography –
Triple-Stage Quadrupole Mass Spectrometry
Laszlo Hollosi, Katerina Bousova, Michal Godula
Thermo Fisher Scientific, Food Safety Response Center, Dreieich, Germany
Method 63899
Key Words
TraceFinder, TSQ, Chromatography, GC, GC-MS, Pesticide Residues,
QuEChERS, Triple Quadrupole
2. Introduction
Pesticide residue analysis in food is one of the most
important and challenging tasks in routine laboratory
practice. The European legislation, which is currently the
most strict legislation (European Regulation 396/2005
and Commission Directive 2006/125/EC), sets maximum
residue limits (MRL) of pesticides in different products
of plant and animal origin. This presents a significant
analytical challenge with respect to the low limits of
quantification (LOQ) required for some specified food
matrices. A variety of GC and HPLC methods have been
developed for multi-residue determination of pesticides
employing a variety of sample preparation and cleanup
techniques. In recent years the QuEChERS method has
become widely adopted for preparing samples of fruit
and vegetables, but the continuous need for more
sensitive and accurate measurements requires new
developments from the instrument producers as well.
Homogenization
Sample + IS
1. Weigh 10 g sample in 50 mL extraction tube
Extraction
GC-MS/MS
2. Add 9.8 mL acetonitrile (20 mL water + 10 mL
acetonitrile for wheat flour) and 200 μL stock IS
3. Shake for 10 min, centrifuge at 5000 rpm for 5 min
Clean up
4. Transfer supernatant into a 15 mL clean-up tube
5. Centrifuge samples at 5000 rpm for 5 min
6. Transfer supernatant into a GC vial
7. Add 50 µL sorbitol and 20 µL of injection standard
1. Schematic of Method
