Page 40 - Volume 3, Issue 2, July 2010

1

Laboratory of Pesticide Residues, Department of

Pesticides Control and Phytopharmacy, Benaki Phy-

topathological Institute, 8 St. Delta Str., GR-145 61 Ki-

fissia (Athens), Greece.

2

Chemistry Laboratory, Department of Science, Agri-

cultural University of Athens, 75 Iera Odos Str., GR-118

55 Athens, Greece

Corresponding author:

c.anagnostopoulos@bpi.gr

Introduction

In recent years, the safety of children’s and

infants diet has received special attention.

Because they are still growing and develop-

ing, their metabolism, as well as other phys-

iological and biochemical processes, dif-

fer from that of adults (11). However, as with

adults, diet can be a significant source of

exposure to pesticides. Trace quantities of

pesticides and their breakdown products

present on or in foodstuffs are termed as

“residues”. Residue levels reflect the amount

of pesticide applied to a crop, the time that

has elapsed since application, and the rate

of pesticide dissipation and evaporation

(11). To ensure the safety of foods specifical-

ly produced for infants (children under the

age of 12 months) and young children (be-

tween 1 and 3 years), the European Commis-

Hellenic Plant Protection Journal

3:

71-80, 2010

Validation of the QuEChERS method for the determination

of 25 priority pesticide residues in cereal-based baby foods

by gas chromatography with electron capture and nitrogen

phosphorous detection

C.J. Anagnostopoulos

1

, P. Aplada Sarli

1

, G.E. Miliadis

1

and C.A. Haroutounian

2

Summary

A multiresidue method for the simultaneous analysis of 25 pesticides and metabolites in-

cluded in Commission Directives 2006/141/EC and 2006/125/EC for baby food was validated in cereal-

based baby foods. The extraction procedure was based on the QuEChERS method and the determina-

tion was performed by gas chromatography combined with electron capture detector (ECD) and nitro-

gen phosphorus detector (NPD). The analytical performance was demonstrated by the analysis of ex-

tracts of spiked samples at two concentration levels, 3 and 30 μg/kg, for each analyte. Good sensitivi-

ty and selectivity of the method were obtained with limits of quantification at 3 μg/kg in all cases. All

pesticides and metabolites, with the exception of omethoate, gave recovery values ranging from 79.2

to 124.6% with relative standard deviations less than 28% at both spiking levels for most analytes.

Additional keywords

:

GC-NPD, GC-ECD, linearity, precision, trueness, validation

sion (EC) has set rules for these categories of

food (6). Regarding pesticides, the EC spec-

ifies a maximum residue level (MRL) of 10

μg/ kg of pesticide residue in baby food and

has banned highly toxic pesticides (ADI ≤0.5

mg/kg body weight) in agricultural produce

intended for processed baby foods. The

MRLs for highly toxic pesticides set by the

EC are even more strict, ranging from 3 to

8 μg/kg (European Union Directive 91/321/

EC and subsequent revisions, 1999/50/EC,

European Union Directive 96/5/EC and sub-

sequent revisions, 1999/39/EC, European

Union Directives 2003/13/EC, 2003/14/EC,

2006/125/EC and 2006/141/EC).

Considering the low concentration levels

that must be detected for successful moni-

toring of pesticide residues in infant foods,

sensitive and reliable confirmation methods

are required.

Many different extraction methods, such

as supercritical fluid extraction (SFE) (8) and

acetone-based extraction (1, 17), have been

used for the extraction of pesticides in cere-

als and flour. Acetonitrile was also adopted

as extraction solvent with various applica-

tions in low water and fat content commod-