7
12.6 Robustness
A robustness study was performed by varying parameters
like laboratory personnel, extraction and clean-up
batches. Results were compared to the original method
and significant differences were sought based on
ANOVA analysis. None of the parameters which were
varied led to significant differences in measured values,
consequently indicating that the method was robust.
13. Conclusion
Full in-house validation of a complete method intended
for routine pesticide residue measurements was carried
out. The goal of the study was to obtain an objective
and realistic overview of the analytical performance of a
widely used and accepted sample preparation method
combined with state of the art analytical instrumentation.
The method performance parameters indicate that the
performance for the majority of target compounds complies
with current regulatory requirements. Independent,
external quality control materials were additionally
applied to improve confidence in the measurement
results. In some cases method performance parameters
could not be established or measured values fell outside
of the targeted range due to individual properties of
compounds or strong matrix influences on the analytical
results. For those compounds (in the relevant matrix),
individually optimised sample preparation (additional or
special clean-up) and instrumental methods have to be
applied. From a practical point of view (especially for
instable or active compounds) the best performance can
be achieved by replacing the liner (and septum) after
40–50 injections. Overall it can be concluded that the
complete workflow solution offered by Thermo Fisher
Scientific in conjuction with the newly developed TSQ
8000 GC-MS system delivers the required system
performance for the target compounds especially
regarding sensitivity, selectivity and recovery.
14. References
1. European Commission 2002/657/EC
2. European Commission 2006/125/EC
3. European Commission SANCO/12495/2011
4. European Commission 788/2012/EC
5. Fussell et al. (2007)
Food Additives & Contam
,
24:1247-1256
6. Thermo Scientific TSQ 8000 Pesticide Analyzer
Brochure,
/
D22018~.pdf
7. EU Pesticides Database,
_
pesticides/public/index.cfm
8. Anastassiades et al. (2003)
J. Chromatogr A,
1015:163-184
