Fipronil in breakfast eggs?
Fipronil in breakfast eggs:
detected with UHPLC-MS/MS
Analysis was performed using a Nexera X2 UHPLC system coupled with
LCMS-8060 triple quadrupole mass spectrometer as shown in Figure 2.
4/2017 eFOOD-Lab international 11
Determination of pesticides in eggs, honey & co using UHPLC-MS/MS
Authors: Uwe Oppermann, Market Manager Food, Shimadzu Europa GmbH,
Anja Grüning, CIPS, Shimadzu Europa GmbH, Telefon: 0203/7687-0,
E-Mail: email@example.com, Website: www.shimadzu.eu
The use of pesticides in the food chain is frequently in the
public eye through media coverage of food scandals.
In August, Fipronil (a broad spectrum insecticide) was
found in eggs from the Netherlands and Germany. Millions of
eggs were destroyed as a result. However, many were already
on sale or being further processed. By now, eggs contaminated
with Fipronil have spread far beyond the borders of Europe.
What is Fipronil?
Figure 1: Fipronil structural formula
Fipronil is a broad-spectrum insecticide used in the control of pests
such as ants, fleas, lice, ticks, cockroaches and mites. Use on foodproducing
animals (livestock) is not permitted. The World Health
Organization (WHO) classifies Fipronil as a toxic substance which
can damage the liver and kidneys after consumption of contaminated
food. The Federal Institute for Risk Assessment (BfR) in
Berlin, Germany, recorded analysis results from Fipronil polluted
eggs in a concentration range of 0.0031 to 1.2 mg per kg, posing a
health risk to children 1.
In order to protect consumers permanently from pesticide-contaminated
food products as well as from non-intentionally added
substances (NIAS) such as heavy metals or mineral oil hydrocarbons,
regular food controls must be carried out. Only a fast and
reliable analysis ensures early detection of exceeded maximum
allowable concentrations, avoiding health risks to consumers and
animals. Shimadzu has developed a high-sensitivity method to
determine Fipronil and its metabolites in foods such as eggs and
Figure 2: UHPLC-MS/MS system
Compound extraction was performed using a simple QuEChERS (Quick,
Easy, Cheap, Effective, Rugged and Safe) method. 5 g of egg (egg white and
eggyolk) were weighted into a 50 mL polypropylene tube, diluted with 5
mL of water and spiked with a respective amount of Fipronil, Fipronilsulfone
and inaddition Fipronil-desulfinyl and Fipronil-sulfide (neochema, Germany).
10 mL of acetonitrile was added and the samples were mixed vigorously.
After that ready to use QuEChERS extraction salts (Q-sepTM Q110, Pouch
and tubes – cat. #26235, Restek) were added for sample drying and buffering.
Samples were mixed again and centrifuged at 4500 rpm for 5 minutes.
1 mL of the supernatant was transferred into a dSPEtube (Q-sepTMQuEChERS
dSPE – cat. #26217, Restek), shaken for 2 minutes, centrifuged, the
supernatant was transferred into a glass vial and the pH was adjusted with
5 % formic acid solution in acetonitrile (10 μL/mL supernatant).
Dangers for bee colonies
Insecticides such as Fipronil and the neonicotinoids thiamethoxam,
clothianidin and imidacloprid which are applied to protect crops, canola,
soybeans, fruit and vegetables on agricultural land, affect the central
nervous system of insects leading to paralysis and ultimately to death.