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Goscinny S.,Scientific Institute of Public Health | Unterluggauer H.,Austrian Agency for Health and Food Safety AGES GmbH | Aldrian J.,Austrian Agency for Health and Food Safety AGES GmbH | Hanot V.,Scientific Institute of Public Health | Masselter S.,Austrian Agency for Health and Food Safety AGES GmbH
Food Analytical Methods | Year: 2012

A straightforward analytical method has been developed for the determination of glyphosate and aminomethylphosphonic acid (AMPA), its major metabolite in cereals. This method entails a rapid extraction and derivatization with 9-fluorenylmethyl chloroformate followed by separation with a conventional reversed-phase rapid chromatography used in daily routine analysis and detection by electrospray ionization tandem mass spectrometry. To overcome matrix effects and compensate for any analyte losses during sample treatment, an isotopic dilution approach was used. Since 2010, the monitoring of cereals for the widely used herbicide glyphosate is obligatory to all European Union (EU)-member states, laid down in Commission Regulation (EC) No. 1213/2008. Hence, there is definitively a need for a reliable and easy-to-handle analytical method for monitoring of this compound. The proposed method can be run without having to make time-consuming changes on the equipment used for daily routine analysis. The analytical performance of the method was evaluated according to SANCO/10684/2009 criteria and demonstrated that this method is rugged and cost-effective, therefore suitable for monitoring purposes as well as legislative enforcements within the EU. The apparent recoveries of both analytes were between 97% and 113% with relative standard deviations less than 20%. The limits of quantification of glyphosate and AMPA were 0. 02 mg/kg in cereal matrices. Finally, the accuracy of the method was assessed by analyzing a proficiency test material which was available from a previous round (EUPT-C4). © 2012 Springer Science+Business Media, LLC. Source


Ferrer Amate C.,University of Almeria | Unterluggauer H.,Austrian Agency for Health and Food Safety AGES GmbH | Fischer R.J.,Austrian Agency for Health and Food Safety AGES GmbH | Fernandez-Alba A.R.,University of Almeria | Masselter S.,Austrian Agency for Health and Food Safety AGES GmbH
Analytical and Bioanalytical Chemistry | Year: 2010

Based on several alerts from European countries over the last years concerning spices, we have been encouraged to establish an accurate method for the determination of dyes, aflatoxins and pesticides in various types of spices using reversed-phase (RP) liquid chromatography-tandem mass spectrometry interfaced with electrospray (LC-ESI-MS/MS). A simple sample treatment procedure entailing the use of an extraction step with acetonitrile without further cleanup has been developed. A C18 column with an aqueous ammonium formate/methanol mixture as the mobile phase was used, and gradient elution was performed. Mass spectral acquisition was done in positive ion mode by applying multiple reaction monitoring of at least two fragmentation transitions per compound to provide a high degree of selectivity. The method was in-house validated in terms of linearity, sensitivity, repeatability, recovery and selectivity on six kinds of spices. Satisfactory results in the majority of the cases were obtained for all analytes and matrices, with practical limits of quantitation acceptable for routine monitoring purposes. Extraction recoveries for most of the compounds ranged from 60% to 140% at spiking levels of 0.05 and 0.5 mg kg-1. The applicability of the method for the simultaneous determination of dyes, aflatoxins and pesticides in several types of spices was demonstrated, and the method successfully applied to a limited number of products from the local market. © 2010 Springer-Verlag. Source


Lichtmannegger K.,Austrian Agency for Health and Food Safety AGES GmbH | Fischer R.,Austrian Agency for Health and Food Safety AGES GmbH | Steemann F.X.,Austrian Agency for Health and Food Safety AGES GmbH | Unterluggauer H.,Austrian Agency for Health and Food Safety AGES GmbH | Masselter S.,Austrian Agency for Health and Food Safety AGES GmbH
Analytical and Bioanalytical Chemistry | Year: 2015

The approach for pesticide residue analysis in food of animal origin differs strongly from the one established for food of plant origin, as laboratories mainly focus on conventional methods for the analysis of non-polar pesticides known to accumulate in fatty tissues. However, these group-specific methods are very laborious and cost intensive and typically require extraction of fat components followed by extensive clean-up steps to remove matrix constituents. This work highlights the development and validation of a straightforward QuEChERS-derived clean-up procedure enabling facile, precise, and reliable identification and quantitation of pesticide residues in food of animal origin, which can be extended to various other commodities with moderate fat content and applied to replace traditional group-specific methods. Two additional methods for lean and highly fatty commodities complete this well-established “simplified modular system”. The proposed method was in-house validated in terms of accuracy and precision, recovery and linearity as well as specificity and sensitivity on two representative commodities for food of animal origin (egg and meat). For the majority of the more than 80 pesticides investigated, satisfactory results were obtained. Procedural matrix calibration was applied for screening purposes in conjunction with GC-MS/MS or LC-MS/MS as integral part of the approach. Apparent recoveries for most of the compounds ranged from 70 to 120 % (RSD < 20 %) at spiking levels of 0.01 (LOQ level) and 0.05 mg/kg. Accuracy of the method has been demonstrated by application to reference material from previous EU proficiency tests. Only in case of positive screening results a standard addition approach was applied for precise quantitation. © 2015 Springer-Verlag Berlin Heidelberg Source

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