12 · I ss u es 3 -6 · A p r -J u n 20 07 · w w w. e uros urve ill an c e . o rg O u t b r e a k r e p o r t

A simple, low-cost and sensitive method for the determination of six phthalate acid esters (dimethyl phthalate, diethyl phthalate, dibutyl phthalate, benzyl butyl phthalate, bis(2-ethylhexyl) phthalate and dioctyl phthalate) and one adipate (bis(2-ethylhexyl) adipate) in beer has been developed using head-space solid-phase microextraction (HS-SPME) followed by gas chromatography coupled to mass spectrometry (GC/MS). SPME conditions were optimised, and optimum extraction parameters were found to be 95°C at 100 min, without addition of NaCl. Matrix interference was avoided by using a deuterated internal standard (ISTD). Limits of detection ranged from 0.006 to 0.590 μg/L. The method showed good linearity with coefficients of determination ranging from 0.963 to 0.999 and satisfactory accuracy (74-101 %) and repeatability (3.56-27.86 %) values. The method was applied to 15 samples of beer from Luxembourgish breweries, stored in different containers (can, glass and aluminium bottle), and phthalates were detected in all samples with concentrations as high as 61.56 μg/L for total phthalates. The exact origins of phthalates in beer were difficult to determine from the data in this study, though the brewing and bottling process seems to be a major contributor.

Sudan dyes are red, synthetic azo dyes that are not allowed in foodstuffs in the European Union (Council Directive 94/36/EC). However, subppm levels of Sudan dye in spices are regularly reported, and it is assumed that these appearances are due to cross-contamination. In this paper, we present a newly developed fast and sensitive method for the quantification of Sudan I, II, III, and IV, using liquid-liquid extraction and UPLC-MS/MS analysis, and giving quantification limits ranging from 2.5 to 200 μg/kg. The method was applied to 21 samples, and 17 of them contained Sudan dye at low concentrations (3.3-8 709 μg/kg). Interestingly, it was observed that the distribution of Sudan dye in the sample is not homogeneous, which may lead to false negatives or to overestimations of the concentration, and that the pretreatment (blending or not) of the sample seriously influences the final result of the analysis.

Chronic intake of cereals contaminated with ergot alkaloids can cause ergotism and result in the loss of toes and fingers or even death. Today, due to common risk management practices, ergotism is rare as a human disease but remains a problem in livestock husbandry. Each alkaloid coexists under two forms (R and S), though only the Rform presents toxic effects. The epimerization occurs spontaneously but the mechanisms remain globally unknown. Therefore, different processing methods were evaluated for their respective influences on the epimerization. The results suggest that ergotamine and ergosine are very stable ergot alkaloids, and neither their concentrations, nor their respective R/S ratios, are significantly influenced by heating, protic solvents or UV light. In contrast, for ergocristine, ergokryptine, ergocornine and ergometrine, heating can decrease the concentrations of these alkaloids and heat, protic solvents and UV light influence the R/S ratio towards the S-form, though the respective influence on the epimerization of these compounds is variable. In addition, the total concentration of all ergot alkaloids is reduced through heating. However, all these effects are not strong enough to change the composition of ergot alkaloids in feed substantially and to transform toxic feed into non-toxic feed.

Ergot alkaloids are toxins produced by some species of fungi in the genus Claviceps, that may infect rye and triticale and, in a minor degree, other types of cereals. In this study, a new UHPLC-FLD method for the quantification of the six major ergot alkaloids as well as their corresponding epimers was developed. The sample preparation was done by a solid-liquid extraction with acetonitrile and clean-up via freeze-out. The method was fully validated and then applied to 39 samples (wheat, rye, triticale, and barley) harvested in Luxembourg in 2016. Samples were sieved (1.9 × 20 mm) prior to analysis in order to remove sclerotia, hosting the alkaloids. However, 23 samples still contained at least one ergot alkaloid > LOQ and concentrations of the sum of the 6 ergot alkaloids ranged from 0.3 to 2530.1 μg/kg. Interestingly, the highest concentrations were measured in wheat and not in rye or triticale, suggesting that all kinds of cereals should be included in monitoring programs. The outcome of this study allowed giving a first overview of ergot alkaloid concentrations in cereals harvested in Luxembourg, and the measured concentrations were in similar ranges than in other parts of the world (e.g., Canada, France, Germany).