A new fast and sensitive method based on on-line solid-phase extraction on a fused-core precolumn coupled to liquid chromatography with fluorescence detection has been developed for ochratoxin A (OTA) and citrinin (CIT) determination in lager beer samples. Direct injection of 100 μL filtered beer samples into an on-line SPE-HPLC system enabled fast and effective sample extraction including separation in less than 6 min. Preconcentration of OTA and CIT from beer samples was performed on an Ascentis Express RP C18 guard column (5 × 4.6 mm), particle size 2.7 μm, with a mobile phase of methanol/0.5% aqueous acetic acid pH 2.8 (30:70, v/v) at a flow rate of 2.0 mL min(-1). The flow switch from extraction column to analytical column in back-flush mode was set at 2.0 min and the separation was performed on the fused-core column Ascentis Express Phenyl-Hexyl (100 × 4.6 mm), particle size 2.7 μm, with a mobile phase acetonitrile/0.5% aqueous acetic acid pH 2.8 in a gradient elution at a flow rate of 1.0 mL min(-1) and temperature of 50 °C. Fluorescence excitation/emission detection wavelengths were set at 335/497 nm. The accuracy of the method, defined as the mean recoveries of OTA and CIT from light and dark beer samples, was in the range 98.3-102.1%. The method showed high sensitivity owing to on-line preconcentration; LOQ values were found to be 10 and 20 ng L(-1) for OTA and CIT, respectively. The found values of OTA and CIT in all tested light, dark and wheat beer samples were significantly below the maximum tolerable limits (3.0 μg kg(-1) for OTA and 2000 μg kg(-1) for CIT) set by the European Union.

Sample preparation prior to chromatographic separation plays an important role in the analytical process. To avoid time-consuming and manual handling sample-prep, automated on-line techniques such as on-line SPE-HPLC are therefore preferred. In this study, two different on-line extraction approaches for mycotoxin/endocrine disruptor zearalenone (ZEA) determination using either molecularly imprinted polymer (MIP) with selective cavities and binding sites for extraction or a reversed-phase sorbent C18 providing non-selective interactions have been developed, validated, and compared. The validation characteristics were compared and the two methods were evaluated as being almost equal in terms of linearity, repeatability, precision, and recovery. Recoveries were in the range of 99.0-100.1% and limits of detection were found the same for both methods (1.5 μg L). Method precision calculated for spiked beer samples was better for C18 sorbent (2.5 vs. 5.4% RSD). No significant differences in the selectivity of either extraction method were observed. The possible reasons and further details associated with this finding are discussed. Finally, both validated methods were applied for the determination of ZEA contamination in beer samples. Due to ZEA's native fluorescence, chromatographic separation with fluorimetric detection (λ = 270 nm and λ = 458 nm) was selected. Graphical abstract Determination of zearalenone in beer using an on-line extraction chromatography system.

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Beer is one of the most popular alcoholic beverages worldwide. For consumer acceptance, significant factors are its taste, flavour and colour. This study determines selected synthetic green, blue and yellow food colorants in popular Easter herb-coloured green beers on tap produced in breweries on Holy Thursday. The abuse of beer colouring with Tartrazine (E 102), Quinoline yellow (E 104), Sunset yellow (E 110), Patent blue (E 131), Indigo carmine (E 132), Brilliant blue FCF (E 133), Green S (E 142) and Fast green FCF (E 143) was assessed in 11 green beer samples purchased in local restaurants. HPLC was used for the separation and detection of artificial colorants with diode-array detection and a Chromolith Performance CN 100 × 4.6 mm column with guard pre-column Chromolith CN 5 × 4.6 mm. Separation was performed in gradient elution with mobile phase containing methanol-aqueous 2% ammonium acetate at pH 7.0. The study showed that eight beers (70%) marketed in the Czech Republic contained artificial colorants (Tartrazine and Brilliant blue FCF). The concentration of colorants found in analysed green herb-coloured beers ranged from 1.58 to 3.49 mg l(-)(1) for Tartrazine, 0.45-2.18 mg l(-)(1) for Brilliant blue, while Indigo carmine was detected only once at concentration 2.36 mg l(-)(1). Only three beers showed no addition of the synthetic colorants. However, the levels of artificial colorants found in beers marketed in the Czech region were very low and did not show a serious risk for consumers' health.