An analytical method for the determination of aflatoxin B1 in a tiger nut-based soft drinks named 'horchata' is described. The method is based on an immunoaffinity clean-up, followed by HPLC separation and fluorescence detection after electrochemical post-column derivatization. The detection limit (S/N = 3) and the quantification limit (S/N = 10) were 0.02 and 0.06 microg kg(-1), respectively. The mean recovery at a level of 2 microg l(-1) was 88% (n = 6) and the coefficient of variation was 9%. The method was applied to conduct a small market survey for a beverage named 'horchata' that is frequently consumed by parts of the population in Southern Europe. Twenty-two samples from Spanish and Belgian supermarkets were analysed. As a result, only one sample was found to contain aflatoxin B1 at the limit of quantitation of the method.
An interlaboratory trial for the determination of patulin in apple juice and fruit puree was conducted, involving 17 participants representing a cross section of industry, official food control, and research facilities. Mean recoveries reported ranged from 74 (10 ng/g) to 62% (25 ng/g) for apple juice and from 72 (25 ng/g) to 74% (10 ng/g) for fruit puree. Based on results for spiked samples (blind pairs at 2 levels), as well as naturally contaminated samples (blind pairs at 3 levels), the relative standard deviation for repeatability (RSDr) in juice ranged from 8.0 to 14.3% and in puree from 3.5 to 9.3%. The relative standard deviation for reproducibility (RSDR) in juice ranged from 19.8 to 39.5% and in puree from 12.5 to 35.2%, reflecting HORRAT values from 0.6 to 1.0 for juice and 0.4 to 0.9 for puree. The method showed acceptable within-laboratory and between-laboratory precision for each matrix, as required by current European legislation.
An interlaboratory trial for determination of zearalenone (ZON) in baby food and animal feed was conducted. The study involved 39 participants in 16 European Union member states, as well as Turkey, Uruguay, and China, representing a cross-section of industry, and official food control and research institutes. The method is based on immunoaffinity column cleanup followed by high-performance liquid chromatography using fluorimetry (HPLC-Fl). The test portion of the sample is extracted with methanolwater (75 + 25, v/v). The sample extract is filtered, diluted, and passed over an immunoaffinity column. ZON is eluted with methanol. The separation and determination of ZON is performed by reversed-phase HPLC-Fl with an excitation wavelength of 274 nm and an emission wavelength of 446 nm. Test portions of the samples were spiked at levels of 20 and 30 g/kg ZON in baby food and at levels of 100 and 150 g/kg ZON in animal feed. Mean recoveries from each participant ranged from 78 to 119 with an average value of 92 for baby food and from 51 to 122 with an average value of 74 for animal feed. Based on results for spiked samples (blind duplicates at 2 levels), as well as naturally contaminated samples (blind duplicates at 3 levels), the relative standard deviation for repeatability (RSDr) in baby food ranged from 2.8 to 9.0. For animal feed, this value ranged from 5.7 to 9.5. The relative standard deviation for reproducibility (RSDR) in baby food ranged from 8.2 to 13.3, and for animal feed this value ranged from 15.5 to 21.4. The Horwitz ratio (HorRat) in baby food ranged from 0.3 to 0.4, and for animal feed this value ranged from 0.6 to 0.9. The method showed acceptable within-and between-laboratory precision for each matrix, as required by European legislation.
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