Validation of an analytical method to determine the content of T-2 and HT-2 toxins in cereals and compound animal feed by immunoaffinity column clean-up and GC-MSFunded under: FP7-JRC
A method for the determination of T-2 toxin and HT-2 toxin in cereals and compound animal feed was validated by collaborative study. In short, the method is as follows: A test portion of a sample is extracted with a mixture of methanol/water (80/20, v/v). This raw extract is then diluted, filtered, and applied to an immunoaffinity column. After washing and elution with acetonitrile the eluate is evaporated to dryness. T-2 and HT-2 toxins in the dry residue are then derivatised with N-methyl-N-trimethylsilyl-trifluoroacetamid (MSTFA)/ trimethylchlorosilane (TMCS) (99/1, v/v), injected into a gas chromatograph, and detected and quantified by mass spectrometry. Fourteen laboratories from ten different countries were selected to participate in the collaborative study. They received six different test materials as blind duplicates. The test materials consisted of a blank cereal mix, two cereal mixes naturally contaminated with T-2 and HT-2 toxins at different levels, a blank compound animal feed, and two compound animal feeds naturally contaminated with T-2 and HT-2 toxins at different levels. Furthermore, two blank cereal mixes and two blank compound animal feeds together with specific spiking solutions were provided for recovery determination. The sum of the mass fractions of T-2 & HT-2 toxins after spiking were 50 mu g/kg in the cereal mix, and 75 mu g/kg in the compound animal feed. Reported apparent recoveries in the cereal mix ranged from 59 to 143% for the sum of T-2 & HT-2 toxins with a mean value of 105%. Reproducibility relative standard deviations (RSDR) for the cereal matrix were 30% at a natural contamination level of ca. 25 mu g/kg, 21% at ca. 87 mu g/kg, and 27% for the spiked material at 50 mu g/kg. For compound animal feed the recovery values ranged from 87 to 145% with 113% for the mean value. The RSDR values were 25% at a natural contamination level of ca. 92 mu g/kg, 19% at ca. 125 mu g/kg, and 16% for the spiked material at 75 mu g/kg.
Bibliographic Reference: EUR 23560 EN (2008), 72 pp. Free of charge
Availability: http://bookshop.europa.eu/is-bin/INTERSHOP.enfinity/WFS/EU-Bookshop-Site/en_GB/-/EUR/ViewPublication-Start?PublicationKey=LANA23560 (Catalogue Number: LA-NA-23560-EN-C)
ISBN: ISBN: 978-92-79-10532-6
Record Number: 200910254 / Last updated on: 2009-07-06
Original language: en
Available languages: en