Capillary gas chromatographic determination of T-2 toxin, HT-2 toxin, and diacetoxyscirpenol in cereal grains.

A capillary gas chromatographic (GC) method using an electron capture detector is described for determining T-2 and HT-2 toxins and diacetoxyscirpenol (DAS) in cereal grains at levels as low as 100 ppb for T-2 and DAS and 50 ppb for HT-2. Samples are extracted with methanol-water according to the Scott method, and further purified on a silica gel cartridge and a cyano column. Heptafluorobutyrylimidazole (HFBI) is added to form the esters of the analytes. Ester(s) of T-2, HT-2 and DAS are separated on a 30 m X 0.32 mm DB-5 fused silica column and measured with a 63Ni electron capture detector. Samples were confirmed by gas chromatography/mass spectrometry using electron impact ionization and single ion monitoring at the molecular mass of 501.11 m/z for T-2, 665.08 m/z for HT-2, and 502.12 m/z for DAS at 10 000 resolving power. The method was applied to wheat, oats, and barley. Average recoveries ranged from a low of 65% for T-2 in barley to a high of 99% for DAS in oats.