Cohen H, Lapointe M
J Assoc Off Anal Chem. 1984 Nov-Dec;67(6):1105-7.
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.
本文描述了一种采用电子捕获检测器的毛细管气相色谱（GC）方法，用于测定谷物中T-2毒素、HT-2毒素和二醋酸雪腐镰刀菌烯醇（DAS），其检测限低至T-2和DAS为100 ppb，HT-2为50 ppb。样品根据斯科特方法用甲醇-水提取，并在硅胶柱和氰基柱上进一步纯化。加入七氟丁酰咪唑（HFBI）以形成分析物的酯。T-2、HT-2和DAS的酯在30 m×0.32 mm的DB-5熔融石英柱上分离，并用63Ni电子捕获检测器进行测定。通过气相色谱/质谱联用仪，采用电子轰击电离和单离子监测，在10000的分辨率下，分别对T-2的501.11 m/z、HT-2的665.08 m/z和DAS的502.12 m/z的分子质量进行确认。该方法应用于小麦、燕麦和大麦。平均回收率范围从大麦中T-2的低至65%到燕麦中DAS的高至99%。
