谷物样品经乙腈-水（84＋16）溶液提取，离心后经自制中性氧化铝-活性炭-二氧化硅固相萃取柱净化，所得净化液经三甲基硅烷咪唑（TMSI）-N，O-双三甲基硅基乙酰胺（BSA）-三甲基氯硅烷（TMCS）（3＋3＋2）试剂衍生后，产物用RTX-5MS毛细管柱分离，用电子捕获检测器测定脱氧雪腐镰刀菌烯醇（DON）与雪腐镰刀菌烯醇（NIV）。D（）N和NIV的质量浓度在0．05～4．0mg·L^-1之间与峰面积呈线性关系，方法的检出限（3S／N）为0．01mg·kg。方法用于小麦粉中D（）N、NIV的测定，DON和NIV的加标回收率分别在92．6％～96．6％和90．9％～94．1％之间，测定值的相对标准偏差（n=5）均小于6％。%The sample of cereals was extracted with a mixture of acetonitrile-HeO (84+16), and the extract obtained was separated by centrifugation and purified by passing through self-made SPE column of neutral alumina- activated carbon-SlOe. The purified deoxynivalenol (IX)N) and nivalenol (NIV) in the solution after filtration were derivatized with a mixture of TMS1 BSA-TMCS (3+3+2), and the derivatized products were used for GC analysis. RTX-5MS capillary column was used for separation and electron-capture detector (ECD) was adopted in determination. Linear relationships between values of peak area and mass concentration of DON and NIV were obtained in the same range of 0.05--4.0 mg · L^-1, with same detection limits of 0. 01 mg· kg ^-1. The proposed method was applied to the analysis of wheat meal, giving values of recovery in the ranges of 92. 6%--96. 6% for DON and 90. 9%--94. 1% for NIV. Values of RSD's (n=5) found were less than 6%.
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