毛细管柱-气相色谱法测定谷物中脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇含量

Determination of Deoxynivalenol and Nivalenol in Cereals by Capillary Column-Gas Chromatography

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)。DON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-1。方法用于小麦粉中DON、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%.