Xu Jiao-Jiao, Zhou Jian, Huang Bai-Fen, Cai Zeng-Xuan, Xu Xiao-Min, Ren Yi-Ping
Lab of Physicochemical Research, Department of Physicochemical & Toxicology, Zhejiang Provincial Centre for Disease Control and Prevention, Zhejiang, China.
College of Chemical Engineering, Zhejiang University of Technology, Zhejiang, China.
J Sep Sci. 2016 Jun;39(11):2028-35. doi: 10.1002/jssc.201501316.
A simple and reliable method of ultra high performance liquid chromatography coupled with photo-diode array detection has been proposed for the simultaneous determination of deoxynivalenol and its acetylated derivatives in wheat flour and rice, especially focusing on the optimization of sample extraction, cleanup, and chromatographic separation conditions. Sample pretreatment consisted of a first step using a quick, easy, cheap, effective, rugged, and safe based extraction procedure and a subsequent cleanup step based on solid-phase extraction. The method was extensively validated in wheat flour and rice, obtaining satisfactory analytical performance with good linearity (R(2) ≥ 0.999), acceptable recoveries (80.0-104.4%), and repeatability (RSDs 1.3-10.7%). The limits of detection (21.7-57.4 μg/kg) and quantitation (72.3-191.4 μg/kg) for deoxynivalenols were lower than those usually permitted by various countries' legislation in these food matrices. The method was applied to 34 wheat and rice samples. The results were further compared with results of ultra high performance liquid chromatography with electrospray ionization tandem mass spectrometry.
提出了一种简单可靠的超高效液相色谱-光电二极管阵列检测法，用于同时测定小麦粉和大米中的脱氧雪腐镰刀菌烯醇及其乙酰化衍生物，尤其着重于样品提取、净化及色谱分离条件的优化。样品预处理包括第一步采用基于快速、简便、廉价、高效、耐用且安全的提取程序，以及后续基于固相萃取的净化步骤。该方法在小麦粉和大米中得到了广泛验证，获得了令人满意的分析性能，具有良好的线性（R(2)≥0.999）、可接受的回收率（80.0 - 104.4%）和重复性（相对标准偏差1.3 - 10.7%）。脱氧雪腐镰刀菌烯醇的检测限（21.7 - 57.4 μg/kg）和定量限（72.3 - 191.4 μg/kg）低于各国针对这些食品基质通常规定的限值。该方法应用于34个小麦和大米样品。结果进一步与超高效液相色谱-电喷雾电离串联质谱法的结果进行了比较。
