Josephs R D, Krska R, Grasserbauer M, Broekaert J A
Center for Analytical Chemistry, Institute for Agrobiotechnology (IFA-Tulln), Austria.
J Chromatogr A. 1998 Feb 6;795(2):297-304. doi: 10.1016/s0021-9673(97)00944-8.
The extraction behaviour of the Fusarium mycotoxin deoxynivalenol (DON) and some related type B trichothecenes from spiked seasand, spiked wheat flour and naturally contaminated wheat flour with modified supercritical CO2 has been investigated and optimized under several conditions. The extraction fluid was decompressed over a solid-phase trap and the amount of deposited analytes was determined by HPLC-diode array detection (DAD) or GC-electron capture detection (ECD) without any further clean-up. Recovery rates as high as 90.1 +/- 10.7% were achieved for spiked wheat samples and 53.0 +/- 3.2% for naturally contaminated samples. The performance of the optimized supercritical fluid extraction (SFE) method was compared with an already well established analytical method employing extraction on a rotary shaker in combination with Mycosep clean-up. Moreover, the SFE procedure developed for naturally DON contaminated wheat was employed for the simultaneous extraction of 5 type B trichothecenes by GC-ECD. This work represents the first successful approach in obtaining an SFE-method for the extraction of Fusarium mycotoxins from wheat with reasonable recoveries and good precision.
研究并优化了在几种条件下,利用改性超临界二氧化碳从加标海沙、加标小麦粉以及天然污染小麦粉中提取镰刀菌霉菌毒素脱氧雪腐镰刀菌烯醇(呕吐毒素,DON)和一些相关的B型单端孢霉烯族毒素的行为。提取液在固相捕集阱上减压,沉积的分析物量通过高效液相色谱-二极管阵列检测(HPLC-DAD)或气相色谱-电子捕获检测(GC-ECD)测定,无需进一步净化。加标小麦样品的回收率高达90.1±10.7%,天然污染样品的回收率为53.0±3.2%。将优化后的超临界流体萃取(SFE)方法的性能与一种已成熟的分析方法进行了比较,后者采用旋转振荡器萃取并结合Mycosep净化。此外,为天然呕吐毒素污染小麦开发的SFE程序用于通过GC-ECD同时萃取5种B型单端孢霉烯族毒素。这项工作代表了首次成功获得一种从小麦中提取镰刀菌霉菌毒素的SFE方法,该方法具有合理的回收率和良好的精密度。