Swanson S P, Dahlem A M, Rood H D, Côte L M, Buck W B, Yoshizawa T
J Assoc Off Anal Chem. 1986 Jan-Feb;69(1):41-3.
A gas chromatographic method is described for the determination of deoxynivalenol (DON) and its metabolite DOM-1 in milk. Milk samples were extracted with ethyl acetate on a commercially available disposable extraction column, followed by hexane-acetonitrile partitioning. Final purification was accomplished on a reverse phase C-18 cartridge. The trimethylsilyl ether (TMS) derivatives of DON were prepared, chromatographed on an OV-17 column, and quantitated with an electron capture detector. Chromatography of the TMS derivatives of milk extracts was compared to that of the corresponding heptafluorobutyryl derivatives. The limit of detection using TMS derivatives was 1 ng/mL for both toxins with recoveries averaging 82% +/- 9% at 2.5 and 10 ng/mL milk for DON and 85% +/- 6% at 10 ng/mL for DOM-1.
本文描述了一种用于测定牛奶中脱氧雪腐镰刀菌烯醇(DON)及其代谢产物DOM-1的气相色谱法。牛奶样品在市售一次性萃取柱上用乙酸乙酯萃取,然后进行正己烷-乙腈分配。最终净化在反相C-18柱上完成。制备DON的三甲基硅醚(TMS)衍生物,在OV-17柱上进行色谱分析,并用电子捕获检测器进行定量。将牛奶提取物的TMS衍生物色谱图与相应的七氟丁酰衍生物色谱图进行比较。使用TMS衍生物时,两种毒素的检测限均为1 ng/mL,在牛奶中DON浓度为2.5和10 ng/mL时回收率平均为82%±9%,DOM-1在10 ng/mL时回收率为85%±6%。