脱氧雪腐镰刀菌烯醇的制备与鉴定  

Preparation and Identification of Deoxynivalenol

作　　者：郭文博[1,2] 韩铮[1] 杨俊花[1] 韩薇[1] 陈慧英[1,2] 孙真真[1,2] 赵志辉[1] 

机构地区：[1]上海市农业科学院农产品质量标准与检测技术研究所,上海201403 [2]上海海洋大学食品学院,上海201306

出　　处：《分析测试学报》2015年第8期928-933,共6页Journal of Instrumental Analysis

基　　金：沪农科攻字(2014)第3-2号项目

摘　　要：将禾谷镰刀菌(Fusarium graminearum)接种至大米培养基28℃培养4周,通过乙腈-水(84∶16)提取培养基。提取物先经自制净化小柱粗净化除去色素、鞣质等杂质后,以甲醇-水(30∶70)为流动相、Pursuit XRs C18(10 mm×250 mm,5μm)制备色谱柱进行分离,分离组分再以甲醇-水(5∶95)为流动相经Semipreparative SB-CN(9.4 mm×250 mm,5μm)制备色谱柱进一步纯化。所得脱氧雪腐镰刀菌烯醇(DON)经液相色谱-串联质谱(LC-MS/MS)定性,在正、负离子模式下,质谱图中母离子分别为m/z 319.1[M+Na]+,297.1[M+H]+,355.2[M+CH3COO]-,341.2[M+HCOO]-,295.1[M-H]-,子离子碎片分别为m/z175,231,235,249,179,233,237,265,证明该化合物为DON;经外标法测得DON纯度为(99.18±0.11)%。本研究建立的DON分离纯化方法简便易行,分离效果及稳定性好,成本低。Fusarium graminearum was inoculated on rice medium and cultivated at 28 ℃ for 4 weeks in the dark. The medium was extracted with acetonitrile -water（84 ： 16）, and then first cleaned up with home-made clean-up cartridges to remove pigment and tannin, followed by two steps of semi-preparative liquid chromatography for further purification. The target compound was separated on a Pursuit XRs C18 （10 mm × 250 mm, 5 μm）column using methanol-water（30 ： 70）as mobile phase, and then purfied with a Semi-preparative SB -CN column（9. 4 mm x250 mm, 5 i^m） using methanol-water（5 ： 95） as mobile phase. The obtained deoxyuni valenol（DON） was qualified by high performance liquid chromatography tandem mass spectrometry（ HPLC -MS/MS） both in positive elec-trospray ionization mode（ ESI ＋）and negative electrospray ionization mode（ ESI-）. The precursor ions of the compound were 319. 1 [ M ＋ Na] ^＋ , 297. 1 [ M ＋ HI ＋ , 355.2 [ M ＋ CH3COO] ^-, 341.2 [ M ＋ HCOO] -, 295.1 [ M - H]^ -, and the major product ions were 175, 231, 235, 249, 179, 233, 237, 265, which indicated that the obtained substance was DON. The purity of the prepared DON was determined to be （99. 18 ± 0. 11 ）% by the external standard method. Based on the above observations, it was easily concluded that the preparation method for DON was simple, efficient, stable and economical.

关 键 词：脱氧雪腐镰刀菌烯醇 禾谷镰刀菌 中压制备液相色谱法 鉴定 

分 类 号：O657.72[理学—分析化学] S852.44[理学—化学]