Tamura Masayoshi, Mochizuki Naoki, Nagatomi Yasushi, Harayama Koichi, Toriba Akira, Hayakawa Kazuichi
Research Laboratories for Food Safety Chemistry, Asahi Group Holdings, Ltd., 1-21, Midori 1-chome, Moriya-shi, Ibaraki 302-0106, Japan.
Graduate School of Medical Sciences, Kanazawa University, Kakuma-machi, Kanazawa-shi, Ishikawa 920-1192, Japan.
Toxins (Basel). 2015 May 14;7(5):1664-82. doi: 10.3390/toxins7051664.
A high-resolution liquid chromatography-Orbitrap mass spectrometry (LC-Orbitrap MS) method was developed for simultaneous determination of 20 Fusarium toxins (nivalenol, fusarenon-X, deoxynivalenol, 3-acetyl deoxynivalenol, 15-acetyl deoxynivalenol, HT-2 toxin, T-2 toxin, neosolaniol, diacetoxyscirpenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisin A1, fumonisin A2, fumonisin A3, zearalenone, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol) in cereals. The separation of 20 Fusarium toxins with good peak shapes was achieved using a pentafluorophenyl column, and Orbitrap MS was able to detect accurately from cereal matrix components within ±0.77 ppm. The samples were prepared using a QuEChERS kit for extraction and a multifunctional cartridge for purification. The linearity, repeatability, and recovery of the method were >0.9964, 0.8%-14.7%, and 71%-106%, respectively. Using this method, an analysis of 34 commercially available cereals detected the presence of deoxynivalenol, 15-acetyl deoxynivalenol, fumonisin B1, fumonisin B2, fumonisin B3, fumonisn A1, fumonisin A2, fumonisin A3, and zearalenone in corn samples with high concentration and frequency. Trichothecenes was detected from wheat samples with high frequency; in particular, the concentration of deoxynivalenol was high. Conversely, α-zearalenol, β-zearalenol, α-zearalanol, and β-zearalanol were not detected in any of the samples.
建立了一种高分辨率液相色谱 - 轨道阱质谱(LC - Orbitrap MS)方法,用于同时测定谷物中的20种镰刀菌毒素(雪腐镰刀菌烯醇、镰刀菌烯酮 - X、脱氧雪腐镰刀菌烯醇、3 - 乙酰脱氧雪腐镰刀菌烯醇、15 - 乙酰脱氧雪腐镰刀菌烯醇、HT - 2毒素、T - 2毒素、新茄病镰刀菌烯醇、二醋酸镳草镰刀菌烯醇、伏马毒素B1、伏马毒素B2、伏马毒素B3、伏马毒素A1、伏马毒素A2、伏马毒素A3、玉米赤霉烯酮、α - 玉米赤霉醇、β - 玉米赤霉醇、α - 玉米赤霉醛和β - 玉米赤霉醛)。使用五氟苯基柱实现了20种镰刀菌毒素的良好峰形分离,轨道阱质谱能够在±0.77 ppm范围内从谷物基质成分中准确检测。样品采用QuEChERS试剂盒进行提取,并用多功能柱进行净化。该方法的线性、重复性和回收率分别>0.9964、0.8% - 14.7%和71% - 106%。使用该方法对34种市售谷物进行分析,发现玉米样品中高浓度且频繁地存在脱氧雪腐镰刀菌烯醇、15 - 乙酰脱氧雪腐镰刀菌烯醇、伏马毒素B1、伏马毒素B2、伏马毒素B3、伏马毒素A1、伏马毒素A2、伏马毒素A3和玉米赤霉烯酮。小麦样品中频繁检测到单端孢霉烯族毒素;特别是脱氧雪腐镰刀菌烯醇浓度较高。相反,在任何样品中均未检测到α - 玉米赤霉醇、β - 玉米赤霉醇、α - 玉米赤霉醛和β - 玉米赤霉醛。