Food and Agricultural Materials Inspection Center, Saitama Shintoshin National Government Building, Kensato Building, Shintoshin 2-1, Chuo-Ku, Saitama-Shi, Saitama, 330-9731, Japan.
Sendai Regional Center, Food and Agricultural Materials Inspection Center, Sendai National Government Building III, 1-3-15, Gorin, Miyagino-Ku, Sendai-Shi, Miyagi, 983-0842, Japan.
Mycotoxin Res. 2020 Nov;36(4):353-360. doi: 10.1007/s12550-020-00401-z. Epub 2020 Jul 11.
An analytical method for the simultaneous quantitation of ten trichothecenes of type A (HT-2 toxin, T-2 toxin, diacetoxyscirpenol, and neosolaniol) and type B (3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol, deoxynivalenol, deoxynivalenol-3-glucoside, nivalenol, and fusarenon-X) in feed has been developed using liquid chromatography with tandem mass spectrometry. Mycotoxins extracted twice from samples using aqueous acetonitrile were purified using a multifunctional clean-up column, followed by a phospholipid removal column. Trichothecenes were analysed using liquid chromatography atmospheric pressure chemical ionization tandem mass spectrometry. The extraction efficiency of the mycotoxins and the repeatability of some were improved by repeated extractions. Ionization enhancement (signal enhancement) of some mycotoxins was improved by using the phospholipid removal column at the clean-up step. Spike and recovery tests of trichothecenes were conducted on maize, barley, soybean meal, rapeseed meal, and formula feeds (for starting broiler chicks, suckling pigs, and beef cattle). The mean recovery values were 70.6-119% with relative standard deviations < 17%. The limit of quantification and the limit of detection of our method were 20 and 6 μg/kg, respectively, for 3-acetyldeoxynivalenol and 15-acetyldeoxynivalenol; 10 and 3 μg/kg, respectively, for T-2 toxin, deoxynivalenol, and fusarenon-X; and 5 and 2 μg/kg, respectively, for nivalenol and the remaining mycotoxins.
建立了一种同时测定饲料中 A 型（HT-2 毒素、T-2 毒素、二乙酰基脱氧雪腐镰刀菌烯醇和雪腐镰刀菌烯醇）和 B 型（3-乙酰脱氧雪腐镰刀菌烯醇、15-乙酰脱氧雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇、脱氧雪腐镰刀菌烯醇-3-葡萄糖苷、玉米赤霉烯酮和伏马菌素-X）十种镰刀菌毒素的分析方法，采用液相色谱-串联质谱法。采用水-乙腈两次从样品中提取真菌毒素，用多功能净化柱净化，然后用磷脂去除柱净化。采用液相色谱-大气压化学电离串联质谱法分析镰刀菌毒素。通过重复提取，提高了真菌毒素的提取效率和部分重复性。在净化步骤中使用磷脂去除柱，提高了部分真菌毒素的离子化增强（信号增强）。在玉米、大麦、豆粕、菜粕和配合饲料（用于起始肉鸡、仔猪和肉牛）中进行了镰刀菌毒素的加标和回收试验。3-乙酰脱氧雪腐镰刀菌烯醇和 15-乙酰脱氧雪腐镰刀菌烯醇的平均回收率为 70.6-119%，相对标准偏差<17%。该方法的定量限和检测限分别为 3-乙酰脱氧雪腐镰刀菌烯醇和 15-乙酰脱氧雪腐镰刀菌烯醇为 20 和 6μg/kg，T-2 毒素、脱氧雪腐镰刀菌烯醇和伏马菌素-X 为 10 和 3μg/kg，玉米赤霉烯酮和其余真菌毒素为 5 和 2μg/kg。
