Gao Bei, Jiang Deming, Yang Yongtan
Chinese Oil & Foodstuffs Corporation (COFCO) Nutrition and Health Research Institute, Beijing Key Laboratory of Nutrition Health and Food Safety, Beijing 102209, China.
Se Pu. 2017 Jun 8;35(6):601-607. doi: 10.3724/SP.J.1123.2016.12028.
A rapid method was established for the determination of zearalenone (ZON), nivalenol (NIV), deoxynivalenol (DON), 3-acetyl-deoxynivalenol (3-ACDON) and 15-acetyl-deoxynivalenol (15-ACDON) in various grains and their products by liquid chromatography-tandem mass spectrometry (LC-MS/MS). The samples were extracted by acetonitrile-water (84:16, v/v), and cleaned-up by multifunctional column without any further step. The separation was carried out on an Acquity UPLC BEH C18 column (100 mm×2.1 mm, 1.7 μm) with gradient elution using acetonitrile-water as mobile phases. The analytes were quantified by isotope internal standard method. The correlation coefficients () were all above 0.99. The limits of detection (LODs, =3) ranged from 5 μg/kg to 20 μg/kg. The recoveries of the five mycotoxins spiked in blank grain and its product samples varied from 84.2% to 114.5%, with the relative standard deviations (RSDs) of 0.4%-9.9% (=6). The method is accurate, efficient, sensitive and practical.
建立了一种快速测定各种谷物及其制品中玉米赤霉烯酮（ZON）、雪腐镰刀菌烯醇（NIV）、脱氧雪腐镰刀菌烯醇（DON）、3-乙酰基脱氧雪腐镰刀菌烯醇（3-ACDON）和15-乙酰基脱氧雪腐镰刀菌烯醇（15-ACDON）的方法，采用液相色谱-串联质谱法（LC-MS/MS）。样品用乙腈-水（84:16，v/v）提取，并用多功能柱净化，无需进一步处理。在Acquity UPLC BEH C18柱（100 mm×2.1 mm，1.7 μm）上进行分离，以乙腈-水为流动相进行梯度洗脱。采用同位素内标法定量分析物。相关系数（）均大于0.99。检测限（LODs，=3）为5 μg/kg至20 μg/kg。在空白谷物及其制品样品中添加的五种霉菌毒素的回收率为84.2%至114.5%，相对标准偏差（RSDs）为0.4%至9.9%（=6）。该方法准确、高效、灵敏、实用。
