ARPA ER (Regional Environmental Prevention Agency of Emilia Romagna), Analytical Area OGM, Mycotoxin and Food Safety, via Rocchi, 19, 40138 Bologna, Italy.
J Mass Spectrom. 2010 Sep;45(9):1075-80. doi: 10.1002/jms.1802.
In this study, the simultaneous determination of deoxynivalenol (DON), zearalenone (ZEA), T-2 and HT-2 toxins in foodstuff was investigated. A new kind of multi-mycotoxin immunoaffinity columns (IACs) available on the market (DZT MS-PREP(®)) was tested. A sensitive, selective and accurate method by high-performance liquid chromatography and tandem mass spectrometry was developed, with electrospray ionization mass spectrometer operating in multiple reaction monitoring (MRM) mode, with negative-positive-negative ion switching. The method was used for the analysis of samples marked in Italy, in the frame of official monitoring plans. The advantages of combining IACs and LC-MS/MS technique are as follows: efficient removal of matrix interferences, simple chromatographic outline, high selectivity, low detection limits (DLs) and separation of a wide range of molecules with different physico-chemical properties in a single run. The method was studied on two different matrices, breakfast cereal and baby food, at contamination levels close to Regulation limits (EC) 1126/2007. The recoveries obtained (60-100%) fulfil the performance criteria required by Regulation (EC) 401/2006. The DL is 60 µg/kg for DON and 10 µg/kg for ZEA, T-2 and HT-2. Linearity range of the calibration curves is suitable for adult and baby food.
本研究旨在探索食品中脱氧雪腐镰刀菌烯醇(DON)、玉米赤霉烯酮(ZEA)、T-2 毒素和 HT-2 毒素的同时测定方法。我们对市场上一种新型多真菌毒素免疫亲和柱(IACs)(DZT MS-PREP(®))进行了测试。建立了一种基于高效液相色谱-串联质谱(LC-MS/MS),采用电喷雾电离源(ESI),多重反应监测(MRM)模式,并切换正负离子检测,具有高灵敏度、选择性和准确性的方法。该方法用于意大利官方监测计划框架内的标记样品分析。IACs 与 LC-MS/MS 技术结合的优点在于:可有效去除基质干扰,色谱轮廓简单,选择性高,检测限(DLs)低,且可在单次运行中分离具有不同物理化学性质的多种分子。该方法研究了两种不同基质(早餐麦片和婴儿食品)在接近法规(EC)1126/2007 限量水平的污染水平下的情况。获得的回收率(60-100%)满足法规(EC)401/2006 规定的性能标准。DON 和 ZEA、T-2 和 HT-2 的 DL 分别为 60 µg/kg 和 10 µg/kg。校准曲线的线性范围适用于成人和婴儿食品。