Royer D, Humpf H-U, Guy P A
Nestlé Research Center, Nestec Ltd, Vers-Chez-Les-Blanc, CH-1000 Lausanne 26, Switzerland.
Food Addit Contam. 2004 Jul;21(7):678-92. doi: 10.1080/02652030410001711304.
A method for the simultaneous quantitative determination of deoxynivalenol (DON), fumonisin B1 (FB1) and zearalenone (ZEN) in maize by liquid chromatography-atmospheric pressure chemical ionization tandem mass spectrometry (LC-APCIMS/MS), using stable isotopically labelled and structural analogues internal standards, is described. The procedure involves accelerated solvent extraction followed by two solid-phase clean-up steps on strong anion exchange resin and a Mycosep column. Typical recoveries were calculated by spiking blank maize at three different concentrations for deoxynivalenol (200, 400 and 1000 microg kg(-1)) at 70%, for fumonisin B1 (100, 200 and 1000 microg kg(-1)) at 90%, and for zearalenone (50, 100 and 200 microg kg(-1)) at 40%. LC-APCIMS/MS analyses were realized in collision-induced dissociation on an ion-trap instrument to provide a high degree of selectivity and sensitivity. Extraction of ions from two transition reactions, monitored by LC-APCIMS/MS for each analyte, enabled a limit of detection for DON, FB1 and ZEN at, respectively, 10, 20 and 3 microg kg(-1), and a limit of quantification at, respectively, 50, 50 and 10 microg kg(-1). The robustness of the method was also evaluated with the analysis of wheat samples.
描述了一种采用稳定同位素标记和结构类似物内标,通过液相色谱 - 大气压化学电离串联质谱法(LC - APCIMS/MS)同时定量测定玉米中脱氧雪腐镰刀菌烯醇(DON)、伏马菌素B1(FB1)和玉米赤霉烯酮(ZEN)的方法。该方法包括加速溶剂萃取,随后在强阴离子交换树脂和Mycosep柱上进行两步固相净化。通过在空白玉米中添加三种不同浓度的脱氧雪腐镰刀菌烯醇(200、400和1000 μg kg⁻¹),回收率为70%;添加伏马菌素B1(100、200和1000 μg kg⁻¹),回收率为90%;添加玉米赤霉烯酮(50、100和200 μg kg⁻¹),回收率为40%来计算典型回收率。在离子阱仪器上通过碰撞诱导解离进行LC - APCIMS/MS分析,以提供高度的选择性和灵敏度。通过LC - APCIMS/MS监测两种过渡反应的离子提取,使DON、FB1和ZEN的检测限分别为10、20和3 μg kg⁻¹,定量限分别为50、50和10 μg kg⁻¹。还通过对小麦样品的分析评估了该方法的稳健性。