Department of Analytical Chemistry, Faculty of Chemistry, Universidad de Valencia, Dr. Moliner 50, E-46100 Burjassot, Valencia, Spain.
Talanta. 2011 May 30;84(4):1112-7. doi: 10.1016/j.talanta.2011.03.017. Epub 2011 Mar 16.
There is a need to develop sensitive and accurate analytical methods for determining deoxynivalenol (DON), HT-2 toxin and T-2 toxin in paprika to properly assess the relevant risk of human exposure. An optimized analytical method for determination of HT-2 toxin and T-2 toxin using capillary gas chromatography with electron capture detection and another method for determination of DON by liquid chromatography-mass spectrometry in paprika was developed. The method for determination of HT-2 toxin and T-2 toxin that gave the best recoveries involved extraction of the sample with acetonitrile-water (84:16, v/v), clean-up by solid-phase extraction on a cartridge made of different sorbent materials followed by a further clean-up in immunoaffinity column that was specific for the two toxins. The solvent was changed and the eluate was derivatized with pentafluoropropionic anhydride and injected into the GC system. The limits of detection (LOD) for T-2 and HT-2 toxins were 7 and 3 μg/kg, respectively, and the recovery rates for paprika spiked with 1000 μg toxin/kg were 71.1% and 80.1% for HT-2 and T-2 toxins, respectively. For DON determination, the optimized method consisted of extraction with acetonitrile-water (84:16, v/v) solution followed by a solid-phase extraction clean-up process in a cartridge made of different sorbent compounds. After solvent evaporation in N(2) stream, the residue was dissolved and DON was separated and determined by LC-MS/MS. The LOD for this method was 14 μg DON/kg paprika sample and the DON recovery rate was 86.8%.
需要开发灵敏准确的分析方法来测定辣椒粉中的脱氧雪腐镰刀菌烯醇(DON)、HT-2 毒素和 T-2 毒素,以正确评估人类接触的相关风险。本研究建立了同时测定辣椒粉中 HT-2 毒素和 T-2 毒素的毛细管气相色谱-电子捕获检测法和测定 DON 的液相色谱-质谱法。HT-2 毒素和 T-2 毒素的最佳提取方法为乙腈-水(84:16,v/v)提取,固相萃取小柱净化,免疫亲和柱进一步净化,特异性洗脱;DON 的最佳提取方法为乙腈-水(84:16,v/v)提取,固相萃取小柱净化,氮气流下蒸发溶剂,残渣用甲醇溶解。HT-2 毒素和 T-2 毒素的检测限(LOD)分别为 7 和 3 μg/kg,1000 μg 毒素/kg 辣椒粉加标回收率分别为 71.1%和 80.1%;DON 的检测限(LOD)为 14 μg DON/kg 辣椒粉,回收率为 86.8%。