BAM Federal Institute for Materials Research and Testing, Berlin, Germany.
J Chromatogr A. 2010 Apr 9;1217(15):2206-15. doi: 10.1016/j.chroma.2010.02.019. Epub 2010 Feb 18.
A novel, cost-efficient method for the analytical extraction of the Fusarium mycotoxin zearalenone (ZON) from edible oils by dynamic covalent hydrazine chemistry (DCHC) was developed and validated for its application with high performance liquid chromatography-fluorescence detection (HPLC-FLD). ZON is extracted from the edible oil by hydrazone formation on a polymer resin functionalised with hydrazine groups and subsequently released by hydrolysis. Specifity and precision of this approach are superior to liquid partitioning or gel permeation chromatography (GPC). DCHC also extracts zearalanone (ZAN) but not alpha-/beta-zearalenol or -zearalanol. The hydrodynamic properties of ZON, which were estimated using molecular simulation data, indicate that the compound is unaffected by nanofiltration through the resin pores and thus selectively extracted. The method's levels of detection and quantification are 10 and 30 microg/kg, using 0.2g of sample. Linearity is given in the range of 10-20,000 microg/kg, the average recovery being 89%. Bias and relative standard deviations do not exceed 7%. In a sample survey of 44 commercial edible oils based on various agricultural commodities (maize, olives, nuts, seeds, etc.) ZON was detected in four maize oil samples, the average content in the positive samples being 99 microg/kg. The HPLC-FLD results were confirmed by HPLC-tandem mass spectrometry and compared to those obtained by a liquid partitioning based sample preparation procedure.
开发并验证了一种新颖的、经济高效的方法,通过动态共价肼化学(DCHC)从食用油中分析提取镰刀菌真菌毒素玉米赤霉烯酮(ZON),并将其应用于高效液相色谱-荧光检测(HPLC-FLD)。ZON 通过肼基团官能化的聚合物树脂上的腙形成从食用油中提取,然后通过水解释放。这种方法的特异性和精密度优于液液分配或凝胶渗透色谱(GPC)。DCHC 还提取玉米赤烯酮(ZAN),但不提取α-/β-玉米赤醇或玉米赤烯醇。使用分子模拟数据估计的 ZON 流体动力学性质表明,该化合物不受树脂孔纳米过滤的影响,因此可以选择性提取。该方法的检测限和定量限分别为 10 和 30 μg/kg,使用 0.2 g 样品。线性范围为 10-20,000 μg/kg,平均回收率为 89%。偏差和相对标准偏差不超过 7%。在基于各种农产品(玉米、橄榄、坚果、种子等)的 44 种商业食用油的抽样调查中,在 4 种玉米油样品中检测到 ZON,阳性样品中的平均含量为 99 μg/kg。通过高效液相色谱-串联质谱法对 HPLC-FLD 结果进行了确认,并与基于液液分配的样品制备程序获得的结果进行了比较。
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