University of Silesia, Institute of Chemistry, Szkolna 9, 40-006 Katowice, Poland.
University of Silesia, Institute of Chemistry, Szkolna 9, 40-006 Katowice, Poland.
Food Chem. 2022 Oct 1;390:133136. doi: 10.1016/j.foodchem.2022.133136. Epub 2022 May 5.
The paper presents novel analytical methods for sensitive mercury determination in various samples, i.e., waters, beverages, seafood, plants, and biological samples. The procedure is based on selective preconcentration/separation of Hg(II) ions using graphene oxide/thiosemicarbazide in dispersive micro-solid phase extraction (DMSPE) and detection by energy-dispersive (EDXRF) and total-reflection X-ray fluorescence spectrometry (TXRF). The DMSPE/EDXRF and DMSPE/TXRF procedures are characterized by very high enrichment factors and low detection limits (LODs). DMSPE/TXRF allows obtaining LODs of 2.1 pg mL for liquids and 1.8 ng g for solid samples. In the case of DMSPE/EDXRF, the LODs are higher, 60 pg mL for liquid and 73 ng g for solid samples, due to the worse sensitivity of EDXRF measurement. The method was validated using spiked samples (water, apple juice, beer, wine) and certified reference materials (seawater, groundwater, wastewater, herring, cormorant and cod tissues, pig kidney, lobster, tobacco, scallion, celery, and spinach).
本文提出了用于在各种样品（如水、饮料、海鲜、植物和生物样品）中灵敏测定汞的新分析方法。该方法基于使用氧化石墨烯/硫代氨基脲在分散微固相萃取（DMSPE）中选择性预浓缩/分离 Hg(II)离子，并通过能量色散 X 射线荧光光谱法（EDXRF）和全反射 X 射线荧光光谱法（TXRF）进行检测。DMSPE/EDXRF 和 DMSPE/TXRF 程序的特点是具有非常高的富集因子和低检测限（LOD）。DMSPE/TXRF 允许获得液体的 LOD 为 2.1 pg mL，固体样品的 LOD 为 1.8 ng g。对于 DMSPE/EDXRF，由于 EDXRF 测量的灵敏度较差，液体的 LOD 为 60 pg mL，固体样品的 LOD 为 73 ng g。该方法使用加标样品（水、苹果汁、啤酒、葡萄酒）和认证参考材料（海水、地下水、废水、鲱鱼、鸬鹚和鳕鱼组织、猪肾、龙虾、烟草、葱、芹菜和菠菜）进行了验证。
