Pytlakowska Katarzyna
Institute of Chemistry, University of Silesia, ul. Szkolna 9, 40-006 Katowice, Poland
Appl Spectrosc. 2016 Nov;70(11):1891-1899. doi: 10.1177/0003702816644758. Epub 2016 Jun 20.
A simple and effective preconcentration procedure based on dispersive micro solid-phase extraction prior to energy dispersive X-ray fluorescence spectrometric (EDXRF) determination of trace amounts of Ni, Cu, and Zn in coffee infusions was proposed. The method is based on the adsorption of 8-hydroxyquinoline metal complexes on micro amounts of graphene nanoparticles. In order to optimize adsorption process, the influence of some parameters such as pH, graphene mass, concentration of 8-hydroxyquinoline (8-HQ) and Triton X-100, sample volume, and sorption time were examined. At optimal preconcentration conditions, calibration curves were linear from 1 to 150 ng mL for Ni and Cu and from 1 to 200 ng mL for Zn. The recoveries of the metal ions were in the 95-98% range with the precision lower than 4.6%. The obtained detection limits were 0.08 ng mL for Ni and 0.09 ng mL for Cu and Zn. The proposed method was successfully applied to determination of Ni, Cu, and Zn in coffee infusions. Accuracy and repeatability of the proposed procedure were confirmed by the standard addition method and compared to the results obtained by ICP-OES technique.
提出了一种基于分散微固相萃取的简单有效的预富集方法,用于在能量色散X射线荧光光谱法(EDXRF)测定咖啡冲泡液中痕量镍、铜和锌之前进行预富集。该方法基于8-羟基喹啉金属络合物在微量石墨烯纳米颗粒上的吸附。为了优化吸附过程,考察了一些参数如pH值、石墨烯质量、8-羟基喹啉(8-HQ)和Triton X-100的浓度、样品体积和吸附时间的影响。在最佳预富集条件下,镍和铜的校准曲线在1至150 ng/mL范围内呈线性,锌的校准曲线在1至200 ng/mL范围内呈线性。金属离子的回收率在95%-98%范围内,精密度低于4.6%。获得的检测限为镍0.08 ng/mL,铜和锌0.09 ng/mL。该方法成功应用于咖啡冲泡液中镍、铜和锌的测定。通过标准加入法证实了该方法的准确性和重复性,并与电感耦合等离子体发射光谱法(ICP-OES)获得的结果进行了比较。