Department of Analytical Chemistry, Medical University of Lublin, Chodźki 4a, 20-093 Lublin, Poland.
Children's Orthopedics Department, Medical University of Lublin, Gębali 6, 20-093 Lublin, Poland.
Talanta. 2017 Apr 1;165:351-356. doi: 10.1016/j.talanta.2016.12.077. Epub 2016 Dec 27.
Trace analysis plays an important role in medicine for diagnosis of various disorders; however, the appropriate sample preparation is required mostly including mineralization. Although graphite furnace atomic absorption spectrometry (GF AAS) allows the investigation of biological samples such as blood, serum, and plasma without this step, it is rarely used for direct analysis because the residues of the rich organic matrix inside the furnace are difficult to remove and this may cause spectral/matrix interferences and decrease the lifetime of the graphite tube. In our work, the procedure for determination of Se, Cr, Mn, Co, Ni, Cd and Pb with the use of the high resolution continuum source GF-AAS technique in whole blood samples with minimum sample pre-treatment was elaborated. The pyrolysis and atomization temperature as well as the time of signal integration were optimized to obtain the highest intensity and repeatability of the analytical signal. Moreover, due to the apparatus modification, an additional step was added in the for graphite furnace temperature program with minimal argon flow and maximal flow of air during pyrolysis stage to increase the oxidative condition for better matrix removal. The accuracy and precision of the optimized method was verified using certified reference material (CRM) Seronorm Trace Elements Whole Blood L-1 and the developed method was applied for trace analysis of blood samples from volunteer patients of the Orthopedics Department.
痕量分析在医学诊断各种疾病中起着重要作用;然而,通常需要适当的样品制备,包括矿化。虽然石墨炉原子吸收光谱(GF AAS)允许在不进行此步骤的情况下研究生物样品,如血液、血清和血浆,但由于炉内富含有机基质的残留物难以去除,这可能会引起光谱/基质干扰并降低石墨管的寿命,因此很少用于直接分析。在我们的工作中,详细阐述了使用高分辨率连续光源 GF-AAS 技术在最小样品预处理的全血样品中测定硒、铬、锰、钴、镍、镉和铅的程序。优化了热解和原子化温度以及信号积分时间,以获得分析信号的最高强度和重复性。此外,由于仪器改装,在石墨炉温度程序中添加了一个额外的步骤,在热解阶段最小化氩气流和最大化空气流量,以增加氧化条件,更好地去除基质。使用认证参考物质(CRM)Seronorm Trace Elements Whole Blood L-1 验证了优化方法的准确性和精密度,并将该方法应用于骨科志愿者患者的血液样本进行痕量分析。