Sajnóg Adam, Tkaczyk Marcin, Stańczyk Małgorzata, Szaflik Krzysztof, Suliburska Joanna, Kocyłowski Rafał, Barałkiewicz Danuta
Department of Trace Analysis, Faculty of Chemistry, Adam Mickiewicz University, Poznań, ul. Uniwersytetu Poznańskiego 8, 61-614, Poznań, Poland; Center for Advanced Technology, Adam Mickiewicz University, Poznań, ul. Uniwersytetu Poznańskiego 10, 61-614, Poznań, Poland.
Department of Pediatrics, Immunology and Nephrology, Polish Mother's Memorial Hospital Research Institute, ul. Rzgowska 281/289, 93-338, Lódź, Poland.
Talanta. 2021 Jan 15;222:121672. doi: 10.1016/j.talanta.2020.121672. Epub 2020 Sep 17.
The procedure for determination of 21 macro- and trace elements - Li, Na, Mg, Al, K, Ca, V, Cr, Mn, Fe, Co, Cu, Zn, Se, Sr, As, Cd, Sb, Ba, Pb and U - in human fetal urine by inductively coupled plasma mass spectrometry (ICP-MS) was developed and validated. The application of a micronebulizer and a dynamic reaction cell (DRC) allowed to perform a full analysis of small volumes (200 μL) of urine collected from human fetuses without the need for sample digestion with closed microwave systems. The procedure and ICP-MS instrument was thoroughly optimized in order to reliably determine both macroelements and ultra-trace concentrations of elements. The internal standard method (Ge, Rh and Tb) was applied in order to encompass signal drift and non-spectral interferences. The rules of metrology were used in order to ensure the quality of the results: (1) the procedure was validated, (2) the uncertainty of the measurement results was estimated and (3) the traceability of the measurement result was established by using the certified reference material with matching matrix (Seronorm Trace Elements Urine L-1). Also, the analyte addition method to the artificial urine was employed for additional confirmation of trueness of the procedure. The selected parameters of the procedure were as follows: (a) limits of detection - (0.00023-53 μg L) for U and Ca, respectively, (b) recoveries of the reference value - 81%-136% for Mn and Cd, respectively (c) linearity expressed as R - greater than 0.999, and (d) expanded relative uncertainties (k = 2) - 13%-66% for Sr and Cd, respectively. The developed and validated procedure was applied to 58 samples of urine collected from human fetuses. The samples were diluted with nitric acid and analyzed without further treatment. The procedure allowed to reliably determine both macro- and trace elements in very low volume of sample in a single analytical run.
建立并验证了用电感耦合等离子体质谱法（ICP-MS）测定人胎儿尿液中21种常量和微量元素——锂（Li）、钠（Na）、镁（Mg）、铝（Al）、钾（K）、钙（Ca）、钒（V）、铬（Cr）、锰（Mn）、铁（Fe）、钴（Co）、铜（Cu）、锌（Zn）、硒（Se）、锶（Sr）、砷（As）、镉（Cd）、锑（Sb）、钡（Ba）、铅（Pb）和铀（U）的方法。使用微量雾化器和动态反应池（DRC），无需用密闭微波系统对样品进行消解，就能对从人胎儿采集的少量（200 μL）尿液进行全面分析。对该方法和ICP-MS仪器进行了全面优化，以便可靠地测定常量元素和超痕量元素浓度。采用内标法（锗、铑和铽）来克服信号漂移和非光谱干扰。运用计量学规则以确保结果的质量：（1）对方法进行验证；（2）估算测量结果的不确定度；（3）通过使用具有匹配基质的有证标准物质（Seronorm Trace Elements Urine L-1）来建立测量结果的溯源性。此外，还采用了向人工尿液中添加分析物的方法来进一步确认该方法的准确性。该方法选定的参数如下：（a）检测限——铀和钙分别为（0.00023 - 53 μg/L）；（b）参考值回收率——锰和镉分别为81% - 136%；（c）以R表示的线性度——大于0.999；（d）扩展相对不确定度（k = 2）——锶和镉分别为13% - 66%。将已建立并验证的方法应用于58份从人胎儿采集的尿液样本。样本用硝酸稀释后无需进一步处理即可进行分析。该方法能够在单次分析运行中可靠地测定极少量样本中的常量和微量元素。
