D'Ilio S, Violante N, Di Gregorio M, Senofonte O, Petrucci F
Department of Environment and Primary Prevention, Istituto Superiore di Sanità, Viale Regina Elena, 299, 00161 Rome, Italy.
Anal Chim Acta. 2006 Oct 10;579(2):202-8. doi: 10.1016/j.aca.2006.07.027. Epub 2006 Jul 18.
A quadrupole inductively coupled plasma mass spectrometer (Q-ICP-MS) equipped with a dynamic reaction cell (DRC) and coupled with a desolvating nebulization system (APEX-IR) was employed to determine 17 elements (Al, As, Ba, Cd, Co, Cr, Li, Mn, Mo, Ni, Pb, Sb, Se, Sn, Sr, V, and Zr) in blood samples. Ammonia (for Al, Cr, Mn, and V) and O2 (for As and Se) were used as reacting gases. Selection of the best flow rate of the gases and optimization of the quadrupole dynamic bandpass tuning parameter (RPq) were carried out, using digested blood diluted 1+9 with deionized water and spiked with 1 microg L(-1) of Al, Cr, Mn, V and 5 microgL(-1) of As and Se. Detection limits were determined in digested blood using the 3sigma criterion. The desolvating system allowed a sufficient sensitivity to be achieved to determine elements at levels of ng L(-1) without detriment of signal stability. The accuracy of the method was tested with the whole blood certified reference material (CRM), certified for Al, As, Cd, Co, Cr, Mn, Mo, Ni, Pb, Sb, Se, and V, and with indicative values for Ba, Li, Sn, Sr, and Zr. The addition calibration approach was chosen for analysis. In order to confirm the DRC data, samples were also analyzed by means of sector field inductively coupled plasma mass spectrometry (SF-ICP-MS), operating in medium (m/Deltam=4000) and high (m/Deltam=10,000) resolution mode and achieving a good agreement between the two techniques.
使用配备动态反应池（DRC）并与去溶剂化雾化系统（APEX-IR）联用的四极杆电感耦合等离子体质谱仪（Q-ICP-MS）测定血液样本中的17种元素（铝、砷、钡、镉、钴、铬、锂、锰、钼、镍、铅、锑、硒、锡、锶、钒和锆）。使用氨气（用于测定铝、铬、锰和钒）和氧气（用于测定砷和硒）作为反应气体。采用去离子水1+9稀释并添加1 μg L⁻¹的铝、铬、锰、钒以及5 μg L⁻¹的砷和硒的消化血液，对气体的最佳流速进行选择，并对四极杆动态带通调谐参数（RPq）进行优化。采用3σ准则测定消化血液中的检测限。去溶剂化系统实现了足够的灵敏度，能够测定纳克每升水平的元素，且不影响信号稳定性。使用经认证的全血标准物质（CRM）对该方法的准确性进行测试，该标准物质对铝、砷、镉、钴、铬、锰、钼、镍、铅、锑、硒和钒进行了认证，并给出了钡、锂、锡、锶和锆的指示值。分析采用加法校准方法。为了确认DRC数据，还通过扇形磁场电感耦合等离子体质谱仪（SF-ICP-MS）对样品进行分析，该仪器在中分辨率（m/Δm = 4000）和高分辨率（m/Δm = 10,000）模式下运行，两种技术之间取得了良好的一致性。
