Batista Bruno Lemos, Grotto Denise, Rodrigues Jairo Lisboa, Souza Vanessa Cristina de Oliveira, Barbosa Fernando
Departamento de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto, FCFRP, USP, Avenida do Café, s/n, Monte Alegre, 14040-903, Ribeirão Preto, SP, Brazil.
Anal Chim Acta. 2009 Jul 30;646(1-2):23-9. doi: 10.1016/j.aca.2009.05.022. Epub 2009 May 21.
A simple method for sample preparation of biological samples for trace elements determination by inductively coupled plasma mass spectrometry (ICP-MS) is described. Prior to analysis, 75 mg of the biological samples were accurately weighed into (15 mL) conical tubes. Then, 1 mL of 50% (v/v) tetramethylammonium hydroxide (TMAH) solution was added to the samples, incubated at room temperature for 12 h and the volume made up to 10 mL with a solution containing 0.5% (v/v) HNO(3), 0.01% (v/v) Triton X-100 and 10 microg L(-1) of Rh. After preparation samples may be stored at -20 degrees C during 3 days until the analysis by ICP-MS. With these conditions, the use of the dynamic reaction cell was only mandatory for chromium determination. Method detection limits were 0.2145, 0.0020, 0.0051, 0.0017, 0.0027, 0.0189, 0.02, 0.5, 0.1, 0.0030, 0.0043, 0.0066, 0.0009, 0.020, 0.0043, 0.1794, 0.1 microg(-1) for Al, As, Ba, Cd, Co, Cr, Cu, Fe, Mg, Mn, Mo, Pb, Sb, Se, Sr, V and Zn, respectively. Validation data are provided based on the analysis of six certified reference materials (CRMs) purchased from the National Institute of Standards and Technology (NIST) and National Research Council Canada (NRCC). Additional validation was provided by the analysis of brain, kidney, liver and heart samples collected from rats and analyzed by the proposed method and by using microwave digestion.
本文描述了一种通过电感耦合等离子体质谱法(ICP-MS)测定生物样品中微量元素的简单样品制备方法。分析前,将75毫克生物样品精确称入(15毫升)锥形管中。然后,向样品中加入1毫升50%(v/v)的四甲基氢氧化铵(TMAH)溶液,在室温下孵育12小时,并用含有0.5%(v/v)HNO₃、0.01%(v/v)Triton X-100和10微克/升Rh的溶液将体积补足至10毫升。制备后的样品可在-20℃下保存3天,直至通过ICP-MS进行分析。在这些条件下,仅在测定铬时必须使用动态反应池。方法的检测限分别为铝0.2145、砷0.0020、钡0.0051、镉0.0017、钴0.0027、铬0.0189、铜0.02、铁0.5、镁0.1、锰0.0030、钼0.0043、铅0.0066、锑0.0009、硒0.020、锶0.0043、钒0.1794、锌0.1微克/升。基于对从美国国家标准与技术研究院(NIST)和加拿大国家研究委员会(NRCC)购买的六种有证标准物质(CRM)的分析提供了验证数据。通过对从大鼠收集的脑、肾、肝和心脏样品进行分析,并使用所提出的方法以及微波消解进行分析,提供了额外的验证。