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室温下用氢氧化四甲铵溶解后,通过电感耦合等离子体质谱法(ICP-MS)同时测定指甲样品中的镉、铜、锰、镍、铅和锌:与电热原子吸收光谱法的比较

Simultaneous determination of Cd, Cu, Mn, Ni, Pb and Zn in nail samples by inductively coupled plasma mass spectrometry (ICP-MS) after tetramethylammonium hydroxide solubilization at room temperature: comparison with ETAAS.

作者信息

Batista Bruno L, Rodrigues Jairo L, Nunes Juliana A, Tormen Luciano, Curtius Adilson J, Barbosa Fernando

机构信息

Laboratório de Toxicologia e Essencialidade de Metais, Depto. de Análises Clínicas, Toxicológicas e Bromatológicas, Faculdade de Ciências Farmacêuticas de Ribeirão Preto-USP, Avenida do Café s/n, Monte Alegre 14040-903, Ribeirão Preto-SP, Brazil.

出版信息

Talanta. 2008 Jul 30;76(3):575-9. doi: 10.1016/j.talanta.2008.03.046. Epub 2008 Apr 7.

Abstract

A simple method is described for the determination of Cd, Cu, Mn, Ni, Pb and Zn in nails by using inductively coupled plasma mass spectrometry (ICP-MS) or electrothermal atomic absorption spectrometry (ETAAS). Prior to analysis, 10-20 mg of nail samples were accurately weighed into (15 mL) conical tubes. Then, 1 mL of 25% (w/v) tetramethylammonium hydroxide (TMAH) solution was added to the samples, incubated at room temperature overnight and then further diluted to 10 mL with 1% (v/v) HNO(3). After that, samples were directly analyzed. Rhodium was used as internal standard for ICP-MS analysis. Method detection limits (3 s, n=20) were 0.1, 3.0, 1.0, 4.5, 1.5, 5.0 ng g(-1) for Cd, Cu, Mn, Ni, Pb and Zn, respectively for ICP-MS, and 24, 26, 30, 143, 130 and 1000 ng g(-1), respectively for ETAAS. The key issue addressed here is the elimination of the acid digestion prior to analysis. Moreover, with the use of the proposed method there is a considerable improvement in the sample throughput comparing to the traditional methods using microwave-assisted acid sample digestion prior to analysis. For validation purposes, six ordinary nail samples were solubilized and then directly analyzed by ICP-MS and ETAAS, with no statistical difference between the two techniques at 95% level on applying the t-test.

摘要

本文描述了一种通过电感耦合等离子体质谱法(ICP-MS)或电热原子吸收光谱法(ETAAS)测定指甲中镉(Cd)、铜(Cu)、锰(Mn)、镍(Ni)、铅(Pb)和锌(Zn)的简单方法。分析前,将10 - 20毫克指甲样品精确称重至(15毫升)锥形管中。然后,向样品中加入1毫升25%(w/v)的四甲基氢氧化铵(TMAH)溶液,在室温下孵育过夜,再用1%(v/v)的硝酸(HNO₃)进一步稀释至10毫升。之后,对样品进行直接分析。铑用作ICP-MS分析的内标。ICP-MS分析的方法检测限(3s,n = 20),镉、铜、锰、镍、铅和锌分别为0.1、3.0、1.0、4.5、1.5、5.0纳克/克⁻¹,ETAAS分析的方法检测限分别为24、26、30、143、130和1000纳克/克⁻¹。这里解决的关键问题是消除分析前的酸消解步骤。此外,与分析前使用微波辅助酸消解样品的传统方法相比,采用本方法可显著提高样品通量。为进行验证,将六个普通指甲样品溶解后,直接用ICP-MS和ETAAS进行分析,应用t检验,两种技术在95%置信水平下无统计学差异。

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