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开发了一种使用碱性溶解和石墨炉原子吸收光谱法测定口红中铅的简单方法。

Development of a simple method for the determination of lead in lipstick using alkaline solubilization and graphite furnace atomic absorption spectrometry.

机构信息

Instituto de Ciências Exatas, Departamento de Química, Universidade Federal de Minas Gerais, Avenida Presidente Antônio Carlos, 6627, Pampulha, PO Box 702, CEP 31270-901, Belo Horizonte, Minas Gerais, Brazil.

出版信息

Talanta. 2013 Feb 15;105:272-7. doi: 10.1016/j.talanta.2012.09.021. Epub 2012 Oct 18.

Abstract

A simple method was developed for determining the total lead content in lipstick samples by graphite furnace atomic absorption spectrometry (GFAAS) after treatment with tetramethylammonium hydroxide (TMAH). Multivariate optimization was used to establish the optimal conditions of sample preparation. The graphite furnace heating program was optimized through pyrolysis and atomization curves. An aliquot containing approximately 50mg of the sample was mixed with TMAH and heated in a water bath at 60°C for 60 min. Using Nb as the permanent modifier and Pd as the chemical modifier, the optimal temperatures were 900°C and 1800°C for pyrolysis and atomization, respectively. Under optimum conditions, the working range was from 1.73 to 50.0 μg L(-1), with detection and quantification limits of 0.20 and 0.34 μg g(-1), respectively. The precision was evaluated under conditions of repeatability and intermediate precision and showed standard deviations of 2.37%-4.61% and 4.93%-9.75%, respectively. The % recovery ranged from 96.2% to 109%, and no significant differences were found between the results obtained using the proposed method and the microwave decomposition method for real samples. Lead was detected in 21 tested lipstick samples; the lead content in these samples ranged from 0.27 to 4.54 μg g(-1).

摘要

一种简单的方法是通过石墨炉原子吸收光谱(GFAAS)在经过四甲基氢氧化铵(TMAH)处理后测定口红样品中的总铅含量。多元优化用于建立样品制备的最佳条件。通过热解和原子化曲线优化了石墨炉加热程序。将包含约 50mg 样品的等分试样与 TMAH 混合,并在 60°C 的水浴中加热 60 分钟。使用 Nb 作为永久改性剂和 Pd 作为化学改性剂,热解和原子化的最佳温度分别为 900°C 和 1800°C。在最佳条件下,工作范围为 1.73 至 50.0μg L(-1),检测限和定量限分别为 0.20 和 0.34μg g(-1)。在重复性和中间精密度条件下评估精密度,分别显示标准偏差为 2.37%-4.61%和 4.93%-9.75%。回收率范围为 96.2%至 109%,并且在用所提出的方法和微波分解方法测定实际样品时,未发现结果之间存在显着差异。在 21 个测试的口红样品中检测到铅;这些样品中的铅含量范围为 0.27 至 4.54μg g(-1)。

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