Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.
Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry.
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DOI：
10.1016/j.talanta.2012.10.070
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发表时间：
2013-02
期刊：
影响因子：
6.1
通讯作者：
Andrés Morado Piñeiro;J. Moreda–Piñeiro;E. Alonso-Rodríguez;P. López‐Mahía;S. Muniategui-Lorenzo;D. Pra
中科院分区：
文献类型：
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作者：
Andrés Morado Piñeiro;J. Moreda–Piñeiro;E. Alonso-Rodríguez;P. López‐Mahía;S. Muniategui-Lorenzo;D. Pra
建立了测定人头发中总砷和砷形态(主要是As(III)和As(V))的分析方法。采用电感耦合等离子体质谱(ICP-MS)和高效液相色谱(HPLC)与电感耦合等离子体质谱(ICP-MS)联用技术分别测定总砷和砷形态。所提出的方法包括一种“绿色”、快速、高效和自动化的加压热水浸出(PHWE)方法。采用Plackett-Burman设计(PBD)实验设计，研究了改性剂浓度、萃取温度、静置时间、萃取步骤、压力、平均粒径、硅藻土(DE)质量/样品质量比、冲洗体积等工艺参数。最佳条件为：改性剂浓度(冰醋酸)150 mM，头发粉样充分混合硅藻土(DE)作为分散剂，DE质量/样品质量比为5。在100℃，1500psi的萃取压力下，分4步萃取5min。在优化的条件下，总As、As(III)和As(V)的定量限分别为7.0ng1、6.3ng1和50.3ngg−-1。实现了整个程序的重复性(总As、As(III)和As(V)分别为4.4、7.2和2.1%)。使用GBW-07601(人发)标准物质的分析进行验证。优化后的方法最终应用于几个人的头皮毛发样本。
Analytical methods for the determination of total arsenic and arsenic species (mainly As(III) and As(V)) in human scalp hair have been developed. Inductively coupled plasma-mass spectrometry (ICP-MS) and high performance liquid chromatography (HPLC) coupled to ICP-MS have been used for total arsenic and arsenic species determination, respectively. The proposed methods include a “green”, fast, high efficient and automated species leaching procedure by pressurized hot water extraction (PHWE). The operating parameters for PHWE including modifier concentration, extraction temperature, static time, extraction steps, pressure, mean particle size, diatomaceous earth (DE) mass/sample mass ratio and flush volume were studied using design of experiments (Plackett–Burman design PBD). Optimum condition implies a modifier concentration (acetic acid) of 150mM and powdered hair samples fully mixed with diatomaceous earth (DE) as a dispersing agent at a DE mass/sample mass ratio of 5. The extraction has been carried out at 100°C and at an extraction pressure of 1500psi for 5min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3ngg−1for total As, As(III) and As(V), respectively were achieved. Repeatability of the overall procedure (4.4, 7.2 and 2.1% for total As, As(III) and As(V), respectively) was achieved. The analysis of GBW-07601 (human hair) certified reference material was used for validation. The optimised method has been finally applied to several human scalp hair samples.