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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >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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Arsenic species determination in human scalp hair by pressurized hot water extraction and high performance liquid chromatography-inductively coupled plasma-mass spectrometry

机译:加压热水萃取-高效液相色谱-电感耦合等离子体质谱法测定人头皮中的砷

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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 150 mM 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 1500 psi for 5 min in four extraction step. Under optimised conditions, limits of quantification of 7.0, 6.3 and 50.3 ng g~(-1) for 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.
机译:已经开发了测定人头皮头发中总砷和砷种类(主要是As(III)和As(V))的分析方法。电感耦合等离子体质谱法(ICP-MS)和与ICP-MS耦合的高效液相色谱法(HPLC)分别用于总砷和砷种类的测定。所提出的方法包括通过加压热水提取(PHWE)进行的“绿色”,快速,高效和自动化的物种浸出程序。使用实验设计(Plackett-Burman设计PBD)研究了PHWE的操作参数,包括改性剂浓度,萃取温度,静态时间,萃取步骤,压力,平均粒径,硅藻土(DE)质量/样品质量比和冲洗体积。 。最佳条件意味着改性剂浓度(乙酸)为150 mM,并且粉末状头发样品与硅藻土(DE)作为分散剂完全混合,DE质量/样品质量比为5。萃取在100°C下进行在四个萃取步骤中,在1500 psi的萃取压力下进行5分钟。在优化条件下,总砷,砷(III)和砷(V)的定量限分别达到7.0、6.3和50.3 ng g〜(-1)。整个过程的可重复性(总砷,砷(III)和砷(V)分别为4.4%,7.2%和2.1%)。经GBW-07601(人发)认证的参考材料的分析用于验证。优化的方法已最终应用于几种人类头皮头发样品。

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