Simultaneous speciation analysis of As, Sb and Se redox couples by SF-ICP-MS coupled to HPLC
Simultaneous speciation analysis of As, Sb and Se redox couples by SF-ICP-MS coupled to HPLC
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DOI：
10.1039/c4ay01013b
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发表时间：
2014-06
影响因子：
3.1
通讯作者：
Debo Wu;T. Pichler
中科院分区：
文献类型：
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作者：
Debo Wu;T. Pichler
建立了双聚焦扇形场电感耦合等离子体质谱（SF-ICP-MS）与高效液相色谱（HPLC）联用同时分析流体样品中无机砷（III，V）、锑（III，V）和硒（IV，VI）形态的新方法。采用汉密尔顿PRX-X 100阴离子交换柱，以EDTA（pH 4.7）和3%甲醇为移动的相，对6种化合物进行分离。流速设定为1.5 mL min-1。在引入溶剂梯度（从5 mM至30 mM的线性斜坡）后，对于所有六种所需物质，总分析时间缩短至11分钟内。As（III）、As（V）、Sb（III）、Sb（V）、Se（VI）和Se（IV）的检测限分别为0.02 μg L−1、0.06 μg L−1、0.2 μ g L − 1、0.02 μ g L − 1、0.2 μg L−1和0.4 μg L−1，这些值是从空白的11次重复测量中获得的。对保留时间的稳定性和校准曲线的线性进行了评价。保留时间（至少20次重复测量）的相对标准偏差（RSD）≤9%，校准曲线（至少6次重复实验）的相关系数（R2）≥0.9998。最后，所提出的方法被应用于一个合成样品，两个温泉样品和两个有证标准物质的分析。结果显示，加标回收率良好，表明色谱分离过程中基本没有质量损失。对两种标准物质的测定结果与标准值吻合较好。
A new method was developed for the simultaneous speciation analysis of inorganic arsenic (III, V), antimony (III, V) and selenium (IV, VI) in fluid samples by double-focusing sector field-inductively coupled plasma-mass spectrometry (SF-ICP-MS) coupled with high performance liquid chromatography (HPLC). A Hamilton PRX-X100 anion exchange column with EDTA (pH of 4.7) and 3% methanol as mobile phase was used for separation of the six species. The flow rate was set at 1.5 mL min−1. The overall analysis time was shortened down to within 11 minutes for all six desired species after a solvent gradient (linear ramp from 5 mM to 30 mM) was introduced in. The detection limits for As(III), As(V), Sb(III), Sb(V), Se(VI) and Se(IV) were 0.02 μg L−1, 0.06 μg L−1, 0.2 μg L−1, 0.02 μg L−1, 0.2 μg L−1 and 0.4 μg L−1 respectively, which were obtained from 11 replicate measurements of blank. The stability of retention time and linearity of calibration curve were also evaluated. Relative standard deviations (RSD) of ≤9% for retention times (at least 20 replicate measurements) and correlation coefficients (R2) of ≥0.9998 for calibration curves (at least 6 replicate experiments) were obtained. Finally, the proposed method was applied to the analysis of one synthetic sample, two hot spring samples and two certified reference materials. The results showed a good spike recovery, indicating that basically no mass loss occurred during chromatographic separation. For two certified reference materials, the detected results were in good agreement with the certified values.