Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University, Wuhan 430072, Hubei Province, PR China.
Talanta. 2010 Apr 15;81(1-2):578-85. doi: 10.1016/j.talanta.2009.12.034. Epub 2010 Jan 4.
A new, simple and sensitive method by combining headspace Pd(II)-coated graphite bar microextraction (GBME) with electrothermal vaporization-inductively coupled plasma mass spectrometry (ETV-ICP-MS) was developed for the determination of trace Se, Te and Bi in seawater and human hair. In this method, the graphite bar was coated with Pd(II) and then used for headspace trapping of the hydrides of Se(IV), Te(IV) and Bi(III). The graphite bar with enriched hydrides of analytes was inserted directly into the graphite tube and subsequently determined by ETV-ICP-MS according to the established temperature program. The experimental parameters, which may affect the extraction and vaporization of target analytes, were systematically investigated and the optimal experimental conditions were established. Under the optimal conditions, the detection limits of the method were 8.6, 2.6 and 0.2 ng l(-1) and the relative standard deviations (RSDs) were 7.0%, 6.2% and 8.0% (C=0.20 microg l(-1), n=7) for Se, Te and Bi, respectively. Linearity was obtained over the range of 0.05-20.00, 0.01-5.00 and 0.01-20.00 microg l(-1) with the correlation coefficients of 0.9942, 0.9997 and 0.9976 for Se, Te and Bi, respectively. The proposed method was successfully applied for the determination of trace Se, Te and Bi in seawater and human hair samples. In order to validate the method, the proposed method has also been applied for the determination of trace Se, Te and Bi in the certified material of GBW07601 human hair, and the determined values were in good agreement with the certified values.
建立了一种新的、简单而灵敏的方法,将顶空 Pd(II)涂覆石墨棒微萃取(GBME)与电热蒸发-电感耦合等离子体质谱(ETV-ICP-MS)相结合,用于测定海水中痕量硒、碲和铋。在该方法中,石墨棒涂覆 Pd(II),然后用于氢化物的顶空捕集硒(IV)、碲(IV)和铋(III)。富集有分析物的氢化物的石墨棒直接插入石墨管中,然后根据建立的温度程序通过 ETV-ICP-MS 进行测定。系统研究了可能影响目标分析物萃取和蒸发的实验参数,并确定了最佳实验条件。在最佳条件下,该方法的检出限分别为 8.6、2.6 和 0.2ngL-1,相对标准偏差(RSD)分别为 7.0%、6.2%和 8.0%(C=0.20μgL-1,n=7)。硒、碲和铋的线性范围分别为 0.05-20.00、0.01-5.00 和 0.01-20.00μgL-1,相关系数分别为 0.9942、0.9997 和 0.9976。该方法成功应用于海水和人发样品中痕量硒、碲和铋的测定。为了验证该方法,还将其应用于 GBW07601 人发标准物质中痕量硒、碲和铋的测定,测定值与标准值吻合良好。