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低温电热蒸发电感耦合等离子体质谱联用技术用于环境和生物样品中痕量元素分析前的中空纤维液相微萃取

Hollow-fiber liquid-phase microextraction prior to low-temperature electrothermal vaporization ICP-MS for trace element analysis in environmental and biological samples.

作者信息

Xia Linbo, Wu Yunli, Hu Bin

机构信息

Department of Chemistry, Wuhan University, Wuhan 430072, PR China.

出版信息

J Mass Spectrom. 2007 Jun;42(6):803-10. doi: 10.1002/jms.1216.

Abstract

A new method of hollow-fiber liquid-phase microextraction (HF-LPME) prior to electrothermal vaporization (ETV) inductively coupled plasma mass spectrometry (ICP-MS) determination of trace Cu, Zn, Pd, Cd, Hg, Pb and Bi, based on gaseous compounds introduction into the plasma as their diethyldithiocarbmate (DDTC) chelates, was developed. The use of the reagent DDTC as chemical modifier could not only enhance the analytical signals, but also decrease the vaporization temperature. At a temperature of 1300 degrees C, trace Cu, Zn, Pd, Cd, Hg, Pb and Bi can be vaporized completely into the ICP. The factors affecting the formation of the chelates and their vaporization behaviors were investigated in detail, and the microextraction conditions were optimized. Under the optimized conditions, the detection limits of the proposed method were 12.4, 28.7, 7.9, 4.5, 3.3, 4.8 and 1.6 pg ml(-1) for Cu, Zn, Pd, Cd, Hg, Pb and Bi, respectively. Enrichment factors of 305, 284, 24, 29, 20, 73 and 43 could be achieved within 15 min of extraction time, and the relative standard deviations (RSDs) for the seven determinations of 0.5 ng ml(-1) of target analytes were 8.8, 6.9, 7.1, 9.4, 10.2, 6.1 and 10.8%, respectively. The newly developed method has been applied to the determination of trace Cu, Zn, Pd, Cd, Hg, Pb and Bi in environmental water and human serum samples, and the recoveries for the spiked samples were in the range of 88-116%. In order to validate this method, two certified reference materials, GBW08501 peach leaves and GBW(E)080040 seawater, were analyzed, and the determined values were in good agreement with the certified values.

摘要

建立了一种基于二乙基二硫代氨基甲酸盐(DDTC)螯合物将气态化合物引入等离子体的电热蒸发(ETV)电感耦合等离子体质谱(ICP-MS)测定痕量铜、锌、钯、镉、汞、铅和铋之前的中空纤维液相微萃取(HF-LPME)新方法。使用试剂DDTC作为化学改性剂不仅可以增强分析信号,还可以降低蒸发温度。在1300℃的温度下,痕量铜、锌、钯、镉、汞、铅和铋可以完全蒸发进入ICP。详细研究了影响螯合物形成及其蒸发行为的因素,并优化了微萃取条件。在优化条件下,该方法对铜、锌、钯、镉、汞、铅和铋的检测限分别为12.4、28.7、7.9、4.5、3.3、4.8和1.6 pg ml⁻¹。在15分钟的萃取时间内,富集因子可达305、284、24、29、20、73和43,对0.5 ng ml⁻¹目标分析物进行七次测定的相对标准偏差(RSD)分别为8.8%、6.9%、7.1%、9.4%、10.2%、6.1%和10.8%。新开发的方法已应用于环境水和人血清样品中痕量铜、锌、钯、镉、汞、铅和铋的测定,加标样品的回收率在88-116%范围内。为了验证该方法,分析了两种有证标准物质GBW08501桃叶和GBW(E)080040海水,测定值与认定值吻合良好。

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