Aggarwal S K, Kinter M, Herold D A
Department of Pathology, University of Virginia Health Sciences Center, Charlottesville 22908.
J Chromatogr. 1992 May 8;576(2):297-304. doi: 10.1016/0378-4347(92)80203-3.
A gas chromatographic-mass spectrometric method for the determination of cobalt in biological materials employing stable enriched 62Ni as an internal standard and using lithium bis(trifluoroethyl)dithiocarbamate as a chelating agent is described. The method involves the addition of a known amount (1 microgram) of 62Ni to the sample, the formation of the chelate and the determination by selected-ion monitoring of the m/z 571/574 ratio, which corresponds to 59Co/62Ni. No appreciable memory effect was observed, and an acceptable dynamic range of 100 was found. There was good agreement between the cobalt concentration values determined by gas chromatography-mass spectrometry and electrothermal atomic absorption spectrometry. The present method has high sensitivity and can be used for the quantitation of cobalt at concentrations as low as 1 microgram/l. The use of enriched 62Ni circumvents the problem caused by endogenous nickel and simultaneously provides data on the nickel concentration in the biological sample without any additional experimental effort.
描述了一种气相色谱 - 质谱法，用于测定生物材料中的钴，该方法采用稳定富集的(^{62}Ni)作为内标，并使用双（三氟乙基）二硫代碳酸锂作为螯合剂。该方法包括向样品中加入已知量（(1)微克）的(^{62}Ni)，形成螯合物，并通过选择离子监测(m/z 571/574)的比率进行测定，该比率对应于(^{59}Co/^{62}Ni)。未观察到明显的记忆效应，并且发现了(100)的可接受动态范围。气相色谱 - 质谱法和电热原子吸收光谱法测定的钴浓度值之间具有良好的一致性。本方法具有高灵敏度，可用于低至(1)微克/升浓度的钴的定量分析。使用富集的(^{62}Ni)避免了内源性镍引起的问题，同时无需任何额外的实验工作即可提供生物样品中镍浓度的数据。
