On-line removal of interferences via anion-exchange column separation for the determination of germanium, arsenic and selenium in biological samples by inductively coupled plasma mass spectrometry

On-line removal of interferences via anion-exchange column separation for the determination of germanium, arsenic and selenium in biological samples by inductively coupled plasma mass spectrometry
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电感耦合等离子体质谱法测定生物样品中的锗、砷和硒通过阴离子交换柱分离在线去除干扰

DOI:
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发表时间:
1996
期刊:
影响因子:
--
通讯作者:
Mo
Mo
中科院分区:
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文献类型:
--
作者:
F. Ko;Mo

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建立了微波消解-在线阴离子交换分离-电感耦合等离子体质谱法测定尿和血中锗、砷和硒的方法。样品经酸消解后,主要以H2 GeO 3、H3 AsO 3、H3 AsO 4、H2SeO 3和H2SeO 4的形式存在。分析物的分离是通过在相对碱性介质中将分析物作为阴离子物质吸附在柱上,随后在酸性介质中将分析物作为未解离的中性物质从柱上解吸来实现的。通过将调节至约pH 11.5的消化样品加载到在线分离系统的柱上,分析物以及可能在电感耦合等离子体质谱测定中引起光谱干扰的Cl和S被保留在柱上。在随后的洗脱步骤中,用pH约为1.6的洗脱液,分析物从柱上解吸,而Cl和S仍然保留。该系统可使~(72)Ge和~(75)As的测定分别不受~(35)Cl ~(37)Cl和~(40)Ar ~(35)Cl的干扰。通过以下建立的微波消解和在线分离过程中,锗,砷和硒的检出限分别低至0.07,0.13和0.3 ng ml-1,分别。通过分析市售尿液和全血标准品,评价了所提出方法的分析可靠性,发现所得结果与文献值相当吻合。
A method was developed for the determination by inductively coupled plasma mass spectrometry of germanium, arsenic and selenium in urine and blood after microwave acid digestion and on-line anion-exchange separation. After acid digestion, the analytes exist mainly as H2GeO3, H3AsO3, H3AsO4, H2SeO3 and H2SeO4 in the resulting sample solution. Separation of the analytes is achieved by adsorption of the analytes as anionic species on the column in relatively alkaline media with subsequent desorption of the analytes from the column as undissociated neutral species in acidic media. By loading the digested sample, adjusted to about pH 11.5, onto the column of the on-line separation system, the analytes as well as CI and S, which may cause spectral interference in the inductively coupled plasma mass spectrometric determination, are retained on the column. In the subsequent elution step with eluent of about pH 1.6, the analytes are desorbed from the column while Cl and S are still retained. With this on-line analytical system, the determination of 72Ge and 75As could be completely free from the interference caused by 35Cl37Cl and 40Ar35Cl, respectively. By following the established microwave digestion and on-line separation process, the detection limits obtained for Ge, As and Se were as low as 0.07, 0.13 and 0.3 ng ml–1, respectively. The analytical reliability of the proposed method was evaluated by analysing commercially available urine and whole blood standards, and the results obtained were found to be in reasonably good agreement with the literature values.
气动雾化和氢化物发生电感耦合等离子体质谱法用于硒同位素分析的比较。
DOI: 10.1021/ac00182a013
发表时间: 1989
影响因子: 7.4
作者:
Janghorbani,M;Ting,BT
通讯作者: Ting,BT