Vanderpool R A, Buckley W T
Grand Forks Human Nutrition Research Center, United States Department of Agriculture, Grand Forks, North Dakota 58203, USA.
Anal Chem. 1999 Feb 1;71(3):652-9. doi: 10.1021/ac980538b.
A published procedure for the liquid-liquid extraction of Cd by sodium diethyldithiocarbamate (NaDDC) was modified and tested on 12 biological matrixes of plant and animal origin for use with isotope dilution (ID) inductively coupled plasma mass spectrometry (ICPMS). The tested matrixes were reference materials, certified for Cd, and a feces in-house standard. The digested and extracted standards were analyzed for Cd stable isotopes by ICPMS and the resulting isotope ratios examined for isobaric and polyatomic interferences. Cadmium recoveries, after extraction, ranged from 73% to 20% and apparently were inversely related to Cd concentration, even in the presence of excess chelator. For each reference material, the measured isotope ratios for Cd were corrected for instrumental bias and compared to natural abundance Cd isotope ratios. Nonextracted samples had large isotope ratio deviations for all but one or two ratios. Extraction improved all the isotope ratios measured (lowered % error relative to natural abundances), but interferences were noted for a few samples. The extracted human in-house feces standard was found to have Sn signals reduced by 300-fold, but residual Sn concentrations still interfered with 116Cd, though not 112Cd or 114Cd. Thus, evaluation of the NADDC-extracted in-house fecal standard and reference materials indicate the successful removal of interferences that otherwise prevented accurate determinations of Cd by IDICPMS and show that a number of Cd isotope ratios could be accurately measured (< 1.5% error) for multiple stable isotope tracer studies in a broad range of NaDDC-extracted biological matrixes.
已发表的二乙基二硫代氨基甲酸钠(NaDDC)液液萃取镉的方法经过改进,并在12种动植物来源的生物基质上进行了测试,用于同位素稀释(ID)电感耦合等离子体质谱(ICPMS)分析。测试的基质包括经镉认证的参考物质和一种粪便内部标准物质。对消化和萃取后的标准物质进行ICPMS分析,测定镉稳定同位素,并检查所得同位素比值是否存在同量异位素和多原子干扰。萃取后镉的回收率在73%至20%之间,即使在存在过量螯合剂的情况下,回收率显然也与镉浓度呈负相关。对于每种参考物质,测量得到的镉同位素比值经过仪器偏差校正后,与天然丰度镉同位素比值进行比较。除了一两个比值外,未萃取的样品所有同位素比值都有较大偏差。萃取改善了所有测量的同位素比值(相对于天然丰度降低了误差百分比),但有少数样品存在干扰。发现萃取后的人类粪便内部标准物质中锡信号降低了300倍,但残留的锡浓度仍对116Cd有干扰,不过对112Cd或114Cd没有干扰。因此,对NaDDC萃取的粪便内部标准物质和参考物质的评估表明,成功消除了原本会妨碍通过ID-ICPMS准确测定镉的干扰,并表明在广泛的NaDDC萃取生物基质中,对于多种稳定同位素示踪研究,可以准确测量多个镉同位素比值(误差<1.5%)。