Shahtaheri S J, Khadem M, Golbabaei F, Rahimi-Froushani A
Department of Occupational Health, Tehran University of Medical Sciences, Iran.
Anal Chem Insights. 2007 Dec 11;2:125-32.
Chromium is an important constituent widely used in different industrial processes for production of various synthetic materials. For evaluation of workers' exposure to trace toxic metal of Cr (III), environmental and biological monitoring are essential processes, in which, preparation of samples is one of the most time-consuming and error-prone aspects prior to analysis. The use of solid-phase extraction (SPE) has grown and is a fertile technique of sample preparation as it provides better results than those produced by liquid-liquid extraction (LLE). SPE using mini columns filled with XAD-4 resin was optimized regarding to sample pH, ligand concentration, loading flow rate, elution solvent, sample volume, elution volume, amount of resins, and sample matrix interferences. Chromium was retained on solid sorbent and was eluted with 2 M HNO(3) followed by simple determination of analytes by using flame atomic absorption spectrometry. Obtained recoveries of metal ion were more than 92%. The optimized procedure was also validated with three different pools of spiked urine samples and showed a good reproducibility over six consecutive days as well as six within-day experiments. Through this study, suitable results were obtained for relative standard deviation, therefore, it is concluded that, this optimized method can be considered to be successful in simplifying sample preparation for trace residue analysis of Cr in different matrices for evaluation of occupational and environmental exposures. To evaluate occupational exposure to chromium, 16 urine samples were taken, prepared, and analyzed based on optimized procedure.
铬是一种重要成分,广泛应用于不同工业生产各种合成材料的过程中。为评估工人对痕量有毒金属铬(III)的接触情况,环境和生物监测是必不可少的过程,其中,样品制备是分析前最耗时且最容易出错的环节之一。固相萃取(SPE)的应用不断增加,是一种有效的样品制备技术,因为它比液液萃取(LLE)能提供更好的结果。使用填充有XAD - 4树脂的微型柱的固相萃取在样品pH值、配体浓度、上样流速、洗脱溶剂、样品体积、洗脱体积、树脂量和样品基质干扰方面进行了优化。铬保留在固体吸附剂上,用2 M硝酸洗脱,然后通过火焰原子吸收光谱法简单测定分析物。金属离子的回收率超过92%。优化后的程序还用三种不同的加标尿样池进行了验证,在连续六天以及六次日内实验中均显示出良好的重现性。通过这项研究,获得了相对标准偏差的合适结果,因此得出结论,这种优化方法可被认为成功简化了不同基质中铬痕量残留分析的样品制备,用于评估职业和环境暴露。为评估职业性铬暴露情况,采集了16份尿样,按照优化程序进行制备和分析。