Scancar J, Milacic R, Benedik M, Bukovec P
Department of Environmental Sciences, Jozef Stefan Institute, Jamova 39, 1000, Ljubljana, Slovenia.
Clin Chim Acta. 2000 Mar;293(1-2):187-97. doi: 10.1016/s0009-8981(99)00239-9.
A rapid and reliable analytical method for the determination of trace elements in human bone by atomic absorption spectrometry is reported. Calcium was determined to estimate the homogeneity of samples. Human bone from the iliac crest was obtained at autopsy of adult subjects. Before analysis samples were decomposed by microwave digestion and acid digestion in a Parr bomb. Zinc, rubidium, strontium, calcium and iron were determined by flame atomic absorption spectrometry (FAAS) and aluminium, copper and lead by electrothermal atomic absorption spectrometry (ETAAS) at optimum measurement conditions. The results for the two digestion procedures agreed for zinc, rubidium and calcium within +/-5%, for copper within +/-7% and for strontium, iron, aluminium and lead within +/-10%. The repeatability of measurement (R.S.D.) for determination of calcium and trace elements after microwave digestion and acid digestion in a Parr bomb was tested in one representative autopsy bone sample by six parallel determinations. It was found to be better than +/-5% either for microwave digested samples or samples digested in a Parr bomb, for all elements determined by FAAS and ETAAS techniques. The accuracy of the applied digestion procedures was checked by analysis of trace elements in NIST SRM 1486 Bone Meal reference material. Good agreement of the results with certified values was obtained for both digestion procedures. The microwave procedure developed for digestion of small amounts of sample was applied in trace elements analysis of bone biopsy samples from dialysis patients.
报道了一种通过原子吸收光谱法测定人骨中微量元素的快速可靠分析方法。测定钙以评估样品的均匀性。成年受试者尸检时获取髂嵴处的人骨。分析前,样品通过微波消解和在帕尔弹中进行酸消解进行分解。在最佳测量条件下,采用火焰原子吸收光谱法(FAAS)测定锌、铷、锶、钙和铁,采用电热原子吸收光谱法(ETAAS)测定铝、铜和铅。两种消解方法的结果在锌、铷和钙方面的偏差在±5%以内,铜在±7%以内,锶、铁、铝和铅在±10%以内。通过对一个有代表性的尸检骨样品进行六次平行测定,测试了微波消解和在帕尔弹中酸消解后钙和微量元素测定的测量重复性(相对标准偏差,R.S.D.)。结果发现,对于通过FAAS和ETAAS技术测定的所有元素,无论是微波消解样品还是在帕尔弹中消解的样品,其重复性均优于±5%。通过分析NIST SRM 1486骨粉标准物质中的微量元素,检验了所采用消解方法的准确性。两种消解方法的结果与认证值均吻合良好。所开发的用于消解少量样品的微波方法应用于透析患者骨活检样品的微量元素分析。