Todorovska Nadica, Karadjova Irina, Stafilov Trajce
Institute of Preventive Medical Care and Toxicology, Military Health Institution Center, 1000 Skopje, Macedonia.
Anal Bioanal Chem. 2002 Jul;373(4-5):310-3. doi: 10.1007/s00216-002-1328-5. Epub 2002 May 23.
Methods for the direct determination of Ni in human blood serum and urine by electrothermal atomic absorption spectrometry (ETAAS) are described. Hydrogen peroxide was proposed as matrix modifier, assisting thermal decomposition of proteins during the ashing step. A pyrolysis temperature of 1,200 degrees C was found to be optimal while 2,100 degrees C and 2,200 degrees C were found to be optimal atomizing temperatures for Ni in serum and urine respectively. Calibration was performed by using a calibration curve prepared with aqueous standard solutions of Ni (glycine must be used as modifier for Ni in aqueous solutions). The limits of detection, defined as the blank values plus 3 times the standard deviation of the blank values, were 0.2 microg/L for both serum and urine samples. Relative standard deviations for serum samples with concentrations of Ni in the range 0.5-2 microg/L were 10-15% and for urine samples with Ni concentrations in the range 0.5-2.5 microg/L were 8-10%.
描述了用电热原子吸收光谱法(ETAAS)直接测定人血清和尿液中镍的方法。提出用过氧化氢作为基体改进剂,在灰化步骤中辅助蛋白质的热分解。发现1200℃的热解温度是最佳的,而2100℃和2200℃分别是血清和尿液中镍的最佳原子化温度。通过使用由镍的水溶液标准溶液制备的校准曲线进行校准(在水溶液中必须使用甘氨酸作为镍的改进剂)。检测限定义为空白值加上空白值标准偏差的3倍,血清和尿液样品的检测限均为0.2μg/L。镍浓度在0.5 - 2μg/L范围内的血清样品的相对标准偏差为10 - 15%,镍浓度在0.5 - 2.5μg/L范围内的尿液样品的相对标准偏差为8 - 10%。