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目的研究以胶体钯作为基体改进剂在石墨炉原子吸收光谱法测定全血中铅、镉、锰的应用效果。方法用血样稀释剂将全血样品稀释10倍后,以胶体钯为基体改进剂,优化待测元素的灰化和原子化温度后,以石墨炉原子吸收光谱仪检测全血中铅、镉、锰水平,并与普通钯盐作为基体改进剂的应用效果进行比较。结果胶体钯作为基体改进剂的最佳用量为5.00μL;其可将全血中铅、镉、锰的灰化温度分别提高至900、800和1 400℃,将原子化温度分别提高至1 900、1 800和2 000℃;与普通钯盐比较,胶体钯使3种待测元素有更宽的灰化和原子化温度范围。本方法全血中铅、镉、锰分别在质量浓度0.12~100.00、0.05~4.00和0.02~10.00μg/L呈良好线性关系,相关系数均大于0.999;最低检出浓度分别为1.20、0.50和0.20μg/L(以样品稀释10倍计);平均加标回收率分别为99.2%~104.0%、102.8%~105.5%和98.3%~103.2%;批内相对标准偏差(RSD)分别为1.2%~2.6%、2.7%~5.3%和2.3%~2.8%,批间RSD分别为1.6%~3.9%、4.0%~6.1%和3.2%~4.4%。结论胶体钯用于测定全血中的铅、镉、锰,背景干扰小,有利于改善检测的精密度和灵敏度,是一种优良的基体改进剂。
Objective To study the application of colloidal palladium as matrix modifier in the determination of lead, cadmium and manganese in whole blood by graphite furnace atomic absorption spectrometry. Methods Blood samples were diluted 10-fold with blood thinner to determine the ashing and atomization temperature of the tested elements with colloidal palladium as the matrix modifier. The contents of lead, cadmium and manganese in the whole blood were determined by graphite furnace atomic absorption spectrometry Level, and with the ordinary palladium salt as a matrix modifier application effect comparison. Results The optimal dosage of colloidal palladium as matrix modifier was 5.00 μL. The ashing temperature of lead, cadmium and manganese in whole blood were increased to 900,800 and 1400 ℃, respectively, and the atomization temperature increased to 1 900 , 1800 and 2000 ℃. Compared with the common palladium salts, the colloidal palladium made the three kinds of analytes have a wider ashing and atomization temperature range. The method of the whole blood lead, cadmium and manganese in the mass concentration of 0.12 ~ 100.00,0.05 ~ 4.00 and 0.02 ~ 10.00μg / L showed a good linear relationship, the correlation coefficient was greater than 0.999; minimum detectable concentrations were 1.20,0.50 and 0.20 μg / L diluted 10 times of the sample. The average recoveries were 99.2% -104.0%, 102.8% -105.5% and 98.3% -103.2%, respectively. The relative standard deviations (RSDs) within the batch were 1.2% 2.6%, 2.7% -5.3% and 2.3% -2.8%, respectively. The inter-assay RSD was 1.6% -3.9%, 4.0% -6.1% and 3.2% -4.4% respectively. Conclusion Colloidal palladium is an excellent matrix modifier for the determination of lead, cadmium and manganese in whole blood with small background interference and is conducive to improving the precision and sensitivity of detection.