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目的快速测定人体尿液中痕量铀元素的可行性。方法首先对高纯水和高纯硝酸进行再蒸馏,使其本底铀元素含量降低约30%,提高了测定的精度;再次,采用微波消解法处理尿液样品,消除其中的有机物等杂质,优化各项仪器参数消除质谱干扰。在0.0005~0.008、0.01~0.08μg·L~(-1)两段浓度范围内做标准曲线。对检出限及回收率进行研究;最后通过采集某核设施周边16个成年人的实际尿液样品,用高分辨电感耦合等离子体质谱法(HR-ICPMS)快速测定。该方法检出限为1.41×10~(-4)μg·L~(-1),定量限为4.71×10~(-4)μg·L~(-1),平均回收率为94.9%~101.2%,相对标准不确定度为0.019%。结果人体尿液痕量铀平均值为0.024μg·L~(-1),与国内外文献记录值相当。结论高分辨电感耦合等离子体质谱法(HR-ICP-MS)快速测定尿液中痕量铀元素的方法可行、可靠。
Objective To determine the feasibility of rapid determination of trace amounts of uranium in human urine. The method first re-distills high purity water and high purity nitric acid to reduce the content of uranium in its background by about 30%, and improves the precision of the determination. Thirdly, the urine sample is treated by microwave digestion to eliminate impurities such as organic matter, Instrument parameters to eliminate interference with mass spectrometry. The calibration curves were made in the range of 0.0005 ~ 0.008,0.01 ~ 0.08μg · L ~ (-1). The detection limits and recoveries were studied. Finally, actual urine samples from 16 adults around a nuclear facility were collected and rapidly determined by HR-ICPMS. The detection limit was 1.41 × 10 -4 μg · L -1, and the limit of quantification was 4.71 × 10 -4 μg · L -1 .The average recovery was 94.9% 101.2%, the relative standard uncertainty is 0.019%. Results The average urinary trace uranium in human urine was 0.024 μg · L ~ (-1), which was comparable with the documented data at home and abroad. Conclusion High-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS) for rapid determination of trace amounts of uranium in urine is feasible and reliable.