酸性溴酸钾/溴化钾消解原子荧光法测定尿汞
Acidic Potassium Bromate/Potassium Bromide Digestion System for Determination of Total Mercury in Urine Using Atomic Fluorescence Spectrometry
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摘要:
目的 研究不同的尿样消解方法,寻求一种快速、准确、高通量的适用于样品量大的职业性人群尿汞测定方法。 方法 采用微波消解法、低温高锰酸钾氧化法及酸性溴酸钾/溴化钾氧化法在一定的条件下处理尿样,比较3种方法的准确度、精密度、灵敏度、回收率以及检测时间。 结果 微波消解法与酸性溴酸钾/溴化钾氧化法测定尿汞含量吻合。两种方法相对标准偏差分别为2.4%、1.7%;加标回收率分别为101.5%~112.2%及105.5%~110.0%;样品前处理耗时分别为6 h、15 min。低温高锰酸钾氧化法测定尿汞结果偏高,加标回收率约为130%。采用酸性溴酸钾/溴化钾氧化法测定冻干人尿汞质控样品,结果与标准值吻合性良好。 结论 本研究比较3种尿汞样品消解方法,结果表明以酸性溴酸钾/溴化钾氧化法较为新颖、准确、高效、快速,适合大批量职业性人群尿汞的简便快速测定。 Abstract:Objective To find a rapid, precise, and high-throughput method for the determination of total urine mercury levels of occupational population by comparing several pretreatment methods of urine samples. Methods Three pretreatment methods including microwave digestion, constant-temperature potassium permanganate oxidation, and acidic potassium bromatepotassium bromide (KBrO3/KBr) digestion system were applied under optimal conditions. Parameters of method performance such as accuracy, precision, sensitivity, recovery, and time for detection were compared. Results The results of microwave digestion and KBrO3/KBr digestion system were in excellent agreement. The spiked recovery rates of the two methods were in the range of 101.5%-112.2% and 105.5%-110.0%, with relative standard deviations of 2.4% and 1.7%, respectively. The pretreatment time of the two methods was 6 h and 15 min, respectively. In addition, the results by constant-temperature potassium permanganate oxidation method were on the higher side with spiked recovery rate about 130%. Certified reference samples of lyophilized urine were used to validate the KBrO3/KBr digestion method and the results were in good agreement with the reference values. Conclusion Acidic KBrO3/KBr digestion method is precise, efficient and rapid for the determination of total mercury in batches of urine samples of occupational population.
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