直接稀释电感耦合等离子体质谱测定尿中汞

葛成相; 李四生; 宋晓琼; 李建伟; 李昌安; 单晓梅

doi:10.13421/j.cnki.hjwsxzz.2022.05.007

直接稀释电感耦合等离子体质谱测定尿中汞

Determination of mercury in urine by ICP-MS with direct dilution

摘要

摘要:
目的改进尿中汞含量电感耦合等离子体质谱(ICP-MS)测定方法。
方法采用200 μg/L Au⁺-5%硝酸溶液直接稀释尿样, 铋(²⁰⁹ Bi)为内标, Au⁺溶液克服汞记忆效应, ICP-MS进行测定。
结果汞浓度在(0.00-2.00)μg/L范围内线性相关系数r为0.999 4, 最低检出浓度为0.012 μg/L, 汞高、中、低三种浓度平均加标回收率分别为105.8%、102.0%和100.3%, 日内精密度相对标准偏差(RSD)小于5.97%, 日间精密度RSD为1.55%~4.84%。常见干扰元素对测定无干扰。尿样在常温、冷藏、冷冻和低温条件下均可稳定3天。
结论本研究改进尿中汞的ICP-MS测定方法具有快速、准确、灵敏度、重现性好等优点, 适用于尿液中汞含量测定。

Abstract:
Objective To modify the method of inductively coupled plasma mass spectrometry (ICP-MS) for the determination of mercury in urine.
Methods Urine samples were directed diluted with 200 μg/L Au⁺-5% HNO₃ solution, and the mercury content in urine was analyzed by ICP-MS using bismuth (²⁰⁹Bi) as an internal standard and Au⁺ solution to eliminate the mercury memory effect.
Results Mercury concentration had a linear correlation coefficient r of 0.9994 within the range of 0.00-2.00 μg/L, and the minimum detectable concentration was 0.012 μg/L. The high, medium and low mass concentrations of mercury had an average spiked recovery of 105.8%, 102.0% and 100.3%, respectively. The relative standard deviation (RSD) of intra-day precision was below 5.97%, and the RSD of inter-day precision was 1.55%-4.84%. Common interfering elements did not interfere with the determination, and urine samples remained stable for 3 days at room temperature and under refrigerated, frozen, and cryogenic conditions.
Conclusion The modified method is rapid and accurate with good sensitivity and repeatability, and it is suitable for the determination of mercury in urine.

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