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验证一种用于测定人尿液中纳克级铍的标准化方法。

Validation of a standardised method for determining beryllium in human urine at nanogram level.

机构信息

Laboratory of Biological Monitoring of Inorganic Exposure, Department of Pollutants and Health, Institut National de Recherche et de Sécurité, Rue du Morvan, CS 60027, 54519, Vandoeuvre-les-Nancy, France,

出版信息

Anal Bioanal Chem. 2013 Oct;405(25):8327-36. doi: 10.1007/s00216-013-7220-7. Epub 2013 Jul 28.

Abstract

The potential toxicity of beryllium at low levels of exposure means that a biological and/or air monitoring strategy may be required to monitor the exposure of subjects. The main objective of the work presented in this manuscript was to develop and validate a sensitive and reproducible method for determining levels of beryllium in human urine and to establish reference values in workers and in non-occupationally exposed people. A chelate of beryllium acetylacetonate formed from beryllium(II) in human urine was pre-concentrated on a SPE C18 cartridge and eluted with methanol. After drying the eluate, the residue was solubilised in nitric acid and analysed by atomic absorption spectrometry and/or inductively coupled plasma mass spectrometry. The proposed method is 4 to 100 times more sensitive than other methods currently in routine use. The new method was validated with the concordance correlation coefficient test for beryllium concentrations ranging from 10 to 100 ng/L. Creatinine concentration, urine pH, interfering compounds and freeze-thaw cycles were found to have only slight effects on the performance of the method (less than 6%). The effectiveness of the two analytical techniques was compared statistically with each other and to direct analysis techniques. Even with a detection limit of 0.6 ng/L (obtained with inductively coupled plasma mass spectrometry), the method is not sensitive enough to detect levels in non-occupationally exposed persons. The method performance does however appear to be suitable for monitoring worker exposure in some industrial settings and it could therefore be of use in biological monitoring strategies.

摘要

铍在低水平暴露时具有潜在毒性,这意味着可能需要生物和/或空气监测策略来监测研究对象的暴露情况。本文介绍的工作的主要目的是开发和验证一种用于测定人尿中铍含量的灵敏且重现性好的方法,并建立工人和非职业暴露人群的参考值。用人尿中的铍(II)形成的乙酰丙酮合铍螯合物被预浓缩在 SPE C18 小柱上,然后用甲醇洗脱。洗脱液干燥后,残留物用硝酸溶解,并通过原子吸收光谱法和/或电感耦合等离子体质谱法进行分析。与目前常规使用的其他方法相比,该方法的灵敏度提高了 4 到 100 倍。使用 10 至 100ng/L 范围内的铍浓度进行了一致性相关系数测试,对新方法进行了验证。发现肌酐浓度、尿液 pH 值、干扰化合物和冻融循环对方法的性能只有轻微影响(小于 6%)。这两种分析技术的有效性通过统计学方法与彼此以及与直接分析技术进行了比较。即使检测限为 0.6ng/L(通过电感耦合等离子体质谱法获得),该方法的灵敏度也不足以检测非职业暴露人群的水平。然而,该方法的性能似乎适合于监测某些工业环境中的工人暴露情况,因此它可能对生物监测策略有用。

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