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头发中汞的形态分析 - 顶空注射-气相色谱-原子荧光光谱法(甲基汞)和燃烧-原子吸收光谱法(总汞)。

Mercury speciation in hair by headspace injection-gas chromatography-atomic fluorescence spectrometry (methylmercury) and combustion-atomic absorption spectrometry (total Hg).

机构信息

Analytical and Environmental Chemistry Department (ANCH), Vrije Universiteit Brussel (VUB), Pleinlaan 2, 1050 Brussel, Belgium.

出版信息

Talanta. 2010 Oct 15;82(5):1919-23. doi: 10.1016/j.talanta.2010.08.012. Epub 2010 Aug 17.

Abstract

The speciation of Hg in human hair was carried out with combustion-atomic absorption spectrometry for total Hg (THg) and headspace-gas chromatography-atomic fluorescence spectrometry (HS-GC-AFS) for methylmercury (MMHg). The determination of total Hg in hair was carried out with the AMA analyzer (Advanced Mercury Analyser 254). Accuracy and reproducibility were assessed on a Certified Reference hair sample (IAEA-086 CRM), yielding, respectively, a recovery of 97.5% and a RSD of 3.2%. Analyses of 10 blank measurements resulted in a detection limit of 1.5 ng g(-1) of THg for a 20mg sample of human hair. MMHg concentrations in hair were assessed with HS-GC-AFS in a single analysis step. Either acid or alkaline extraction can be applied because they yielded very similar results on a IAEA-086 CRM: we observed a recovery of 103% and a RSD of 7% with acid extraction and a recovery of 110% and a RSD of 9% with alkaline extraction. Optimization of the headspace vial, injection and GC parameters is described. The detection limit of the MMHg determination in human hair, which amounts to 0.04 ng g(-1) for a 20mg sample, is far below the concentrations observed in natural samples. The number of samples that can be analyzed per hour, respectively, amounts to 8 for THg and 4 for MMHg. Finally, Hg speciation in natural human hair samples was carried out by combining both AMA and HS-GC-AFS analysis methods. THg levels were at the μg g(-1), level, with an average MMHg fraction of about 70%.

摘要

采用燃烧-原子吸收光谱法(C-AAS)测定总汞(THg),采用顶空-气相色谱-原子荧光光谱法(HS-GC-AFS)测定甲基汞(MMHg),对人发中的汞形态进行了研究。总汞的测定采用 AMA 分析仪(高级汞分析仪 254)进行。在认证参考头发样品(IAEA-086 CRM)上评估了准确度和重现性,分别得到 97.5%的回收率和 3.2%的 RSD。对 10 个空白测量的分析得出,对于 20mg 人发样品,THg 的检测限为 1.5ng g(-1)。采用 HS-GC-AFS 可在单个分析步骤中评估头发中的 MMHg 浓度。可以应用酸或碱提取,因为它们在 IAEA-086 CRM 上得到非常相似的结果:我们观察到酸提取的回收率为 103%,RSD 为 7%,碱提取的回收率为 110%,RSD 为 9%。描述了顶空瓶、进样和 GC 参数的优化。对于 20mg 样品,MMHg 测定的检测限为 0.04ng g(-1),远低于天然样品中观察到的浓度。分别可分析的样品数,THg 为 8 个,MMHg 为 4 个。最后,通过结合 AMA 和 HS-GC-AFS 分析方法对天然人发样品中的汞形态进行了研究。THg 水平在μg g(-1)水平,平均 MMHg 分数约为 70%。

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