Key Laboratory of Green Chemistry & Technology, Ministry of Education, College of Chemistry, Sichuan University, Chengdu, Sichuan 610064, China.
Analyst. 2013 Jun 21;138(12):3494-501. doi: 10.1039/c3an00010a. Epub 2013 May 13.
A novel, green and efficient post-column oxidation method using Fe(3)O(4) magnetic nanoparticles (MNPs) was developed to on-line convert hydride generation/cold vapor generation (HG/CV) inactive species to their active species without microwave/UV irradiation. It was applied to high performance liquid chromatography HG/CV atomic fluorescence spectrometry (HPLC-HG/CV-AFS) to enable sensitive speciation analysis of both HG/CV inactive and active species. Inorganic mercury (Hg(2+)), methylmercury (MeHg), ethylmercury (EtHg) and phenylmercury (PhHg) were selected as model compounds to validate the methodology. Separation of these mercury species was accomplished on a RP-C18 column with a mixture of acetonitrile and water (10 : 90) at pH 6.8 containing 0.12% (m/v) L-cysteine as the mobile phase. In the presence of 0.6% (v/v) H(2)O(2), on-line conversion of the organomercury species eluted from the HPLC column to Hg(2+) was obtained using the advanced oxidation method at pH 2.0. Optimum conditions for the separation, oxidation and cold vapor generation were carefully investigated. The limits of detection (LODs) were 0.7, 1.1, 0.8 and 0.9 μg L(-1) (as Hg) for Hg(2+), MeHg, EtHg and PhHg, respectively, corresponding to 14, 22, 16 and 18 pg absolute detection limits for Hg(2+), MeHg, EtHg and PhHg by using a 20 μL sample loop, which are comparable to or better than those previously reported. National Research Council Canada DORM-2 fish muscle tissue and several real water samples were analyzed to validate the accuracy of the proposed method.
一种新颖、绿色、高效的柱后氧化方法，使用 Fe(3)O(4)磁性纳米粒子（MNPs），无需微波/UV 照射，即可将氢化物发生/冷蒸气发生（HG/CV）的非活性物质在线转化为其活性物质。该方法应用于高效液相色谱 HG/CV 原子荧光光谱法（HPLC-HG/CV-AFS），实现了 HG/CV 非活性和活性物质的灵敏形态分析。选择无机汞（Hg(2+)）、甲基汞（MeHg）、乙基汞（EtHg）和苯基汞（PhHg）作为模型化合物验证该方法。这些汞形态的分离是在 pH 6.8 的含有 0.12%（m/v）L-半胱氨酸的乙腈和水（10:90）的混合液作为流动相的 RP-C18 柱上完成的。在 0.6%（v/v）H(2)O(2)存在下，使用先进的氧化方法在 pH 2.0 下，在线将从 HPLC 柱洗脱的有机汞物种转化为 Hg(2+)。仔细研究了分离、氧化和冷蒸气生成的最佳条件。Hg(2+)、MeHg、EtHg 和 PhHg 的检出限（LOD）分别为 0.7、1.1、0.8 和 0.9 μg L(-1)（以 Hg 计），对应于使用 20 μL 进样环时 Hg(2+)、MeHg、EtHg 和 PhHg 的绝对检出限分别为 14、22、16 和 18 pg，与之前报道的结果相当或更好。对加拿大国家研究委员会 DORM-2 鱼肉组织和几种实际水样进行了分析，以验证该方法的准确性。
