A simple method for methylmercury, inorganic mercury and ethylmercury determination in plasma samples by high performance liquid chromatography-cold-vapor-inductively coupled plasma mass spectrometry

被引:73
作者
de Souza, Samuel S. [1 ]
Campiglia, Andres Dobal [2 ]
Barbosa, Fernando, Jr. [1 ]
机构
[1] Univ Sao Paulo, Fac Ciencias Farmaceut Ribeirao Preto, Lab Toxicol & Essencialidade Met, BR-14049 Ribeirao Preto, SP, Brazil
[2] Univ Cent Florida, Dept Chem, Orlando, FL 32816 USA
基金
巴西圣保罗研究基金会;
关键词
ICP-MS; Speciation; Plasma; Mercury; Sample preparation; Liquid chromatography; BIOLOGICAL SAMPLES; ATOMIC SPECTROMETRY; FORMIC-ACID; WHOLE-BLOOD; GENERATION; SOLUBILIZATION; POLYMORPHISMS; SPECIATION; EXPOSURE; CADMIUM;
D O I
10.1016/j.aca.2012.11.038
中图分类号
O65 [分析化学];
学科分类号
070302 [分析化学];
摘要
A simple and sensitive method with a fast sample preparation procedure is proposed for the determination of mercury species in plasma/serum. The method combines online high-performance liquid chromatography separation, Hg cold-vapor formation and inductively coupled plasma mass spectrometry detection. Prior to analysis, plasma (250 mu L) was accurately pipetted into 15 mL conical tubes. Then, an extractant solution containing mercaptoethanol, L-cysteine and HCl was added to the samples following sonication for 10 min. Quantitative mercury extraction was achieved with the proposed procedure. Separation of mercury species was accomplished in less than 8 min on a C8 reverse phase column with a mobile phase containing 3% v/v methanol + 97% v/v (0.5% v/v 2-mercaptoethanol + 0.05% v/v formic acid). The method detection limits were found to be 12 ng L-1, 5 ng L-1 and 4 ng L-1 for inorganic mercury, ethylmercury and methylmercury, respectively. Method accuracy is traceable to Standard Reference Material (SRM) 966 Toxic Metals in Bovine Blood from NIST. Additional validation was provided by the analysis of a secondary reference serum sample from the INSQ-Canada. Finally, the method was successfully applied for the speciation of mercury in plasma samples collected from volunteers exposed to methylmercury through fish consumption. For the first time to our knowledge, levels of different species of Hg in plasma samples from riverside populations exposed to MeHg were determined. (C) 2012 Elsevier B.V. All rights reserved.
引用
收藏
页码:11 / 17
页数:7
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