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Dithizone-functionalized solid phase extraction-displacement elution-high performance liquid chromatography-inductively coupled plasma mass spectrometry for mercury speciation in water samples

机译:双硫i功能化固相萃取-置换洗脱-高效液相色谱-电感耦合等离子体质谱法测定水样中的汞

摘要

A novel and simple solid phase extraction (SPE)-high performance liquid chromatography (HPLC)-inductively coupled plasma mass spectrometry (ICP-MS) method was developed for determination of inorganic mercury (IHg), methylmercury MeHg and ethylmercury (EtHg) in water samples in the present work The procedure involves pre-functionalization of the commercially available C18 SPE column with dithizone, loading water sample, displacement elution of mercury species by Na2S2O3 solution. followed by HPLC-ICP-MS determination Characterization and optimization of operation parameters of this new SPE procedure were discussed, including eluting reagent selection, concentration of eluting reagent, volume of eluting reagent, effect of NaCl and humic acid in sample matrix At optimized conditions, the detection limits of mercury species for 100 mL water sample were about 3 ng L-1 and the average recoveries were 93 7,83 4. and 71.7% for MeHg. IHg and EtHg, respectively, by spiking 0 2 mu g L-1 mercury species into de-ion water. Stability experiment reveals that both the dithizone-functionalized SPE cartridge and the mercury species incorporated were stable in the storage procedure These results obtained demonstrate that SPE-HPLC-ICP-MS is a simple and sensitive technique for the determination of mercury species at trace level in water samples with high reproducibility and accuracy (C) 2010 Elsevier B V All rights reserved.
机译:建立了一种新颖,简单的固相萃取-高效液相色谱-电感耦合等离子体质谱法(ICP-MS),用于测定水中的无机汞(IHg),甲基汞MeHg和乙基汞(EtHg)本工作中的样品该程序包括用双硫zone对市售C18 SPE色谱柱进行预功能化,加载水样,用Na2S2O3溶液置换汞物种。然后通过HPLC-ICP-MS测定讨论了该新SPE程序的表征和优化操作参数,包括洗脱剂的选择,洗脱剂的浓度,洗脱剂的体积,样品基质中NaCl和腐殖酸的影响在优化条件下, 100 mL水样中汞的检出限约为3 ng L-1,MeHg的平均回收率为93 7,83 4.和71.7%。通过将0 2μgL-1汞物质掺入去离子水中分别提取IHg和EtHg。稳定性实验表明,双硫zone功能化的SPE柱和所含汞物种在储存过程中均稳定。这些结果表明,SPE-HPLC-ICP-MS是一种简单灵敏的测定痕量汞的方法。高重复性和准确性的水样品(C)2010 Elsevier BV保留所有权利。

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