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首页> 外文期刊>Journal of chromatography, A: Including electrophoresis and other separation methods >On-line coupling of flow injection displacement sorption preconcentration to high-performance liquid chromatography for speciation analysis of mercury in seafood
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On-line coupling of flow injection displacement sorption preconcentration to high-performance liquid chromatography for speciation analysis of mercury in seafood

机译:流动注射置换吸附预浓缩与高效液相色谱在线耦合用于海鲜中汞的形态分析

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A simple and cost-effective method for speciation analysis of trace mercury in seafood was developed by on-line coupling flow injection microcolumn displacement sorption preconcentration to high-performance liquid chromatography (HPLC) with UV detection. The methodology involved the presorption of the Cu-PDC (pyrrolidine dithiocarbamate) chelate onto a microcolumn packed with a cigarette filter sorbent, simultaneous preconcentration of Hg(II), methylmercury (MeHg), ethylmercury (EtHg), and phenylmercury (PhHg) onto the microcolumn through a displacement reaction with the presorbed Cu-PDC, and their subsequent elution from the microcolumn for on-line HPLC separation. Interferences from heavy metal ions with lower stability of their PDC chelates relative to Cu-PDC were minimized without the need of any masking agents. With the consumption of 4.0 ml of sample solution, the enrichment factors were about 80. The detection limits were 10-25 ng g(-1) (as Hg) in fresh tissue. Precision (R.S.D. (%), n = 5) ranged from 2 to 3% at the 500 mug 1(-1) (as Hg) level. The developed technique was validated by analyzing a certified reference material (DORM-2, dogfish-muscle), and was shown to be useful for mercury speciation in real seafood samples. (C) 2004 Elsevier B.V. All rights reserved.
机译:通过在线耦合流动注射微柱置换吸附预富集与高效液相色谱(HPLC)在线检测,开发了一种简单,经济高效的海产品中痕量汞形态分析方法。该方法包括将Cu-PDC(吡咯烷二硫代氨基甲酸酯)螯合物预吸附到装有香烟过滤嘴吸附剂的微柱上,同时将Hg(II),甲基汞(MeHg),乙基汞(EtHg)和苯基汞(PhHg)预先浓缩。微柱通过与预吸附的Cu-PDC发生置换反应,然后从微柱中洗脱出来进行在线HPLC分离。相对于Cu-PDC,具有较低PDC螯合物稳定性的重金属离子的干扰得以最小化,而无需使用任何掩蔽剂。消耗4.0 ml样品溶液,富集因子约为80。在新鲜组织中的检出限为10-25 ng g(-1)(以Hg计)。精度(R.S.D.(%),n = 5)在500杯1(-1)(以Hg为单位)的水平范围内为2-3%。通过分析经认证的参考物质(DORM-2,dog鱼肌肉)验证了该开发的技术,该技术可用于实际海鲜样品中的汞形态分析。 (C)2004 Elsevier B.V.保留所有权利。

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