Quantitative selenium speciation in cod muscle by isotope dilution ICP-MS with a reaction cell: comparison of different reported extraction procedures

Quantitative selenium speciation in cod muscle by isotope dilution ICP-MS with a reaction cell: comparison of different reported extraction procedures
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通过反应池同位素稀释 ICP-MS 定量鳕鱼肌肉中的硒形态:不同报道的提取程序的比较

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发表时间:
2004
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影响因子:
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通讯作者:
A. Sanz
A. Sanz
中科院分区:
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文献类型:
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作者:
V. Huerta;María Luisa Fernández Sánchez;A. Sanz

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为了定量回收从鳕鱼肌肉中提取的硒,我们对四种不同的提取程序进行了评估。具有八极反应系统的 ICP-MS 已用于消除 Se 特异性检测中的干扰氩二聚体。通过使用反相和尺寸排阻 HPLC 分离物质来进行形态分析,并将强度色谱图转换为质量流量色谱图(通过适当的数学校正)后,通过柱后同位素稀释对分离的 Se 化合物进行在线定量。在校正 SeH+ 形成的强度信号后,使用 78Se/77Se 比率来量化总 Se 和每种含硒化合物。当使用酶消化时,硒回收率最高,而当使用“软”提取程序(MeOH/HCl)时,仅提取了鳕鱼中总硒的 5%。酶水解产物中发现的主要硒化合物是硒代蛋氨酸。 MeOH/HCl 提取物中不存在这种硒化合物,表明 Se 主要掺入蛋白质中。在鳕鱼肌肉组织中也检测到了许多未识别的硒种类,此处记录了它们的存在。
Four different extraction procedures have been evaluated aiming at quantitative recovery of Se species in their extraction from cod muscle. ICP-MS with an octopole reaction system has been used to allow the elimination of interfering argon dimers in Se specific detection. Speciation analysis was performed by separating the species using both reversed-phase and size exclusion HPLC and the separated Se compounds were quantified on-line by post-column isotope dilution after converting intensity chromatograms into mass flow chromatograms (via adequate mathematical corrections). 78Se/77Se ratio was used, after correction of intensity signals for SeH+ formation, to quantify both total Se and each selenocompound. The highest Se recoveries were obtained when using enzymatic digestions whereas only 5% of total Se in cod was extracted when a “soft” extraction procedure (MeOH/HCl) was used. The main selenocompound found in enzymatic hydrolysates was selenomethionine. This selenocompound was absent in MeOH/HCl extracts indicating that Se is mainly incorporated into proteins. A number of unidentified Se species have also been detected in cod muscle tissue and their presence is documented here.