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首页> 外文期刊>Bulletin of the Korean Chemical Society >Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material
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Development of Isotope Dilution LC-MS/MS Method for Accurate Determination of Arsenobetaine in Oyster Certified Reference Material

机译:同位素稀释LC-MS / MS方法的开发,用于准确测定牡蛎认证标准物质中的砷甜菜碱

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An isotope dilution liquid chromatography tandem mass spectrometry (ID LC-MS/MS) method has been developed and applied to the determination of arsenobetaine (AsB, (CH3)3 +AsCH2COO−) from oyster candidate certified reference material (CRM). The exact matching isotope dilution approach was adopted for accurate determination of AsB using 13C2-labeled AsB as an internal standard. Efficiencies of different AsB extraction methods were evaluated using a codfish reference material and a simple sonication method was selected as the method of choice for the certification of the oyster candidate CRM. The hydrophilic interaction liquid chromatography (HILIC) combined with electrospray ionization tandem mass spectrometry (ESI/MS/ MS) in selected reaction monitoring (SRM) mode was optimized for adequate chromatographic retention and robust quantification of AsB from codfish and oyster samples. By analyzing 12 subsamples taken from each 12 bottles systematically selected from the whole oyster CRM batch, the certified value of AsB was determined as 6.60 mg·kg−1 ± 0.31 mg·kg−1 and it showed excellent between-bottle homogeneity of less than 0.42%, which is represented by relative standard deviation of 12 bottles from the CRM batch. The major source of uncertainty was the certified value of the AsB standard solution.
机译:已经开发了一种同位素稀释液相色谱串联质谱(ID LC-MS / MS)方法,并将其应用于牡蛎候选认证参考材料(CRM)中的砷甜菜碱(AsB,(CH3)3 + AsCH2COO-)测定。采用精确匹配的同位素稀释法,以13 C2标记的AsB作为内标物来准确测定AsB。使用鳕鱼参考材料评估了不同的AsB提取方法的效率,并选择了一种简单的超声处理方法作为牡蛎候选CRM认证的选择方法。在选定的反应监测(SRM)模式下,将亲水相互作用液相色谱(HILIC)与电喷雾电离串联质谱(ESI / MS / MS)结合进行了优化,以实现足够的色谱保留和对鳕鱼和牡蛎样品中AsB的可靠定量。通过分析从整个牡蛎CRM批次中系统地选择的每12瓶中抽取的12个子样品,确定AsB的认证值为6.60 mg·kg-1±0.31 mg·kg-1,并且显示出优异的瓶间均质性,小于0.42%,由CRM批次中的12个瓶子的相对标准偏差表示。不确定性的主要来源是AsB标准解决方案的认证价值。

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