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首页> 外文期刊>Journal of mass spectrometry: JMS >Separation and determination of seleno amino acids using gas chromatography hyphenated with inductively coupled plasma mass spectrometry after hollow fiber liquid phase microextractiion
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Separation and determination of seleno amino acids using gas chromatography hyphenated with inductively coupled plasma mass spectrometry after hollow fiber liquid phase microextractiion

机译：中空纤维液相微萃取-电感耦合等离子体质谱联用气相色谱法测定硒氨基酸。

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摘要

A new derivatization-extraction method for preconcentration of seleno amino acids using hollow fiber liquid phase microextraction (HF-LPME) was developed for the separation and determination of seleno amino acids in biological samples by gas chromatography-inductively coupled plasma mass spectrometry (GC-ICP-MS). Derivatization was performed with ethyl chloroformate (ECF) to improve the volatility of seleno amino acids. Parameters influencing microextraction, including extraction solvent, pH of sample solution, extraction time, stirring speed, and inorganic salt concentration have been investigated. Under the optimal conditions, the limits of detection (LODs) obtained for Se-methyl-selenocysteine (SeMeCys), selenomethionine (SeMet), and selenoethionine (SeEth) were 23, 15, and 11 ng Se l(-1), respectively. The relative standard deviations (RSDs) were 14.6%, 16.4%, and 19.4% for SeMeCys, SeMet, and SeEth (c = 1.0 ng ml(-1), n = 7), respectively, and the RSDs for SeMeCys, SeMet could be improved obviously if SeEth was utilized as the internal standard. The proposed method was applied for the determination of seleno amino acids in extracts of garlic, cabbage, and mushroom samples, and the recoveries for the spiked samples were in the range of 96.8-108% and 93.4-115% with and without the use of SeEth as internal standard. The developed method was also applied to the analysis of SeMet in a certified reference material of SELM-1 yeast and the determined value is in good agreement with the certified value.
机译：开发了一种利用中空纤维液相微萃取（HF-LPME）富集硒化氨基酸的新衍生化方法，用于气相色谱-电感耦合等离子体质谱法（GC-ICP）分离和测定生物样品中的硒氨基酸。 -多发性硬化症）。用氯甲酸乙酯（ECF）进行衍生化以提高硒代氨基酸的挥发性。研究了影响微萃取的参数，包括萃取溶剂，样品溶液的pH，萃取时间，搅拌速度和无机盐浓度。在最佳条件下，硒甲基硒代半胱氨酸（SeMeCys），硒代蛋氨酸（SeMet）和硒代乙硫氨酸（SeEth）的检出限（LODs）分别为23 ng，15 ng和11 ng Se l（-1）。 SeMeCys，SeMet和SeEth的相对标准偏差（RSD）分别为14.6％，16.4％和19.4％（c = 1.0 ng ml（-1），n = 7），而SeMeCys，SeMet的RSD可以如果将SeEth用作内标，则可以明显改善。该方法用于大蒜，卷心菜和蘑菇提取物中硒氨基酸的测定，加标和不加标样的回收率在96.8-108％和93.4-115％之间。用SeEth作为内标。所开发的方法还用于SELM-1酵母认证参比物质中SeMet的分析，测定值与认证值高度吻合。

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