首页> 外文期刊>Journal of Analytical Atomic Spectrometry >Separation of selenium compounds by CE-ICP-MS in dynamically coated capillaries applied to selenized yeast samples
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Separation of selenium compounds by CE-ICP-MS in dynamically coated capillaries applied to selenized yeast samples

机译:通过CE-ICP-MS在应用于硒化酵母样品的动态包被的毛细管中分离硒化合物

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摘要

The selenium species in nutritional supplement tablets, based on selenized yeast, were separated by capillary zone electrophoresis using capillaries coated dynamically with poly(vinyl sulfonate) and detected by ICP-MS. Sample pre-treatment consisted of cold-water extraction by sonication and subsequent incubation of the cold-water extract with 6 M hydrochloric acid at 110℃. The total selenium concentration in the cold-water extract was 3.5 mg L~(-1) and corresponded to 9% of the total selenium content of the tablets. More than 20 different selenium compounds were separated in the cold-water extract within 13 min. The efficiency of the system corresponded to 620 000 theoretical plates. When spiking the sample with available standards, co-migration was observed with selenomethionine and selenocystine-Se-methylselenocysteine―the latter species were not separated. When the cold-water extract was hydrolysed in hot hydrochloric acid, 45% of the selenium migrated within a single peak that co-migrated with selenomethionine. Other peaks co-migrated with trimethylselenonium, Se-methylselenomethionine, and selenocystine-Se-methylselenocysteine, respectively. The precision for the analysis of the aqueous extracts expressed as relative standard deviation (n = 3) on peak heights and areas was in the range 1.4-5.3%. Detection limits were better than 15 μg L~(-1), corresponding to absolute detection limits less than 250 fg.
机译:营养补剂片剂中的硒元素(基于硒化酵母)通过毛细管区带电泳进行分离,该毛细管区带使用动态涂有聚(乙烯基磺酸盐)的毛细管进行毛细管电泳,并通过ICP-MS检测。样品预处理包括超声处理冷水提取物,然后将冷水提取物与6 M盐酸在110℃下孵育。冷水提取物中的总硒浓度为3.5 mg L〜(-1),相当于片剂中总硒含量的9%。在13分钟内从冷水提取物中分离出20多种不同的硒化合物。该系统的效率相当于620 000理论塔板。当用可用的标准品加标时,观察到硒代蛋氨酸和硒代半胱氨酸-Se-甲基硒代半胱氨酸的共迁移,后一种没有分离。当冷水提取物在热盐酸中水解时,45%的硒在与硒代蛋氨酸共同迁移的单个峰中迁移。其他峰分别与三甲基硒鎓,Se-甲基硒甲硫氨酸和硒代半胱氨酸-Se-甲基硒代半胱氨酸共同迁移。以峰高和峰面积的相对标准偏差(n = 3)表示的水相萃取物分析精度为1.4-5.3%。检出限优于15μgL〜(-1),对应的绝对检出限小于250 fg。

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