M. Kotrebai, J. Tyson, P. Udén, M. Birringer, E. Block
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引用次数: 101
摘要
采用离子对高效液相色谱(HPLC)、在线电感耦合等离子体质谱(ICP-MS)和电喷雾电离体质谱(ESI-MS)检测对富硒大蒜和酵母样品的提取物和消化液进行分析。酵母中的硒化合物主要为硒代蛋氨酸和硒腺苷-硒同型半胱氨酸,大蒜中的硒代γ-谷氨酰基-硒代甲基半胱氨酸和γ-谷氨酰基-硒代蛋氨酸。所鉴定的化合物分别占酵母和大蒜样品中总硒含量的85%和90%。建立了富硒样品中硒化合物的在线HPLC-ESI-MS选择离子色谱图和质谱。HPLC-ICP-MS的定量限(LOQ,定义为S/N = 10)在10 - 50 ng mL-1 Se范围内。HPLC-ESI-MS的定量限是HPLC-ICP-MS的100倍。
Identification of the principal selenium compounds in selenium-enriched natural sample extracts by ion-pair liquid chromatography with inductively coupled plasma- and electrospray ionization-mass spectrometric detection
Selenium-enriched garlic and yeast sample extracts and digests were analyzed using ion-pair high performance liquid chromatography (HPLC) with on-line inductively coupled plasma-mass spectrometric (ICP-MS) and electrospray ionization-mass spectrometric (ESI-MS) detection. The principal selenium compounds in these samples were identified as selenomethionine, and Se-adenosyl-selenohomocysteine in yeast, and γ-glutamyl-Se-methyl-selenocysteine and possibly γ-glutamyl-selenomethionine in garlic. The compounds identified account for 85 and 90% of the total selenium content of the yeast and the garlic samples, respectively. On-line HPLC-ESI-MS selected ion chromatograms (SIC) and mass spectra of selenium compounds extracted from selenium enriched samples are presented. Limits of quantification (LOQ, defined as S/N = 10) for HPLC-ICP-MS were in the range 10–50 ng mL–1 Se in the injected extracts. LOQ values for HPLC-ESI-MS were ca. 100 times higher than those of HPLC-ICP-MS.