Department of Applied Chemistry, Corvinus University of Budapest, 1118 Budapest, Villányi út 29-33, Hungary.
Metallomics. 2009;1(4):317-29. doi: 10.1039/b901184f. Epub 2009 May 28.
An analytical approach allowing the identification of unknown selenium metabolites in selenium-rich yeast was described. Anion-exchange HPLC of the Se-metabolome fraction co-eluting with salts in size-exclusion chromatography allowed the separation of nine selenium species (excluding isomers and selenate) as monitored by inductively coupled plasma mass spectrometry (ICP MS). The individual fractions were analyzed by electrospray QTOF MS/MS and hybrid linear ion trap/Orbitrap MSn after sample introduction by reversed-phase nanoHPLC and by hydrophilic interaction LC (HILIC), respectively. Out of the nine detected species, eight were identified on the basis of accurate mass measurements and collision induced dissociation/fragmentation information. Seven Se-species (selenohomolanthionine, γ-Glu-selenocystathionine, 2,3-DHP-selenocystathionine, N-acetyl-selenocystathionine, 2,3-DHP-selenohomolanthionine, Se-methyl-selenoglutathione, and 2,3-DHP-Se-methylselenocysteine) were reported for the first time in Se-rich yeast, five of them have never been reported in any biological sample before.
本文描述了一种可用于鉴定富硒酵母中未知硒代谢物的分析方法。采用离子交换 HPLC 对排阻色谱中与盐共洗脱的硒代谢组馏分进行分离，电感耦合等离子体质谱（ICP-MS）监测到 9 种硒化物（不包括异构体和硒酸盐）。通过反相纳升 HPLC 和亲水相互作用 LC（HILIC）分别进样后，采用电喷雾 QTOF MS/MS 和混合线性离子阱/轨道阱 MSn 对各个馏分进行分析。在检测到的 9 种物质中，有 8 种基于精确质量测量和碰撞诱导解离/碎裂信息进行了鉴定。在富硒酵母中首次报道了 7 种硒化物（硒同型硫代半胱氨酸、γ-Glu-硒代半胱氨酸、2,3-DHP-硒代半胱氨酸、N-乙酰-硒代半胱氨酸、2,3-DHP-硒同型硫代半胱氨酸、Se-甲基-谷胱甘肽和 2,3-DHP-Se-甲基硒代半胱氨酸），其中 5 种在以前的任何生物样本中都从未报道过。
