PMID- 19053158 OWN - NLM STAT- MEDLINE DCOM- 20090728 LR - 20151119 IS - 1096-9888 (Electronic) IS - 1076-5174 (Linking) VI - 44 IP - 5 DP - 2009 May TI - Separation and determination of seleno amino acids using gas chromatography hyphenated with inductively coupled plasma mass spectrometry after hollow fiber liquid phase microextraction. PG - 605-12 LID - 10.1002/jms.1533 [doi] AB - 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. CI - 2008 John Wiley & Sons, Ltd. FAU - Duan, Jiankun AU - Duan J AD - Department of Chemistry, Wuhan University, Wuhan 430072, China. FAU - Hu, Bin AU - Hu B LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - England TA - J Mass Spectrom JT - Journal of mass spectrometry : JMS JID - 9504818 RN - 0 (Organoselenium Compounds) RN - 0CH9049VIS (Selenocysteine) RN - 3FPU23BG52 (Toluene) RN - 451W47IQ8X (Sodium Chloride) RN - 7V31YC746X (Chloroform) RN - 964MRK2PEL (Selenomethionine) RN - K848JZ4886 (Cysteine) RN - TWK220499Z (selenomethylselenocysteine) RN - WX1BN24WZT (Ethionine) SB - IM MH - Agaricales/chemistry MH - Brassica/chemistry MH - Chemical Fractionation/*methods MH - Chloroform/chemistry MH - Cysteine/analogs & derivatives/analysis MH - Ethionine/analogs & derivatives/analysis MH - Garlic/chemistry MH - Gas Chromatography-Mass Spectrometry/*methods MH - Organoselenium Compounds/*analysis MH - Selenocysteine/analogs & derivatives MH - Selenomethionine/analysis MH - Sensitivity and Specificity MH - Sodium Chloride/chemistry MH - Toluene/chemistry EDAT- 2008/12/05 09:00 MHDA- 2009/07/29 09:00 CRDT- 2008/12/05 09:00 PHST- 2008/12/05 09:00 [pubmed] PHST- 2009/07/29 09:00 [medline] PHST- 2008/12/05 09:00 [entrez] AID - 10.1002/jms.1533 [doi] PST - ppublish SO - J Mass Spectrom. 2009 May;44(5):605-12. doi: 10.1002/jms.1533.