Low nanogram detection of nucleotides using fast atom bombardment-mass spectrometry

✍ Scribed by Qing-Mei Weng; William M. Hammargren; Debra Slowikowski; Karl H. Schram; Katherine Z. Borysko; Linda L. Wotring; Leroy B. Townsend

• Publisher: Elsevier Science
• Year: 1989
• Tongue: English
• Weight: 437 KB
• Volume: 178
• Category: Article
• ISSN: 0003-2697
• DOI: 10.1016/0003-2697(89)90363-1

✦ Synopsis

The effect of trimethylsilyl (TMS) derivatization on detection limits of mononucleotides in fast atom bombardment-mass spectrometry (FAB-MS) was examined. FAB-MS methods were developed to optimize sensitivity using adenosine 6'-monophosphate as a model compound and then applied to reference standards of two clinically important nucleotides: tricyclic nucleoside-5'-monophosphate (TCNMP) and 5-fluoro-2'-de-oxyuridineG'-monophosphate (FdUMP). The detection limit for the TMS derivative of TCNMP was 2.5-5 ng/ ~1 and less than 2.5 ng/rl for FdUMP as its TMS derivative. This is greater than two orders of magnitude more sensitive than the FAB-MS analysis of the corresponding free compounds. These low detection limits for the TMS derivatives were obtained using a narrow scan range, signal averaging, detection in the negative ion mode, and 3-nitrobenzyl alcohol as the matrix. Hydrolysis of one or more of the labile TMS groups did occur, with the extent of hydrolysis being greatest in the more protic matrices. @ 1989 Academic Press, Inc.