About this Chemistry article

Determination of Nitrogen Mustard Hydrolysis Products, Ethanolamines by Gas Chromatography–mass Spectrometry After Tert-butyldimethylsilyl Derivatization by Isaac Ohsawa; Yasuo Seto is a Chemistry article available to read on EtoBox.

A method for determining N-ethyldiethanolamine (EDEA), N-methyldiethanolamine (MDEA) and triethanolamine (TEA), hydrolysis products of nitrogen mustards, in water, urine and blood samples using gas chromatography-mass spectrometry (GC-MS) after derivatization by tert-butyldimethylsilylation (TBDMS) is described. The sample solution was evaporated to dryness, and reacted with N-methyl-N-(tertbutyldimethylsilyl)trifluoroacetamide (MTBSTFA) at 60 • C for 1 h. The TBDMS derivatives were separated on a DB-5 column and detected by electron-ionization MS. The quantitation of EDEA, MDEA and TEA was performed by measuring the respective peak areas on the extracted ion chromatograms of m/z 216, m/z 202 and m/z 346, respectively, using nonadecane (C 19 ), the peak area of which was measured at m/z 268, as an internal standard. When the water sample was initially analyzed, considerable loss of EDEA, MDEA and TEA occurred by evaporation. The addition of hydrochloric acid (HCl) to the water sample (final 1 mM), however, permitted quantitative recoveries to be achieved (88%, 88% and 79% for EDEA-(TBDMS) 2 , MDEA-(TBDMS) 2 and TEA-(TBDMS) 3 , respectively). The limits of detections (LODs, scan mod

Author

Isaac Ohsawa; Yasuo Seto

Publisher

Elsevier Science; Elsevier ; Elsevier BV (ISSN 1873-3778)

Published

2006

Language

EN

Field

Chemistry (Physical Sciences)