Derivatization of pinacolyl alcohol with phenyldimethylchlorosilane for enhanced detection by gas chromatography-mass spectrometry.
A derivatization procedure for the qualitative gas chromatography-mass spectrometry (GC-MS) analysis of pinacolyl alcohol (PA) that employs phenyldimethylchlorosilane (PhDMClS) and the promoter N-methylimidazole is described. While PA, underivatized, can be detected using conventional gas chromatographic methods, its polarity and low boiling point make its detection in complex matrices challenging. The silylation procedure described herein generates a PA-derivative exhibiting an increased on-column retention time, thus shifting its GC-MS signal away from commonly encountered, volatile, interfering analytes. Derivatized PA could be distinguished from other PhDMClS-derivatized isomeric alcohols by its unique retention time and mass spectrum. The derivatization was demonstrated to perform well in the GC-MS analysis and identification of PA in samples from Proficiency Tests administered by the Organisation for the Prohibition of Chemical Weapons (OPCW).
Lawrence Livermore National Laboratory, Forensic Science Center, 7000 East Avenue, Livermore, CA, 94550, USA.
Rebecca L F
RL
Albo
Carlos A
CA
Valdez
Roald N
RN
Leif
Heather A
HA
Mulcahy
Carolyn
C
Koester
D001711:Biotransformation; D002619:Chemical Warfare Agents / Q000032:analysis*; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D000441:Hexanols / Q000032:analysis* / Q000737:chemistry; D006801:Humans; D066298:In Vitro Techniques; D059021:Laboratory Proficiency Testing; D057230:Limit of Detection; D012821:Silanes / Q000737:chemistry*; D012999:Soman / Q000378:metabolism
D002619:Chemical Warfare Agents; D000441:Hexanols; D012821:Silanes; C053516:3,3-dimethyl-2-butanol; C077878:chlorodimethylphenylsilane; D012999:Soman