Positive and negative ion mass spectrometry of benzophenones, the acid-hydrolysis products of benzodiazepines

Abstract

Positive electron impact (EI), positive chemical ionization (CI), and negative CI mass spectra of 14 benzophenones are presented. In the positive EI mode, intense molecular peaks appeared for most compounds; some other peaks due to splitting at both sides of the carbonyl group also appeared. In the positive CI mode, [M + 1]+ quasi-molecular ions together with [M + C2H5]+ peaks were observed for all compounds; some fragment peaks were common to those in the positive EI mode. In the negative CI mode, the spectra were much simpler than those in the positive EI or CI mode. In the 1 Torr negative CI mode, some spectra showed only single molecular anions; in the 0.01 Torr negative CI mode, halogen or nitro peaks appeared in addition to the molecular anions. An extraction procedure for benzophenones from human urine and plasma after heating in strong acid, and their separation by gas chromatography (GC) are also presented to serve for their actual identification by GC/mass spectrometry.

Rapid and simple analysis of oxazolobenzodiazepine drugs in sera by wide-bore capillary gas chromatography with nitrogen-phosphorus detection using on-column methylation

“…In previous reported studies, oxazolobenzodiazepine drugs were determined in the forms of benzophenones after acid hydrolysis [3,[6][7][8], and in their underivatized forms [3,5,9] by GC or GC/MS. Japp et al [3] reported that underivatized oxazolobenzodiazepines easily decomposed during passage through a BP-1 middle-bore capillary column (25 m × 0.22 mm i.d.)…”

“…Various methods for the determination of benzodiazepines in biological materials have been reported. Analytical methods for underivatized oxazolobenzodiazepines and other benzodiazepines include thin-layer chromatography (TLC) [2,3], high-performance (HP) TLC [4], gas chromatography (GC) [3,[5][6][7], GC-mass spectrometry (MS) [3,5,[7][8][9], high-performance liquid chromatography (HPLC) [3,10,11], and immunoassays [12]. However, simultaneous determination of methylated oxazolobenzodiazepine drugs by GC or GC/MS has not been reported to our knowledge.…”

Opiate & Benzodiazepine Confirmations: To Hydrolyze or Not to Hydrolyze is the Question

“…The formation of nordiazepam had the potential to lead to a false-positive result that should be interpreted with caution (35). Overall, enzymatic hydrolysis is recommended for benzodiazepine drugs because acid hydrolysis can degrade the drugs to benzophenones and limit accurate drug identification (36). Chemical hydrolysis is a faster procedure in comparison to enzyme hydrolysis; however, acid may cause chromatographic interference by producing high background noise through the generation extra peaks in the chromatogram (37).…”

Modern screening strategies in analytical toxicology with special regard to new benzodiazepines

“…A forthcoming title [55] presents the spectra (GLC-MS, LC-MS, UV, IR) of the new benzodiazepines described in this article and many metabolites and hydrolysis products. See Suzuki et al [77] for mass spectra of benzophenones and Schtitz et al [70] for infrared spectroscopy.…”