Abstract

COVALENT ORGANIC NANOSPHERES AS A FIBER COATING FOR SOLID-PHASE MICROEXTRACTION OF GENOTOXIC IMPURITIES FOLLOWED BY ANALYSIS USING GAS CHROMATOGRAPHY–MASS SPECTROMETRY

Jadhav P. R.*, Lasure A. B. and Bawage S. B.

ABSTRACT

Covalent organic nanospheres (CONs) were tested as fiber coating for solid-phase microextraction of genotoxic contaminants (GTIs) from active ingredients (AIs). The CONs are assembled by a simple solution phase process at 25 ° C. The obtained nanospheres exhibited a high surface area, good melting, high acid and alkali resistance, as well as fine and durable gloss. Two types of GTI — alkyl halides (1-iodooctane, 1-chlorobenzene, 1-bromododecane, 1,2-dichlorobenzene, 1-bromooctane, 1-chlorohexane, and 1,8-dibromooctane) and sulfonate esters (methyl p-toluenesulfur) ethyl p-toluenesulfonate) —they were selected as targeted molecules to test coating performance. Fixed coverage acquired advanced features (EFs: 5097–9799) on selected GTI. The strong correlation between CONs and GTIs has been attributed to π – π interactions and hydrophobicity, large CON area, and compact size. Combined with gas chromatography – mass spectrometry, a standardized analysis method detected GTIs samples in capecitabine and imatinib mesylate at wide linear range (0.2–200ng / g) with low detection rate (0.04–2.0ng / g), satisfactory recovery (80.03 % –109.5%), with high frequency (6.20% –14.8%) and rebirth (6.20% –14.1%). Therefore, CON-coated files promise alternatives for critical GTI acquisition in AI samples.

Keywords: Covalent organic nanospheres, Solid-phase microextraction, Genotoxic impurities, Gas chromatography–mass spectrometry.