Development of a novel ultrasound Vacuum -assisted headspace solid phase microextraction approach for determination of solvent residual's in pharmaceuticals and comparison with traditional headspace solid phase microextraction method

Abstract In this report, an ultrasonication and vacuum assisted headspace solid-phase microextraction procedure followed by gas chromatography-flame ionization detection (UVA-HS-SPME-GC-FID) was proposed for direct extraction of solvent residuals, including benzene, toluene, ethyl benzene, m,p-xylene and o-xylene, in pharmaceutical matrices. A novel robust, reliable and durable nanocomposite solid-phase microextraction (SPME) fiber was prepared by layer-by-layer coating of 3-aminopropyltriethoxysilane-functionalized graphene (APTES) on a stainless-steel wire. Then, the proposed fiber was used for headspace SPME (HS-SPME) and trapping of toluene as a residual solvent in solid penicillin, Ampicillin, and Cefazolin vials followed by gas chromatography-flame ionization detection (GC-FID). UVA-HS-SPME-GC-FID achieves better validation parameters, including limit of detection, limit of quantification, linearity, recovery and repeatability, in comparison with conventional HS-SPME-GC-FID. The UVA-HS-SPME-GC-FID strategy is very effective for quantitative tracing of volatile and semivolatile solvent residuals in various pharmaceutical drugs.