Solid phase microextraction coupled to liquid chromatography. Analysis of organosulphur compounds avoiding artifacts formation

•Novel application of the modern hyphenated methodology SMPE–HPLC for analysing OSCs in garlic samples.•Comparison between SPME–GC vs. SPME–HPLC, show evidence about artifacts formation.•The alternative coupling SPME and HPLC techniques was proposed.•We discourage the use of GC techniques for analysis of OSCs in garlic.

This work proposes the novel application of a microextraction technique, solid phase microextraction (SPME), coupled to liquid chromatography with UV detection (HPLC–UV) for the analysis of organosulfur compounds (OSCs) in garlic samples. Additionally, a comparative study of OSCs profiles obtained by SPME coupled to HPLC–UV and gas chromatography with flame photometric detector (GC–FPD), respectively; was carried out. This study provided complementary evidence about OSCs’s lability and “artifacts” formation during the analytical process. Raw, cooked and distilled garlic samples were considered. The target analytes were diallyl disulphide (DADS), diallyl sulphide (DAS), diallyl trisulphide (DATS), allicin, 3-vinyl-4H-1,3-dithiin (3-VD), 2-vinyl-4H-1,2-dithiin (2-VD) and (E)- and (Z)-ajoene, which are the most important OSCs with biological activities present in raw and processed garlic. The coupling of SPME and HPLC showed to be reliable, fast, sensible and selective methodology for OSCs analysis.