Headspace solid-phase microextraction of menthol using a sol–gel titania-based coating along with multiwalled carbon nanotubes on the surface of stainless steel fiber

Abstract

Sol–gel coating technology for the preparation of solid-phase microextraction fibers involves a single-step procedure and allows for in situ creation of chemically bonded coatings which are characterized by high thermal and solvent stabilities. A novel titania sol–gel coating was prepared for the first time on a stainless steel fiber and applied for the headspace solid-phase microextraction (HS-SPME) of menthol with gas chromatography and flame ionization detection. Important parameters influencing the efficiency of SPME process, such as extraction time, extraction temperature and ionic strength, were optimized by central composite design. An extraction time of 40 min at 60 °C gave maximum extraction efficiency, when NaCl (10% w/v) was added to the aqueous sample. The analytical characteristics of the proposed method were comparable with other reported fibers. Under optimized conditions, the linearity was between 0.05 and 100 µg mL− 1. The relative standard deviations (RSDs) determined at 0.5 µg mL− 1 concentration level (n = 5) were as follows: intra-day RSD 7.26%; inter-day RSD 10.87%; fiber-to-fiber RSD 9.05%. The relative recoveries determined after spiking a mint distillate sample at three concentration levels from 0.067 to 50.0 µg mL− 1 varied from 86 to 102%. The proposed method was successfully applied for the analysis of menthol in peppermint samples.