Preparation of sulfonated graphene/polypyrrole solid-phase microextraction coating by in situ electrochemical polymerization for analysis of trace terpenes

• Preparation of sulfonated graphene/polypyrrole coating by in situ electropolymerization.
• High extraction selectivity and capacity to volatile terpenes.
• Practical application for analysis of trace terpenes from spice samples.

In this study, a novel sulfonated graphene/polypyrrole (SG/PPy) solid-phase microextraction (SPME) coating was prepared and fabricated on a stainless-steel wire by a one-step in situ electrochemical polymerization method. Crucial preparation conditions were optimized as polymerization time of 15 min and SG doping amount of 1.5 mg/mL. SG/PPy coating showed excellent thermal stability and mechanical durability with a long lifespan of more than 200 stable replicate extractions. SG/PPy coating demonstrated higher extraction selectivity and capacity to volatile terpenes than commonly-used commercial coatings. Finally, SG/PPy coating was practically applied for the analysis of volatile components from star anise and fennel samples. The majority of volatile components identified were terpenes, which suggested the ultra-high extraction selectivity of SG/PPy coating to terpenes during real analytical projects. Four typical volatile terpenes were further quantified to be 0.2–27.4 μg/g from star anise samples with good recoveries of 76.4–97.8% and 0.1–1.6 μg/g from fennel samples with good recoveries of 80.0–93.1%, respectively.