Abstract In this study, the efficiency of nanoporous aluminium wires as fibres for headspace solid-phase microextraction (HS-SPME) of volatile compounds from Lippia citriodora was investigated and compared with two anodised methods. The prepared fibres are durable with very good chemical and thermal stability which can be coupled to GC and GC/MS. A one at-a-time optimisation strategy was applied for optimising the important extraction parameters such as extraction temperature, extraction time, sample mass and added water. Compared with hydrodistillation (HD), HS-SPME provide the advantages of a small amount of sample, time-saving, simplicity and cheapness.