In this study, a combination sampling method, including headspace solid-phase micro-extraction (HSSPME), simultaneous distillation extraction (SDE) and steam distillation (SD), were used to study the aroma profile characteristics of durian (Durio zibethinus Murr.) pulp during storage, followed by gas chromatography-mass spectrometric (GC-MS) detection; 26 and 22 aroma volatiles of fresh and deteriorated durian pulps were identified according to different degrees of certainty. Volatile esters were identified as the main aromatic components of durian pulp. Most ethyl esters reduced in concentration during storage, whereas the methyl, propyl and butyl esters increased. Different aroma profile characteristics at the fresh and deteriorated storage phases obtained by HSSPME were specified by principal component analysis (PCA). Five typical aroma volatiles contributing greatly to the difference of aroma profile characteristics of durian pulp at the fresh and deteriorated storage phases were distilled by common model strategy. These compounds are potential bio-markers for durian degradation, but further study is needed. Tentative results suggest that combining HSSPME with conventional volatile isolation methods would yield more representative data on changes in the aroma of durian pulp during storage.