Headspace solid phase microextraction (HS-SPME) was used to isolate volatile compounds (VOCs) from mangoes (Harumanis cv.). Among the four SPME fibres investigated, the mixed phase coating, 65 μm polydimethyl siloxane–divinylbenzene (DVB/PDMS) showed the highest efficiency in extracting VOCs as 26 compounds were detected with the total area of 9.6 x 109. The optimization of SPME factors was conducted in 2 stages using multivariate design. The first stage involved screening of the significant factors using the Plackett–Burman (P–B) design, followed by the optimization of the significant factors utilizing Central Composite Design (CCD). The experimental design for both P-B and CCD design was generated using Design-Expert version 6.0.4 (Stat Ease Software). Extraction time and temperature appeared to be the most significant factors in extracting VOCs in mangoes, with the optimum conditions prevailing at 55°C and 34 minutes respectively.