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.