The respiration rate of PH3 susceptible strain was significantly higher than the resistant strain. The results showed no significant effect of oxygen level on the respiration rate of both strains. Phosphine reduced the respiration rate of both strains when it was applied in average concentrations. However, the rate of respiration of the resistant beetles increased significantly under a high level of phosphine. The increase of respiration rate was associated with the higher emission of VOCs which prove the acceleration of metabolic processes to face the phosphine action for survival. Flat grain beetle Cryptolestes pusillus and rusty grain beetle C. ferrugineus are similar insect species, but only C. ferrugineus is capable to develop a high phosphine resistance. A direct immersion solid phase microextraction gas chromatography-mass spectrometry (DI-SPME-GCMS) technology has identified the different fatty acids from PH3 resistant and susceptible strain of Tribolium castaneum.