HS-SPME-GC-MS is widely used to characterize the profile of volatile compounds despite some bad uses with a lack of information on the precision and repeatability of this technique. This work proposes a method, including a calibration step, to determine the global volatile compounds profile of a pea protein isolate at different pH of extraction. At the same time, nine compounds of interest were semi-quantified: hexanal, nonanal, 2-nonenal, 3methylbutanal, benzaldehyde, 1-octen-3-ol, 3-octen-2-one, 2-pentylfuran, and 2,5-dimethylpyrazine. The variation coefficient of the method for a single fiber was 15%. Semi-quantification was done by external calibration. The global volatile compounds profile was composed of 39 compounds including 13 aldehydes, 9 alcohols, 13 ketones, and 4 furans. The quantification of the nine compounds of interest at different extraction pHs showed the importance of pH for aroma release from pea protein isolates. For example, hexanal release was found 59% higher with extraction using pH 4.5 than with pH 6.5.