In order to study the types, relative contents and differences in aroma components of the volatile components in the peel and pulp of Shatian pomelo, to expand the reuse of Shatian pomelo processing by-products and enable the preparation of Shatian pomelo essence and flavoring, headspace solid-phase microextraction (HS-SPME)-gas chromatography-mass spectrometry (GC-MS) was used to determine the volatile components in the peel and pulp of the same batch of Shatian pomelo. The volatile components of peel and pulp were analyzed by ROAV analysis, heat map, column diagram, percentage chord diagram and radar charts. The results showed that 104 volatile components were detected in the peel, with the primary components being D-limonene (16.61%) and β-pinene (12.83%). 50 kinds of volatile components were detected in the flesh, with the predominant constituents being geraniol (12.24%) and D-limonene (9.75%). Based on the cumulative ROAV values, the substance that contributes the most to the flavor of the peel was laurene, whilst caproaldehyde was the greatest contributor to the flesh flavor. Furthermore, in the peel, the contents of D-juniperene and β-pinene exceeded that of D-limonene, whilst the pulp contained a larger amount of hexaldehyde, with the presence of n-hexanol may be the reason for the distinct aroma of Shatian pomelo from the Lingnan region compared with the pomelos from other regions or other varieties. Through an analysis of volatile components in Shatian pomelo fruit sourced from Lingnan, this study provides a reference for comprehensive development of Shatian pomelo, the reuse of pomelo residue and preparation of Shatian pomelo essence.