SummaryWine ageing is of great importance to the quality and organoleptic properties of Huangjiu. The aim of the present work was to investigate the effect of ageing temperature on the content changes in ethyl carbamate (EC) and its precursors including citrulline, arginine, ornithine and urea in Hakka Huangjiu. Aroma compound changes were also detected using headspace solid‐phase microextraction coupled with gas chromatography spectrometry. Results indicated that with the increase in ageing temperature, citrulline and EC concentrations increased, whereas arginine and ornithine concentrations decreased. Urea was decreased slightly from 4 to 20 °C while increased at 37 °C. Pearson test demonstrated that ageing temperature had significant correlation with EC and arginine. The concentrations of aroma compounds, especially esters, alcohols, acids and heterocyclic compounds were different in different ageing temperatures. Ageing temperature of Hakka Huangjiu was suggested setting in a lower temperature as for strictly controlling contents of urea and citrulline, as well as EC.