A　method　for　the　analysis　of　Baijiu　volatile　aroma　composition　via　adopting　the　pretreatment　method　of　liquid-liquid　extraction　combined　with　two-dimensional　gas　chromatography-quadrupole　mass　spectrometry　technology.　The　column　system　of　Rtx-WAX　chromatographic　column(30　m×0.25　mm×0.25　μm,　as　one-dimensional　chromatography　column),　and　BPX-5(2.5　m×0.1　mm×0.1　μm,　as　two-dimensional　chromatographic　column)　was　used　for　separation　and　the　modulation　period　was　4.2　s,　and　the　condition　of　quadrupole　mass　spectrometer　scanning　range　was　35~320　u.　The　separation　regularity　of　the　volatile　aroma　compositions　under　two-dimensional　chromatography　of　Fuyu　flavor　Baijiu　was　analyzed,　and　the　compound　regular　distribution　characters　were　found.　Using　this　method,　308　kinds　of　volatile　aroma　compositions　form　Fuyu　flavor　base　Baijiu　were　distinguished,　mainly　including　102　kinds　of　ester　substances,　42　kinds　of　alcohols　substances,　33　kinds　of　acids　substances,　26　kinds　of　aldehyde　substances,　19　kinds　of　ketone　substances　and　86　kinds　of　other　substances.　Meanwhile,　this　method　was　applied　to　analyze　the　Fuyu　flavor　Baijiu　in　market　with　different　classifications.　The　analysis　results　were　used　as　model　and　chromatography　analysis　was　combined　with　principal　component　analysis　to　predict　the　sensory　rating.　The　results　showed　that　principal　component　analysis　could　be　used　to　observe　the　classification　trend　of　different　Fuyu　flavor　Baijiu　in　market,　and　the　analysis　results　were　consistent　with　the　sensory　evaluation,　so　this　method　could　provide　the　theoretical　guidance　for　the　sensory　rating　in　Baijiu　production　process.　©　2019,　Editorial　Department　of　Journal　of　Food　Science　and　Technology.　All　right　reserved.