Background : Spiraea prunifolia var. simpliciflora (Rosaceae) called “Brial wreath” is a deciduous latifoliate shrub that is widely distributed throughout in Northeast Asia. Phytochemical and biological investigation of S. prunifolia have led to the discovery of biologically active compounds. Pharmacological studies revealed that the extract of the root of S. prunifolia possess antioxidant, antipyretic and anti-inflammatory activities. Some chemical constituents such as sterols, phenolics, terpene and fatty acid, as well as ethanolic extracts from the roots of S. prunifolia, have previously been reported to modulate the deleterious effects of diabetes, to prevent high-fat diet-induced obesity, and to prevent cisplatin-induced nephrotoxicity. Our continuing research was carried out to search for other phytochemical constituents from the leavess of S. prunifolia. The chemical structures of compounds were determined by NMR and FAB/MS spectroscopic data interpretation. Methods and Results : Multiple-preparative liquid chromatography (MPLC) purifications were carried out on YMC LC-forte/R instrument (YMC Kyoto, Japan) equipped with YMC-Pack ODS-A columns (ODS gel : 5 ㎛, 10 ㎜ × 250 ㎜). High-performance liquid chromatography (HPLC) was performed on Agilent Technologies instrument (Aglient Tec., Santa clara, CA, USA) equipped with YMC–Pack Pro C18 columns (ODS gel : 5 ㎛, 4.6 ㎜ × 250 ㎜). Next, quantitative analysis was carried out on UPLC-QqQ/MS 3200 Q-TRAP instrument (AB SCIEX Toronto, Canada) using a ACQUITY UPLC (waters corp.) with an ACQUITY BEH C18 column (2.1 ㎜ × 100 ㎜, 1.7 ㎛). The metabolite samples was applied to preparative reversed-phase HPLC and UPLC using gradient method, solvent A [water + 0.1% formic acid (v/v)] and solvent B [acetonitrile + 0.1% formic acid (v/v)]. Conclusion : In this study, we isolated the major metabolites from the stem of Spiraea prunifolia var. simpliciflora by using MPLC and HPLC. UPLC-QqQ/MS was also used to quantify target compounds. Finally, we established methodology and performed the quantitative analysis on target compounds from the stem of Spiraea prunifolia var. simpliciflora.