LC–DAD–MS Determination of the Major Constituents in Radix Angelicae sinensis

Column liquid chromatography with diode array and mass spectrometric detection was developed for the qualitative and quantitative analysis of the major constituents in Radix Angelicae sinensis. Sixteen compounds including phthalic acid, vanillic acid, ferulic acid, guaiacol, Z-6,7-epoxyligustilide, senkyunolide F, carvacrol, Z-ligustilide, Z-butylidenephthalide, E-6,7-dihydroxydihydroligustilide, senkyunolide I or senkyunolide H, coniferyl ferulate, sendanelolide, butylphthalide, E-ligustilide, E-butylidenephthalide except guaiacol and carvacrol were identified using online ESI–MS in comparisons with literature data and standard compounds. Nine compounds were quantified by LC–DAD simultaneously. For chromatographic analysis, a Merck C18 column (5 μm, 250 mm × 4.6 mm) with a compatible guard column (C18, 5 μm, 7.5 mm × 4.6 mm) was used. The mobile phase consisted of (A) 0.1% aqueous formic acid and (B) acetonitrile. Ten microliters of each sample solution were injected and eluted at a flow rate of 1 mL min-1. The column temperature was maintained at 30 °C. The validation of this method proved good linear regression (r2 > 0.9992) within the test ranges, desirable repeatability with overall intra- and inter-day variations of less than 4.91% and well acceptable recoveries varied between 90.91 and 96.73% while the RSDs were below 3.23% (n = 3). The proposed method was successfully applied to the quantification of the nine components in sixteen samples from different localities in China. This assay provides a valid and an overall quality control of Radix Angelicae sinensis.