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Objective:To systematically and comprehensively analyze coumarin components in Angelicae Sihensis Radix by an efficient and stable HPLC-Q-TOF-MS/MS method,in order to offer the theoretical basis to develop coumarin,establish the quality control standard and apply in clinic. Method:The separation effect of coumarin components was extracted by adjusting the column,temperature,mobile phase,flow rate,sample concentration and other conditions,and various coumarin components in Angelicae Sihensis Radix were identified by corresponding standards,precise molecular mass,polarity,pyrolysis pattern. Result:In this study,a high-efficiency and stable coumarin separation method was established that can be used to separate complex components,and 14 coumarin components were identified in this study,including phellopterin and osthenol that were rarely reported as effective components in Angelicae Sihensis Radix. Major fragment ions of coumarin components were analyzed. The cleavage in methoxy bond or anisole bond on the parent nucleus was the primary pattern for coumarin components, which was summarized for detecting unknowing coumarins. Conclusion:Abundant coumarins were contained in Angelicae Sihensis Radix. Further qualitative and quantitative analysis of coumarins are conducive to improving the quality standards of Angelicae Sihensis Radix,and providing reference for the development of coumarins and clinical application of Angelicae Sinensis Radix.
ABSTRACT
<p><b>OBJECTIVE</b>To investigate the chemical constituents of the herbs of Taraxacum mongolicum.</p><p><b>METHOD</b>The chemical constituents were isolated by various column chromatographic methods and their structures elucidated mainly by NMR and MS evidences.</p><p><b>RESULT</b>Forty-four components were obtained and identified were as artemetin (1), quercetin (2), quercetin-3', 4', 7-trime-thyl ether (3), luteolin (4), luteolin-7-O-beta-D-glucopyranoside (5), luteolin-7-O-beta-D-galactopyranoside (6), genkwanin (7), isoetin (8), hesperetin (9), genkwanin-4'-O-beta-D-lutinoside (10), hesperidin (11), quercetin-7-O-[beta-D-glucopyranosyl (1-->6) -beta-D-glucopyranoside (12), quercetin-3, 7-O-beta-D-diglucopyranoside (13), isoetin-7-O-beta-D-glucopyranosyl- 2'-O-alpha-L-arabinopyranoside (14), isoetin-7-O-beta-D-glucopyranosyl-2'-O-alpha-D-glucopyranoside (15), isoetin-7- O-beta-D-glucopyranosyl-2'-O-beta-D-xyloypyranoside (16), caffeic acid (17), furulic acid (18), 3-O-caffeoylquinic acid (19), 3, 5-di-O-caffeoylquinic acid (20), 3, 4-di-O-caffeoylquinic acid (21), 4, 5-di-O-caffeoylquinic acid (22), 1-hydroxymethyl-5-hydroxy-phenyl-2-O-beta-D-glucopyranoside (23), p-hydroxybenzoic acid (24), p-coumaric acid (25), 3, 5-dihydroxylbenzoic acid (26), gallic acid (27), gallicin (28), syringic acid (29), 3, 4-dihydroxybenzoic acid (30), caffeic acid ethyl ester (31), esculetin (32), rufescidride (33), mongolicumin A [6, 9, 10-trihydroxy-benzoxanthene-1, 2-dicarboxylic acid] (34), mongolicumin B [1 l-hydroxy-2-oxo-guaia-1 (10), 3, 5-trien-8, 12-lactone] (35), isodonsesquitin A (36), taraxacin (37), sesquiterpene ketolactone (38), taraxasteryl acetate (39), phi-taraxasteryl acetate (40) and lupenol acetate (41), palmitic acid (42), beta-sitosterol (43), and stigmasterol (44).</p><p><b>CONCLUSION</b>Four compounds (14, 15, 34 and 35) were new compounds, compounds 1, 3, 6-13, 20-22, 30 and 31 were isolated from this genus for the first time, while compounds 18, 23-29, 32 and 37-42 were obtained from this species for the first time.</p>
Subject(s)
Drugs, Chinese Herbal , Chemistry , Flavonols , Chemistry , Mass Spectrometry , Taraxacum , ChemistryABSTRACT
<p><b>OBJECTIVE</b>To study the chemical constituents of Taraxacum mongolicum.</p><p><b>METHOD</b>Repeated column chromatography over silica gel, C-18 and Sephadex LH-20 were used to isolate chemical constitutes and their structures were elucidated by spectroscopic methods MS, 1H-NMR, 13C-NMR including 2D-NMR techniques and by direct comparing spectral data with those reported in literatures.</p><p><b>RESULT</b>Eight compounds were identified as artemetin (1), quercetin (2), luteolin (3), luteolin-7-O-beta-D-glucopyranoside (4), caffeic acid (5), esculetin (6), stigmasterol (7), taraxasteryl acetate (8), respectively.</p><p><b>CONCLUSION</b>Compound 1 was obtained from this genus and compound 6, 8 from this species for the first time. Furthermore, the 13 carbon data of compound 6 from the literature were corrected with 2D-NMR techniques in this paper.</p>