Rapid Simultaneous Quantitative Analysis of Polygalaxanthone III and 3,6'-Disinapoyl Sucrose in Polygala Radix

Nishihara, Masakazu; Nukui, Keiji; Osumi, Yuko; Shiota, Hironori

doi:10.2116/bunsekikagaku.67.201

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“…Although PGX III is used to evaluate the quality of Onji by Chart 1. Plausible Fragmentations of PGX III and XI HPLC quantification both in China 7) and Japan, 8,9) we found the possibility that authentic samples could sometimes be imprecise. In this study we propose using the LC-MS/MS detection method, which discriminates PGX III and XI.…”

Section: Resultsmentioning

confidence: 77%

“…Using such a standard substance, Nishihara et al reported a quantification method for PGX III in Onji. 8,9) During our successive studies to establish a quality control method for single herbal extracts, 10) we found that two of the purchased PGX III samples showed the same retention time by LC analysis, but one showed a different time. It is thus important to identify the true structure being used as the reference sample for quality control methods.…”

Section: Introductionmentioning

confidence: 99%

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Structural Analysis of Polygalaxanthones, C-Glucosyl Xanthones of Polygala tenuifolia Roots

et al. 2019

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Polygalaxanthone III, a xanthone glycoside that is a major constituent of "Polygala Root" (Polygala tenuifolia roots, Onji in the Japanese Pharmacopoeia), has been used as a standard in the quality control of crude drugs. However, we previously noted differences in the chromatographic properties of one of three samples of polygalaxanthone III. Therefore, standardization of the standard itself is extremely important. The structures of three standard samples commercially available as polygalaxanthone III were characterized by LC/MS and NMR. LC/MS analysis revealed that two molecular types exist. Both types are chromatographically separable but have an identical mass number with distinguishable MS/MS spectra. One dimensional (1D)-NMR analyses demonstrated that both had the same xanthone moiety and heteronuclear multiple bond correlation (HMBC) analyses revealed that they are structural isomers at the connecting position of glucose to apiose 1-position. Consequently, the isomers were identified as polygalaxanthone III and its regioisomer, polygalaxanthone XI. Based on the findings, we recommend using the LC-MS/MS detection method, which discriminates polygalaxanthone III and XI, to confirm the quality of the standard.

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Section: Resultsmentioning

confidence: 77%