Hu-Gu capsule is a traditional Chinese medical formula for preventing glucocorticoid-induced osteoporosis. In this work, an ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry was developed for chemical identification of the phytochemical compositions in positive ion mode. A total of 41 compounds were detected in Hu-Gu capsule, and 25 compounds were characterized and identified by retention time,accurate mass within 5 ppm error and characteristic fragment ions. Among of them, four major flavonoids were further quantified by high performance liquid chromatography diode array detection in the four batches. The method was validated in terms of calibration curve regression coefficient (r2 > 0.9994), repeatability (RSD < 3.5%), intra- and inter-day precision (RSD < 1.1%), recovery (93.0–106.4%), limit of detection (0.1 μg/ml), and limit of quantification (1 μg/ml). The research could provide the analysis of chemical composition and be helpful to control the quality of HGC.
Ding, X.P., Wang, X.T., Chen, L.L., Guo, Q., Wang, H., Qi, J., Yu, B.Y., 2011. On-line high-performance liquid chromatography-diode array detection-electrospray ionization-mass spectrometry-chemiluminescence assay of radical scavengers in Epimedium. J. Chromatogr. A 1218, 1227–1235.
Guan, X.Y., Li, H.F., Yang, W.Z., Lin, C.H., Sun, C., 2011. HPLC-DAD-MSn analysis and HPLC quantitation of chemical constituents in Xian-ling-gu-bao capsules. J. Pharm. Biomed. Anal. 55, 932–933.
Li, X.H., Xiong, Z.L, Lu, S., Zhang, Y., Li, F.M., 2010. Pharmacokinetics of naringin and its metabolite naringenin in rats after oral administration of rhizome drynariae extract assayed by UPLC-MS/MS. Chin. J. Nat. Med. 8, 40–46.
Liu, Q.F., Jiao, Z., Liu, Y., Li, Z.D., Shi, X.J., Wang, W.J., Wang, B., Zhong, M.K., 2016. Chemical profiling of San-Huang decoction by UPLC-ESI-Q-TOF-MS. J. Pharm. Biomed. Anal. 131, 20–32.
Liu, W.Y., Zhou, C., Yan, C.M., Xie, S.L., Feng, F., Wu, C.Y., Xie, N., 2012. Characterization and simultaneous quantification of multiple constituents in Aurantii Fructus Immaturus extracts by HPLC-DAD-ESI-MS/MS. Chin. J. Nat. Med. 10, 456–463.
Luo, Q.L., Nurahmat, M., Li, M.H., Sun, J., Chen, M.X., Liu, F., Wei, Y., Dong, J.C., 2014. Pharmacological investigation of a HPLC/MS standardized three herbal extracts containing formulae (Bu-Shen-Yi-Qi-Tang) on airway inflammationand hypothalamic-pituitary-adrenal axisactivity in asthmatic mice. Phytomedicine 21, 1439–1450.
Naseer, S., Lone, S.H., Lone, J.A., Khuroo, M.A., Bhat, K.A., 2015. LC-MS guided isolation, quantification and antioxidant evaluation of bioactive principles from Epimedium elatum. J. Chromatogr. B 989, 62–70.
Qiu, X.H., Zhang, J., Huang, Z.H., Zhu, D.Y., Xu, W., 2013. Profiling of phenolic constituents in Polygonum multiflorum Thunb. by combination of ultra-high-pressure liquid chromatography with linear ion trap-Orbitrap mass spectrometry. J. Chromatogr. A 1292, 121–131.
Ren, Q., Wang, J.A., Liu, SX., Wang, F., Wang, H.Y., 2016. Identification and determination of isoflavones in germinated black soybean sprouts by UHPLC-Q-TOF-MS mass spectrometry and HPLC-DAD. Int. J. Food Prop., https://doi.org/10.1080/10942912.2016.1256303.
Shevlyakova, O.A., Vasil’ev, K.Y., Ikhalainen, A.A., Antokhin, A.M., Taranchenko, V.F., Goncharov, V.M., Mitrofanov, D.A., Aksenov, A.V., Rodin, I.A., Shpigun, O.A., 2016. Identification of barrenwort flavonoids by high-resolution tandem mass spectrometry. J. Anal. Chem. 71, 768–776.
Song, L.J., Zhao, W.C., Zeng, Q.L., Wu, J.D., Li, B.H., 2012. Simultaneous determination of 5 major bioactive components in Hugu Capsule by HPLC-DAD. J. Chin. Med. Mater. 35, 2019–2023.
The State Commission of Chinese Pharmacopoeia, 2010. Chin. Natl. Drug Qual. Stand. 82, 141–143.
Wang, Y.Q., Guo, Z.M., Jin, Y., Zhang, X.L., Wang, L., Xue, X.Y., Liang, X.M., 2010. Identification of prenyl flavonoid glycosides and phenolicacids in Epimedium koreanum Nakai by Q-TOF-MS combined with selective enrichment on “click oligo (ethylene glycol)” column. J. Pharm. Biomed. Anal. 51, 606–616.
Wu, H., Li, X.X., Yan, X.M., An, L., Luo, K.W., Shao, M.J., Jiang, Y., Xie, R., Feng, F., 2015. An untargeted metabolomics-driven approach based on LC-TOF/MS and LC-MS/MS for the screening of xenobiotics and metabolites of Zhi-Zi-Da-Huang decoction in rat plasma. J. Pharm. Biomed. Anal. 115, 315–322.
Xiang, H., Xu, H.Y., Zhan, L.B., 2015. Fingerprint analysis and multi-component determination of Zibu Piyin recipe by HPLC with DAD and Q-TOF/MS method. Nat. Prod. Res. 30, 1081–1084.
Zhao, H.Y., Sun, J.H., Fan, M.X., Fan, L., Zhou, L., Li, Z., Han, J., Wang, B.R., Guo, DA, 2008. Analysis of phenolic compounds in Epimedium plants using liquid chromatography coupled with electrospray ionization mass spectrometry. J. Chromatogr. A 1190, 157–181.
Zhu, M.Q., Wen, J.L, Zhu, Y.H., Su, Y.Q., Sun, R.C., 2016. Isolation and analysis of four constituents from barks and leaves of Eucommia ulmoides Oliver by a multi-step process. Ind. Crops Prod. 83, 124–132.
QR designed and performed the experiments; S-SLong analyzed the data. All authors read and approved the final manuscript.
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The authors declare no conflicts of interest.
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Ren, Q., Long, S. Chemical identification and quantification of Hu-Gu capsule by UHPLC-Q-TOF-MS and HPLC-DAD. Rev. Bras. Farmacogn. 27, 557–563 (2017). https://doi.org/10.1016/j.bjp.2017.06.002
- Hu-Gu capsule