Chemical identification and quantification of Hu-Gu capsule by UHPLC-Q-TOF-MS and HPLC-DAD

Abstract

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.

References

  1. 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.

    CAS  Article  PubMed  Google Scholar 

  2. 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.

    Google Scholar 

  3. 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.

    CAS  Article  Google Scholar 

  4. 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.

    CAS  Article  PubMed  Google Scholar 

  5. 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.

    Google Scholar 

  6. 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.

    CAS  Article  PubMed  Google Scholar 

  7. 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.

    CAS  Article  Google Scholar 

  8. 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.

    CAS  Article  PubMed  Google Scholar 

  9. 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.

    Google Scholar 

  10. 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.

    CAS  Article  Google Scholar 

  11. 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.

    CAS  Google Scholar 

  12. The State Commission of Chinese Pharmacopoeia, 2010. Chin. Natl. Drug Qual. Stand. 82, 141–143.

    Google Scholar 

  13. 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.

    CAS  Article  PubMed  Google Scholar 

  14. 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.

    CAS  Article  PubMed  Google Scholar 

  15. 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.

    Article  PubMed  Google Scholar 

  16. 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.

    CAS  Article  PubMed  Google Scholar 

  17. 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.

    CAS  Article  Google Scholar 

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Correspondence to Qiang Ren or Shi-song Long.

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Authorship

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

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Keywords

  • Hu-Gu capsule
  • UHPLC-Q-TOF-MS
  • HPLC-DAD
  • Identification
  • Quantification