Bulletin of the Korean Chemical Society

Korean Chemical Society (대한화학회)
권호 표지
DOI QR코드

DOI QR Code

Simultaneous Determination of Triterpenoid Saponins from Pulsatilla koreana using High Performance Liquid Chromatography Coupled with a Charged Aerosol Detector (HPLC-CAD)

  • Yeom, Hye-Sun (Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University) ;
  • Suh, Joon-Hyuk (Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University) ;
  • Youm, Jeong-Rok (Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University) ;
  • Han, Sang-Beom (Department of Pharmaceutical Analysis, College of Pharmacy, Chung-Ang University)
  • Received : 2010.02.03
  • Accepted : 2010.02.25
  • Published : 2010.05.20
Download PDF
⟨ Previous Next ⟩

Abstract

Several triterpenoid saponins from root of Pulsatilla koreana Nakai (Ranunculaceae) were studied and their biological activities were reported. It is difficult to analyze triterpenoid saponins using HPLC-UV due to the lack of chromophores. So, evaporative light scattering detection (ELSD) is used as a valuable alternative to UV detection. More recently, a charged aerosol detection (CAD) has been developed to improve the sensitivity and reproducibility of ELSD. In this study, we developed and validated a novel method of high performance liquid chromatography coupled with a charged aerosol detector for the simultaneous determination of four triterpenoid saponins: pulsatilloside E, pulsatilla saponin H, anemoside B4 and cussosaponin C. Analytes were separated by the Supelco Ascentis$^{(R)}$ Express C18 column (4.6 mm ${\times}$ 150 mm, 2.7 ${\mu}m$) with gradient elution of methanol and water at a flow rate of 0.8 mL/min at $30^{\circ}C$. We examined various factors that could affect the sensitivity of the detectors, including various concentrations of additives, the pH of the mobile phase, and the CAD range. Linear calibration curves were obtained within the concentration ranges of 2 - 200 ${\mu}g$/mL for pulsatilloside E, anemoside $B_4$ and cussosaponin C, and 5 - 500 ${\mu}g$/mL for pulsatilla saponin H with correlation coefficient ($R^2$) greater than 0.995. The limit of detection (LOD) and quantification (LOQ) were 0.04 - 0.2 and 2 - 5 ${\mu}g$/mL, respectively. The validity of the developed HPLC-CAD method was confirmed by satisfactory values of linearity, intra- and inter-day accuracy and precision. This method could be successfully applied to quality evaluation, quality control and monitoring of Pulsatilla koreana.

Keywords

References

  1. Bae, K. H. The Medicinal Plants of Korea; Kyo-Hak Press: Seoul, 1999, p 139.
  2. Zhang, X. Q.; Liu, A. R.; Xu, L. X. Yao Hsueh Hsueh Pao 1990, 25, 932.
  3. Ye, W. C.; Ou, B. X.; Ji, N. N.; Zhao, S. X.; Ye, T.; McKervey, M. A.; Stevenson, P. Phytochemistry 1995, 39, 937. https://doi.org/10.1016/0031-9422(95)00021-X
  4. Ye, W. C.; Nine, N. J.; Shou, X. Z.; Jing, H. L.; Tao, Y.; McKervey, M. A.; Stevenson, P. Phytochemistry 1996, 42, 799. https://doi.org/10.1016/0031-9422(96)00043-X
  5. Mimaki, Y.; Yokosuka, A.; Kuroda, M.; Hamanaka, M.; Sakuma, C.; Sashida, Y. J. Nat. Prod. 2001, 64, 1226. https://doi.org/10.1021/np010252t
  6. Harinantenaina, L.; Kasai, R.; Yamasaki, K. Chem. Pharm. Bull. 2002, 50, 1290. https://doi.org/10.1248/cpb.50.1290
  7. Bang, S.; Kim, Y.; Lee, J.; Ahn, B. J. Nat. Prod. 2005, 68, 268. https://doi.org/10.1021/np049813h
  8. Kim, Y.; Kim, S.; You, Y.; Ahn, B. Planta Med. 2002, 68, 271. https://doi.org/10.1055/s-2002-23140
  9. Kim, Y.; Bang, S.; Lee, J.; Ahn, B. Arch Pharm. Res. 2004, 27, 915. https://doi.org/10.1007/BF02975843
  10. Bang, S.; Lee, J.; Song, G.; Kim, D.; Yoon, M.; Ahn, B. Chem. Pharm. Bull. 2005, 53, 1451. https://doi.org/10.1248/cpb.53.1451
  11. Han, C.; Park, Y.; Jin, D.; Hwang, Y. K.; Oh, K.; Han, J. Brain Res. 2007, 1184, 254. https://doi.org/10.1016/j.brainres.2007.09.084
  12. Yoo, H. H.; Lee, S. K.; Lim, S. Y.; Kim, Y.; Kang, M. J.; Kim, E. J.; Park, Y. H.; Im, G.; Lee, B. Y.; Kim, D. J. Pharm. Biomed. Anal. 2008, 48, 1425. https://doi.org/10.1016/j.jpba.2008.09.012
  13. Lee, K. Y.; Cho, Y. W.; Park, J.; Lee, D. Y.; Kim, S. H.; Kim, Y. C.; Sung, S. H. Phytochem. Anal. 2010, in press, DOI 10.1002/pca.1201
  14. Cheng, L.; Zhang, M.; Zhang, P.; Song, Z.; Ma, Z.; Qu, H. Rapid Commun. Mass Spectrom. 2008, 22, 3783. https://doi.org/10.1002/rcm.3801
  15. Ganzera, M.; Stuppner, H. Curr. Pharm. Anal. 2005, 1, 135. https://doi.org/10.2174/1573412054022699
  16. Vehovec, T.; Obreza, A. J. Chromatogr. A 2010, 1217, 1549. https://doi.org/10.1016/j.chroma.2010.01.007
  17. Shaodong, J.; Lee, W. J.; Ee, J. W.; Park, J. H.; Kwon, S. W.; Lee, J. J. Pharm. Biomed. Anal. 2010, 51, 973. https://doi.org/10.1016/j.jpba.2009.10.019
  18. Ramos, R. G.; Libong, D.; Rakotomanga, M.; Gaudin, K.; Loiseau, P. M.; Chaminade, P. J. Chromatogr. A 2008, 1209, 88. https://doi.org/10.1016/j.chroma.2008.07.080
  19. Takahashi, K.; Kinugasa, S.; Senda, M.; Kimizuka, K.; Fukushima, K.; Matsumoto, T.; Shibata, Y.; Christensen, J. J. Chromatogr. A 2008, 1193,151. https://doi.org/10.1016/j.chroma.2008.04.012
  20. Pistorino, M.; Pfeifer, B. A. Anal. Bioanal. Chem. 2008, 390, 1189. https://doi.org/10.1007/s00216-007-1774-1
  21. Dixon, R.W.; Peterson, D. S. Anal. Chem. 2002, 74, 2930. https://doi.org/10.1021/ac011208l
  22. Dixon, R.W.; Peterson, D. S. Anal. Chem. 2002, 74, 2930. https://doi.org/10.1021/ac011208l
  23. Kirkland, J. J.; Truszkowski, F. A.; Dilks, C. H.; Engel, G. S. J. Chromatogr. A 2000, 890, 3. https://doi.org/10.1016/S0021-9673(00)00392-7
  24. Abrahim, A.; Al-Sayah, M.; Skrdla, P.; Bereznitski, Y.; Chen, Y.; Wu, N. J. Pharm. Biomed. Anal. 2010, 51, 131. https://doi.org/10.1016/j.jpba.2009.08.023
  25. Zheng, J.; Patel, D.; Tang, Q.; Markovich, R. J.; Rustum, A. M. J. Pharm. Biomed. Anal. 2009, 50, 815. https://doi.org/10.1016/j.jpba.2009.06.042
  26. Song, W.; Pabbisetty, D.; Groeber, E. A.; Steenwyk, R. C.; Fast, D. M. J. Pharm. Biomed. Anal. 2009, 50, 491. https://doi.org/10.1016/j.jpba.2009.05.011
  27. Q2B Text on Validation of Analytical Procedures: Methodology, International Conference on Harmonisation (ICH) Guidelines. 1997.
  28. Sun, P.; Wang, X.; Alquier, L.; Maryanoff, C. A. J. Chromatogr. A 2008, 1177, 87. https://doi.org/10.1016/j.chroma.2007.11.035

Cited by

  1. Qualitative and quantitative determination of nine main active constituents in Pulsatilla cernua by high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry vol.34, pp.3, 2011, https://doi.org/10.1002/jssc.201000660
  2. Anti-Inflammatory and PPAR Transactivational Effects of Oleanane-Type Triterpenoid Saponins from the Roots of Pulsatilla koreana vol.22, pp.4, 2014, https://doi.org/10.4062/biomolther.2014.047
  3. Techniques for the analysis of pentacyclic triterpenoids in medicinal plants pp.16159306, 2017, https://doi.org/10.1002/jssc.201700201
  4. A rapid and sensitive LC‐MS/MS method for the determination of Pulsatilla saponin D in rat plasma and its application in a rat pharmacokinetic and bioavailability study vol.29, pp.3, 2015, https://doi.org/10.1002/bmc.3286
  5. 두릅 추출물의 기능성 원료 표준화를 위한 HPLC 분석법 검증 vol.24, pp.6, 2010, https://doi.org/10.11002/kjfp.2017.24.6.795
  6. Assessment, Validation and Application to Real Samples of an RP-HPLC Method for the Determination of Guayulins A, B, C and D in Guayule Shrub vol.5, pp.2, 2010, https://doi.org/10.3390/separations5020023