Nat Prod Sci.  2019 Sep;25(3):222-227. 10.20307/nps.2019.25.3.222.

Assessment of the Purity of Emodin by Quantitative Nuclear Magnetic Resonance Spectroscopy and Mass Balance

Affiliations
  • 1Department of Biosystems and Biotechnology, College of Life Sciences and Biotechnology, Korea University, Seoul 02841, Republic of Korea. dongholee@korea.ac.kr
  • 2Graduate School of Pharmaceutical Sciences, College of Pharmacy, Ewha Womans University, Seoul 03760, Republic of Korea.
  • 3Department of Environmental Science and Ecological Engineering, College of Life Sciences and Biotechnology, Korea University, Seoul 02841, Republic of Korea.

Abstract

Quantitative nuclear magnetic resonance (qNMR) is a well-established method adopted by international pharmacopoeia for quantitative and purity analyses. Emodin is a type of anthraquinone, well known as the main active component of Fabaceae, Polygonaceae and Rhamnaceae. Purity analysis of emodin is usually performed by using the high-performance liquid chromatography (HPLC)-UV method. However, it cannot detect impurities such as salts, volatile matter, and trace elements. Using the qNMR method, it is possible to determine the compound content as well as the nature of the impurities. Several experimental parameters were optimized for the quantification, such as relaxation delay, spectral width, number of scans, temperature, pulse width, and acquisition time. The method was validated, and the results of the qNMR method were compared with those obtained by the HPLC and mass balance analysis methods. The qNMR method is specific, rapid, simple, and therefore, a valuable and reliable method for the purity analysis of emodin.

Keyword

qNMR; Emodin; HPLC-UV; Mass balance

MeSH Terms

Chromatography, High Pressure Liquid
Chromatography, Liquid
Emodin*
Fabaceae
Magnetic Resonance Spectroscopy*
Methods
Polygonaceae
Relaxation
Rhamnaceae
Salts
Spectrum Analysis*
Trace Elements
Emodin
Salts
Trace Elements

Figure

  • Fig. 1 The structure of emodin.

  • Fig. 2 The 1H NMR spectrum of emodin and DMSO2 in DMSO-d6.

  • Fig. 3 Test of linearity: gravimetric method and qNMR method of standard solution.


Reference

1. Malz F, Jancke H. J Pharm Biomed Anal. 2005; 38:813–823.
2. Al Deen TS, Hibbert DB, Hook JM, Wells RJ. Anal Chim Acta. 2002; 474:125–135.
3. Al Deen TS, Hibbert DB, Hook JM, Wells RJ. Accred Qual Assur. 2004; 9:55–63.
4. Moura S, Carvalho FG, de Oliveira CDR, Pinto E, Yonamine M. Phytochem Lett. 2010; 3:79–83.
5. Ohtsuki T, Sato K, Sugimoto N, Akiyama H, Kawamura Y. Talanta. 2012; 99:342–348.
6. Izhaki I. New Phytol. 2002; 155:205–217.
7. Cui YT, Liu B, Xie J, Xu P, Habte-Tsion HM, Zhang YY. Fish Shellfish Immunol. 2014; 38:74–79.
8. Gupta SC, Prasad S, Aggarwal BB. Anti-inflammatory Nutraceuticals and Chronic Diseases. Springer: Basel;2016. p. 47–64.
9. Li CL, Ma J, Zheng L, Li HJ, Li P. J Pharm Biomed Anal. 2012; 71:71–78.
10. Simmler C, Napolitano JG, McAlpine JB, Chen SN, Pauli GF. Curr Opin Biotechnol. 2014; 25:51–59.
11. Pauli GF. Phytochem Anal. 2001; 12:28–42.
Article
12. Bharti SK, Roy R. TrAC Trends Anal Chem. 2012; 35:5–26.
13. Saito T, Ihara T, Koike M, Kinugasa S, Fujimine Y, Nose K, Hirai T. Accred Qual Assur. 2009; 14:79–86.
14. Wells R, Cheung J, Hook J. The use of qNMR for the analysis of agrochemicals. Elsevier: Amsterdam;2008. p. 291–315.
Full Text Links
  • NPS
Actions
Cited
CITED
export Copy
Close
Share
  • Twitter
  • Facebook
Similar articles
Copyright © 2024 by Korean Association of Medical Journal Editors. All rights reserved.     E-mail: koreamed@kamje.or.kr