Journal List > Nat Prod Sci > v.23(1) > 1060696

TOOLS
Jeong, Choi, Jang, Yoo, Kim, Kim, Kwon, Roh, Yoon, Shin, and Yang: Optimization of Extraction Conditions for Active Compounds of Herbal Medicinal Formula, DF, by Response Surface Methodology
Original Article

Natural Product Sciences 2017;23(1):9-15.

Published online: 20 January 2017

DOI: https://doi.org/10.20307/nps.2017.23.1.9

Optimization of Extraction Conditions for Active Compounds of Herbal Medicinal Formula, DF, by Response Surface Methodology

Birang Jeong1, Seong Yeon Choi1, Hyeon Seok Jang1, Guijae Yoo2, Seung Hyun Kim2, Jung-Hwan Kim3, Yong Soo Kwon1, Jong Seong Roh4, Yoosik Yoon5, Soon Shik Shin4, Heejung Yang1, ∗

1College of Pharmacy, Kangwon National University, Chuncheon 24341, Korea

2College of Pharmacy, Yonsei Institute of Pharmaceutical Science, Yonsei University, Incheon 21983, Korea

3Department of Pharmacology, School of Medicine, Institute of Health Sciences, Gyeongsang National University, Jinju 52727, Korea

4Department of Formula Sciences, College of Korean Medicine, Dong-Eui University, Busan 47227, Korea

5Department of Microbiology, College of Medicine, Chung-Ang University, Seoul 06974, Korea

∗Author for correspondence Heejung Yang, College of Pharmacy, Kangwon National University, Chuncheon 24341, Korea. Tel: +82-33-250-6919; E-mail: heejyang@kangwon.ac.kr

Received 3 August 2016       Revised 5 October 2016       Accepted 6 October 2016

Copyright © 2017 The Korean Society of Pharmacognosy

This is an Open Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

DF formula is comprised of three traditional herbs, Ephedra intermedia, Rheum palmatum and Lithospermum erythrorhizon, and locally used for treating of the metabolic diseases, such as obesity and diabetes in Korea. We tried to optimize the extraction conditions of two major components, (−)-ephedrine and (+)pseudoephedrine, in DF formula using response surface methodology with Box-Behnken design (BBD). The experimental conditions with 70% for EtOH concentrations, 4.8 hour for extraction hours and 8.7 times for the solvent to material ratio were suggested for the optimized extraction of DF formula with the highest amounts of (−)-ephedrine and (+)-pseudoephedrine in the designed model.

Keywords: Response surface methodology, Ephedra intermedia, (−)-ephedrine, (+)-pseudoephedrine, HPLC

References

(1). Uzuner H.., Bauer R.., Fan T. P.., Guo D. A.., Dias A.., El-Nezami H.., Efferth T.., Williamson E. M.., Heinrich M.., Robinson N.., Hylands P. J.., Hendry B. M.., Cheng Y. C.., Xu Q. J.Ethnopharmacol. 2012. 140:458–468.
(2). Ferreira S. L.., Bruns R. E.., da Silva E. G.., Dos Santos W. N.., Quintella C. M.., David J. M.., de Andrade J. B.., Breitkreitz M. C.., Jardim I. C.., Neto B. B. J.Chromatogr. A. 2007. 1158:2–14.
(3). Roman M. C. J.AOAC Int. 2004. 87:1–14.
(4). Ma G.., Bavadekar S. A.., Davis Y. M.., Lalchandani S. G.., Nagmani R.., Schaneberg B. T.., Khan I. A.., Feller D. R. J.Pharmacol. Exp. Ther. 2007. 322:214–221.
(5). Fleming R. M.Expert Opin. Drug Saf. 2008. 7:749–759.
crossref
(6). Stohs S. J.., Badmaev V.Phytother. Res. 2016. 30:732–740.
(7). Pittler M. H.., Schmidt K.., Ernst E.Obes. Rev. 2005. 6:93–111.
(8). Stohs S. J.Plast. Reconstr. Surg. 2013. 132:876e–877e.
(9). Aichner D.., Ganzera M.Talanta. 2015. 144:1239–1244.
(10). Wang H.., Song H.., Yue J.., Li J.., Hou Y. B.., Deng J. L.Cochrane Database Syst. Rev. 2012. CD008000.
(11). Papageorgiou V. P.., Assimopoulou A. N.., Ballis A. C.Curr. Med. Chem. 2008. 15:3248–3267.
(12). Hu Y.., Jiang Z.., Leung K. S.., Zhao Z.Anal. Chim. Acta. 2006. 577:26–31.
(13). Aslan, N; Cebeci Y.Fuel. 2007. 86:90–97.
(14). Schaneberg B. T.., Crockett S.., Bedir E.., Khan I. A.Phytochemistry. 2003. 62:911–918.
(15). Ichikawa M.., Udayama M.., Imamura K.., Shiraishi S.., Matsuura H.Chem. Pharm. Bull. 2003. 51:635–639.

Fig. 1.
HPLC chromatograms of (+)-pseudoephedrine (1), (−)-ephedrine (2) and DF formula. The detailed HPLC conditions described in Experimental section.
nps-23-9f1.tif
Fig. 2.
3D surface plots of the EtOH concentrations versus the extraction hours (a), the EtOH concentrations versus solvent to material ratio (b) and the extraction hours versus solvent to material ratio (c) for the yield of (−)-ephedrine (e), and the EtOH concentrations versus the extraction hours (d), the EtOH concentrations versus solvent to material ratio (e) and the extraction hours versus solvent to material ratio (f) for the yields of (+)-pseudoephedrine.
nps-23-9f2.tif
Table 1.
Experimental design and responses of the dependent variables to extraction conditions
Std ordera Run orderb Coded variables Independent variables Dependent variables (responses)
X1 X2 X3 EtOH concentration (%) Extraction time (hour) Solvent to material ratio (ml/g) EP (mg/g extract) PSEP (mg/g extract)
1 4 1 1 0 70 6.0 10 37.65 6.55
2 1 –1 –1 0 0 1.0 10 37.00 6.10
3 6 1 0 –1 70 3.5 5 37.05 6.45
4 7 –1 0 1 0 3.5 15 36.45 6.20
5 5 –1 0 –1 0 3.5 5 32.75 5.25
6 10 0 1 –1 35 6.0 5 30.80 5.15
7 16 0 0 0 35 3.5 10 35.15 5.95
8 14 0 0 0 35 3.5 10 35.40 6.05
9 13 0 0 0 35 3.5 10 35.65 6.05
10 9 0 –1 –1 35 1.0 5 32.55 5.40
11 17 0 0 0 35 3.5 10 35.05 5.95
12 3 –1 1 0 0 6.0 10 34.25 5.65
13 8 1 0 1 70 3.5 15 35.90 6.65
14 11 0 –1 1 35 1.0 15 34.10 5.85
15 15 0 0 0 35 3.5 10 35.05 5.90
16 12 0 1 1 35 6.0 15 33.60 5.70
17 2 1 –1 0 70 1.0 10 34.75 6.55

a) Randomized,

b) No randomized.

Table 2.
ANOVA for the response surface quadratic model of EPa
  Sum of Squares Mean Square F value p-value
Model 48.9499 5.4389 18.3083 0.0005
X1 3.0013 3.0013 10.1028 0.0155
X2 0.5512 0.5512 1.8556 0.2153
X3 6.1250 6.1250 20.6179 0.0027
X1 X2 8.1225 8.1225 27.3419 0.0012
X1 X3 5.7600 5.7600 19.3893 0.0031
X2 X3 0.3600 0.3600 1.2118 0.3074
X12 12.6381 12.6381 42.5424 0.0003
X22 4.7981 4.7981 16.1514 0.0051
X32 8.7613 8.7613 29.4922 0.0010
Residual 2.0795 0.2971    
Lack of Fit 1.7275 0.5758 6.5436 0.0506
Pure Error 0.3520 0.0880    
R2 0.9592      
Adj. R2 0.9069      

a (−)-ephedrine

Table 3.
ANOVA for the response surface quadratic model of PSEPb
  Sum of Squares Mean Square F value p-value
Model 3.1033 0.3448 79.7255 < 0.0001
X1 1.0952 1.0952 253.2254 < 0.0001
X2 0.0903 0.0903 20.8815 0.0026
X3 0.5886 0.5886 136.0954 < 0.0001
X1 X2 0.0552 0.0552 12.7688 0.0091
X1 X3 0.1406 0.1406 32.5145 0.0007
X2 X3 0.0064 0.0064 1.4798 0.2632
X12 0.7252 0.7252 167.6666 < 0.0001
X22 0.1813 0.1813 41.9166 0.0003
X32 0.2792 0.2792 64.5513 < 0.0001
Residual 0.0303 0.0043    
Lack of Fit 0.0159 0.0053 1.4699 0.3494
Pure Error 0.0144 0.0036    
R2 0.9903      
Adj. R2 0.9779      

b (+)-pseudoephedrine

Table 4.
The comparison between predicted and experimental values.
Parameters Optimum values
Predicted valuesa Experimental valuesb
EtOH concentration (%) 69.73 70.0
Extraction time (hour) 4.83 4.8
Solvent to material ratio (ml/g) 8.73 8.7
Ephedrine (mg/g extract) 37.7 38.4
Pseudoephedrine (mg/g extract) 6.65 7.80
TOOLS
Similar articles