Article pubs.acs.org/IECR
Application of Mechanochemical Pretreatment Prior to Aqueous Extraction of Eleutheroside B from Eleutherococcus senticosus Liji Jin,†,‡ Huaqiang Li,†,‡ Feifei Wu,†,‡ Xiaoyu Li,†,‡ Haibo Yu,§ Naizhong Cui,†,‡ Jiansong You,†,‡ Zhenhui Cao,†,‡ Xiuhua Sun,†,‡ Jiancheng Zhang,†,‡ Xiaoli Wang,†,‡ Chunna Song,†,‡ Shuying Li,∥ and Yongping Xu*,†,‡,§ †
School of Life Science and Biotechnology and ‡Ministry of Education Center for Food Safety of Animal Origin, Dalian University of Technology, Dalian, 116024, China § State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian, 116012, China ∥ Dalian SEM Bio-Engineering Technology Co. Ltd., Dalian 116620, China ABSTRACT: A mechanochemical pretreatment was used prior to aqueous extraction of eleutheroside B from Eleutherococcus senticosus. The effects of the mechanochemical assisted extraction parameters hydroxypropyl-β-cyclodextrin (HP-β-CD) content, particle size, and circulating water temperature on the extraction yield of eleutheroside B were investigated. The mechanochemical assisted extraction process was optimized based on an orthogonal experimental design. The optimum process conditions were a HP-β-CD content of 23% (w/w), a particle size of D95 ≤ 44 μm and circulating water temperature of 40 °C. The mechanochemical assisted extraction process produced a higher eleutheroside B extraction yield, using a shorter extraction time and a greatly simplified process compared with traditional heat-reflux extraction, which makes mechanochemical assisted extraction a potential tool for eleutheroside B extraction from Eleutherococcus senticosus. Moreover, this technique used water as the solvent, making mechanochemical assisted extraction a less expensive and eco-friendly technique compared with traditional heat-reflux extraction.
1. INTRODUCTION Plants contain a diverse group of bioactive substances with a broad range of applications including medicines1−4 and spices.5 Recent advancements in mechanical devices have enabled the development of mechanochemistry as an effective procedure for use in removing bioactive substances from plants.6−10 The technology involves super fine grinding of plant material in the presence of a solid reagent and combines increased totalcontact surface area with destruction of the cell wall.1 Mechanochemical pretreatment also allows chemical transformations of target substances to improve their water solubility.1 The technique has been used to enhance the aqueous extraction yield of triterpene acids from fir needles by 35.9%7 and the extraction of phytoecdysteroids from Serratula coronata L. by 103.7%.8 A previous investigation in our laboratory determined that mechanochemical pretreatment significantly increased the yield of isofraxidin from Eleutherococcus senticosus (E. senticosus) compared with heat-reflux extraction.1 This new application of mechanochemical assisted extraction proved to be an efficient, rapid extraction technique, requiring only the simple process of stirring with water as the only solvent. With an extraction period of approximately 10 min, this simple, user-friendly technique produced 15 to 50% higher yields than were attained by heat-reflux extraction for 2−6 h.1 Eleutheroside B (Figure 1), also known as syringin, is acknowledged as a major active constituent of E. senticosus. Eleutheroside has many functions such as resisting weariness and senescence and restraining tumor growth.11−13 The development of an environmental friendly, low cost extraction © 2012 American Chemical Society
Figure 1. Molecular structure of Eleutheroside B (syringin).
technique with enhanced efficiency would dramatically accelerate the development of an eleutheroside extract industry. Cyclodexrins are oligosaccharides which are produced by enzymatic degradation of starch by a glucosyltransferase most commonly derived from Bacillus macerans.14,15 β-Cyclodextrins contain seven glucose units bound by 1,4-ether linkages. Cyclodextrins are able to incorporate in their structural cavity large organic molecules by noncovalent interaction forces (i.e., hydrogen bonds and van der Waals forces).16 Previous research has suggested that cyclodextrin and its derivatives are useful for improving the solubility of oil-soluble medicines, stabilization, and absorption enhancement, and is also useful as a carrier for rapid-releasing or release-controlling formulations.14,15 The present project was undertaken to adapt the mechanochemical assisted extraction system previously developed for extraction of isofraxidin from E. senticosus1 and modify it for extraction of eleutheroside B from E. senticosus. In addition, experiments were conducted to individually assess Received: Revised: Accepted: Published: 10695
May 17, 2012 July 2, 2012 July 11, 2012 July 11, 2012 dx.doi.org/10.1021/ie301301e | Ind. Eng. Chem. Res. 2012, 51, 10695−10701
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mill, the appropriate amounts of E. senticosus and HP-β-CD were mixed together, and the mixture was subsequently ground. Extraction was conducted as described above. 2.5. Effect of Sample Particle Size on Extraction Efficiency of Eleutheroside. The effects of four sample particle sizes (D95 ≤ 125 μm, ≤ 74 μm, ≤ 44 μm, and ≤37 μm (equivalent to 95% of the total amount passing through a U.S. sieve of No. 120, 200, 325, and 400 respectively) on mechanochemical assisted extraction of Eleutheroside B were investigated by laser particle size analyzer (model LS100Q1, Beckman Counter Inc., Brea, California). Extraction was conducted as described above. 2.6. Effect of Circulating Water Temperature on Extraction Efficiency of Eleutheroside. One gram (based on dry weight) of super finely processed E. senticosus raw material (particle size, D95 ≤44 μm) was mixed with 50 mL of water and decanted into an Erlenmeyer flask (50 or 100 mL capacity) containing a magnetic stir bar. The Erlenmeyer flasks were placed on a stirring hot plate set at 25 °C for a 10 min extraction period. Following extraction, extracts were clarified by centrifugation at 8000 × g for 10 min. Supernatants were evaporated by a rotary evaporator under vacuum at 0, 20, 40, 60, and 80 °C, and the purified eleutheroside B was subsequently obtained. 2.7. Mechanochemical Assisted Extraction Process Optimum. To optimize process conditions, a 3-factor orthogonal array experiment was conducted testing HP-β-CD content, particle size, and circulating water temperature (Table 1). Parallel extraction experiments were performed in triplicate, and extraction yields were determined.
variables of the extraction process to optimize the procedure and compare it against conventional heat-reflux extraction.
2. MATERIAL AND METHODS 2.1. Reagents and Solvents. Standard eleutheroside B (98% purity) was purchased from the Chinese Medical and Biological Products Institute (Beijing, China). Analytical grade hydroxypropyl-β- cyclodextrin (HP-β-CD) was purchased from Tianjin Siyou Biomedical Technology Company (Tianjin, China). 2.2. Plant Material. E. senticosus roots and rhizomes were purchased from a local medicine market (Dalian, China), chopped in a laboratory blender (model FY177, Taisite Instrument Co.,Ltd., Tianjin, China) to an average particle size of 0.05) until 25% HP-β-CD (Figure 3). The present study suggests that 20% HP-β-CD is optimal for mechanochemical assisted extraction of eleutheroside B from E. senticosus.
mg/g) before extraction using the standard optimal conditions as selected above. 2.10. Eleutheroside B Analysis. Residues obtained after extraction were rinsed twice with 5 mL of water and evaporated to dryness, then dissolved in 50 mL of 80% (v/v) aqueous ethanol, filtrated through a 0.45-μm microporous membrane, and analyzed by HPLC using an Agilent 1100 HPLC system with UV detection at 220 nm and an external standard. The mobile phase was water/acetonitrile (15/85) at 1 mL/min. The injection volume was 10 μL. A Kromasil C18 column (250 mm ×4.6 mm, 5 μm, Johnsson Corporation, Dalian, China) was used with the column temperature set at 25 °C. Eleutheroside B peaks were identified by comparing retention times with those of the eleutheroside B standard determined under the same chromatographic conditions. The calibration curve for Eleutheroside B was strictly linear (r2 = 0.99) in the concentration range from 20 to 200 ng per injection. Eleutheroside B yield was calculated using a linear equation and expressed as μg eleutheroside B per gram of dry material. 2.11. Analysis of Target Compound in Extract from Mechanochemical Treatment with HP-β-CD by Mass Spectrometry. Mass spectrometry analysis was performed on a Shimadzu LC-MS 2010A Mass Spectrometer (Kyoto, Japan) with an electrospray ionization source and mass analyzer in both positive and negative ion mode. 2.12. Statistical Analysis. Statistical analysis was performed using SPSS 11.5 for Windows (SPSS Inc. Chicago, Il). All values were expressed as their mean ± standard deviation (SD) and levels of significance were evaluated using one-way ANOVA with the Student-Neuman-Keuls (SNK) test for multiple comparison. The differences were considered significant at the level of p < 0.05.
Figure 3. Effect of HP-β-CD content on the extraction of Eleutheroside B by mechanochemical assisted extraction. E. senticosus material pretreated by WZJ(BFM)-6J with a D95 ≤ 44 μm and extracted using water as the extraction solvent with a 10 min extraction time, a 50:1 (mL/g) liquid/solid ratio and temperature of 25 °C. Data are presented as mean ± SD (n = 3).
3.3. Effect of Sample Particle Size. The effects of four sample particle sizes (D95 ≤ 125 μm, ≤ 74 μm, ≤ 44 μm, and ≤37 μm (equivalent to 95% of the total amount passing through a U.S. sieve of No. 120, 200, 325, and 400 respectively) on mechanochemical assisted extraction of Eleutheroside B were investigated (Figure 4). Reducing particle size to D95 ≤ 44 μm had a strong influence (p < 0.05) on mechanochemical assisted extraction efficiency, increasing eleutheroside B yield by approximately 27.2%, as compared with D95 ≤ 125 μm. Extraction efficiency was not noticeably improved (p > 0.05) beyond D95 ≤ 44 μm. Considering the longer treatment period and higher energy consumption required for continued processing, the particle size of D95 ≤ 44 μm was selected as the standard condition. 3.4. Effect of Circulating Water Temperature. The effects of five circulating water temperatures (0, 20, 40, 60, and
3. RESULTS AND DISCUSSION 3.1. Structural Changes after Pretreatment. To see what alterations were made to the cells by the different pretreatments used for E. senticosus, the samples were examined by SEM (Figure 2). The structures of the rough chopped material in Figure 2A can be compared with those of the mechanical (Figure 2B) or mechanochemical-treated samples (Figure 2C). Rough-chopped material (Figure 2) showed a majority of closed cells and highly rough surfaces. For both mechanical treatment without HP-β-CD and mechanochemical treatment with HP-β-CD (Figures 2B and 2C), no intact cells were observed, indicating a complete breakup of the cell wall after the mechanical activation (particle size, D95 ≤44 μm). 10697
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efficiency in mechanochemical assisted extraction. To optimize the process conditions, a three factor orthogonal array experiments were conducted. The optimal condition of mechanochemical assisted extraction of eleutheroside B shown in Table 2 is A3B2C3 in which A3 denotes the third Table 2. Results of Orthogonal Experiment Designed to Determine the Optimum Process Conditions for Mechanochemical Assisted Extraction
Figure 4. Effect of particle size on the extraction of Eleutheroside B by mechanochemical assisted extraction. E. senticosus material pretreated by WZJ(BFM)-6J, and extracted using 20% (w/w) HP-β-CD, water as the extraction solvent, a 10 min extraction time, a 50:1 (mL/g) liquid/ solid ratio and temperature of 25 °C. Data are presented as mean ± SD (n = 3).
80 °C) in the rotary evaporator on mechanochemical assisted extraction of Eleutheroside B were investigated (Figure 5).
no.
A
B
C
yield (mg/g)
1 2 3 4 5 6 7 8 9 K1 K2 K3 R
17 17 17 20 20 20 23 23 23 1.27 1.39 1.55 0.28
30 40 50 30 40 50 30 40 50 1.36 1.41 1.44 0.08
37 74 44 44 37 74 74 44 37 1.40 1.43 1.38 0.05
4.0 4.4 4.3 4.6 4.5 4.8 5.0 5.2 5.3
level of 23% for HP-β-CD content, B2 denotes the second level of 40 °C for circulating water temperature, and C3 denotes the third level of D95 ≤ 37 μm for particle size. Under optimum process conditions, parallel extraction experiments were performed in triplicate, and extraction yields were 5.3, 5.5, and 5.2 mg/g, respectively. 3.6. Analysis of Target Compound in Treatment with HP-β-CD Extract by Mass Spectrometry. Positive and negative ion mass spectrometry analysis of the target compound isolated from mechanochemical treatment with HP-β-CD extract by semipreparative HPLC is shown in Figure 6. The ion m/z 394.6 corresponding to the pseudomolecular ion of [M + Na]+ in mass spectrometry positive ionization mode and the peak at m/z 406.6 corresponding to [M + Cl]− in mass spectrometry negative ionization mode were observed in the product ion mass spectrum of protonated compound. The mass spectrometry analytical results are consistent with the standard eleutheroside B with M = 372, indicating that eleutheroside B is not chemically altered during the mechanochemical assisted extraction procedure. 3.7. Recovery of Eleutheroside B. The efficacy of the mechanochemical assisted extraction method was determined by spiking previously analyzed samples with known amounts of pure eleutheroside B (0.02, 0.04, and 0.08 mg/g) before extraction using the standard extraction conditions. The recovery of Eleutheroside B ranged from 81.0 to 85.5% (Table 3). Since quantitative recoveries were observed, a matrix effect does not appear to be an issue using the mechanochemical assisted extraction optimal conditions. 3.8. Comparing Mechanochemical Assisted Extraction with Heat-Reflux and Superfine Grinding Extraction. To investigate the unique mechanical and chemical advantages of mechanochemical assisted extraction over the heat-reflux techniques, four processes were compared including pretreatment with normal grinding by a laboratory pulverizer and passed through a 0.25 mm aperture sieve followed by conventional heat-reflux extraction for 3 h with 60% (v/v) ethanol as solvent, superfine grinding extraction using a
Figure 5. Effect of circulating water temperature on the extraction of Eleutheroside B by mechanochemical assisted extraction. E. senticosus material pretreated by WZJ (BFM)-6J, and extracted using 20% (w/w) HP-β-CD, water as the extraction solvent, a 10 min extraction time, a 50:1 (mL/g) liquid/solid ratio, and extraction temperature of 25 °C. Temperature here refers to the temperature in the rotary evaporator. Data are presented as mean ± SD (n = 3). Means with different letter are significantly different (p < 0.05).
Eleutheroside B yield increased from 3.23 mg/g with a temperature of 10 °C (p < 0.05) to 5.04 mg/g with a circulating water temperature of 40 °C and then decreased significantly (p < 0.05). It is suggested that excessively high or low water temperatures do not favor the extraction process. From these observations, a circulating water temperature of 40 °C was selected as the standard condition for mechanochemical assisted extraction of eleutheroside B from E. senticosus. 3.5. Mechanochemical Assisted Extraction Process Optimum. The results of the three experiments conducted above show that HP-β-CD content, particle size, and circulating water temperature are important factors affecting extraction 10698
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Figure 6. Analysis of target compound in mechanochemical treatment with HP-β-CD extract using Mass Spectrometry. The analysis was performed on a Shimadzu LC-MS 2010A Mass Spectrometer (Kyoto, Japan) with an electospray ionization source and mass analyzer in both positive and negative ion mode.
traditional heat-reflux extraction and involved reduced extraction time (Table 4). Adding HP-β-CD after superfine grinding did not improve (p > 0.05) yield, but enabled the use of water as solvent rather than 60% (v/v) ethanol. The mechanochemical assisted extraction process using the optimized parameter settings defined in this study increased (p < 0.05) yield of eleutheroside B by 32.5% over superfine grinding alone and heat-reflux extraction with ethanol as the solvent. The total handling time was reduced from 4 to 1 h, compared with heatreflux extraction. Mechanochemical treatment has found application in diverse areas such as mechanical alloying,17,18 synthesis of organic or inorganic compounds,19−24 denaturation of cellulose,25−27 and decomposition of organic wastes.28,29 The results of this study also demonstrates the potential of this process for extraction of biologically active compound from medical herbs. With the significantly improved yield and simple stirring extraction with water comparing with heat-reflux, the moderate energy consumption during the mechanochemical pretreatment process dose not seems to be a major problem. Besides, the vibrational mill with different scales available also permits the applicability of the technique to a much larger scale, kg or ton.
Table 3. Recoveries of Eleutheroside B from Mechanochemical Assisted Extraction of E. senticosusa eleutheroside B (mg/g dry material) test run.
initial
added
expected
observed
recovery (%)
1 2 3
4.83 4.80 4.77
0.20 0.40 0.80
5.03 5.20 5.57
4.28 ± 0.13 4.45 ± 0.13 4.51 ± 0.09
85.1 ± 2.6 85.5 ± 2.4 81.0 ± 1.7
a The studies were conducted at optimized conditions using superfine powered plant material (D95 ≤ 44 μm) with 20% (w/w) HP-β-CD content, extracted with water using a liquid/solid ratio of 50:1 mL/g for 10 min at 25 °C. Data are presented as mean ± SD (n = 3).
vibrational mill WZJ(BFM)-6J to produce a superfine E. senticosus powder with D95 ≤ 44 μm particle size, extracted by 60% (v/v) aqueous ethanol for 10 min, superfine E. senticosus particles (D95 ≤ 44 μm) mixed with 20% HP-β-CD after grinding and extraction with water for 10 min and finally mechanochemical assisted extraction using the optimized parameter settings of 23% for HP-β-CD content, 40 °C for circulating water temperature, and D95 ≤ 37 μm for particle size (Table 4). Superfine grinding with no HP-β-CD produced a comparable (p > 0.05) yield of eleutheroside B (4.1 vs 4.0 mg/g) to
Table 4. Comparing Mechanochemical Assisted Extraction With Heat-reflux and Superfine Grinding Extractionsa e
sample weight extraction time total handing time solvent solvent volume eleutheroside B yield (mg/g)
heat-reflux extractionb
superfine grindingc
superfine grinding + HP-β-CDd
mechanochemical assisted extractione
1g 3h 4h 60% ethanol 50 mL 4.0 ± 0.4
1g 10 min 1h 60% ethanol 50 mL 4.1 ± 0.3
1g 10 min 1h water 50 mL 4.3 ± 0.6
1g 10 min 1h water 50 mL 5.3 ± 0.3
Data are presented as mean ± SD (n = 3). Means of Eleutheroside B yields without the same letter are significantly different (p < 0.05). bPlant material ground by laboratory pulverizer and passed through a 0.25-mm aperture sieve. cSuperfine ground material with a D95 ≤ 44 μm. dSuperfine ground material with a D95 ≤ 44 μm and 23.0% HP-β-CD content (w/w) added after grinding. eSuperfine ground material with optimized parameter settings of 23% for HP-β-CD content added before grinding, 40 °C for circulating water temperature, and D95 ≤ 37 μm for particle size. a
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International Symposium on Science and Technology, Ulsan, Korea, June 28−July 6, 2003; Vol. 1, pp 7−20. (9) Xie, J.; Li, H. J.; Zhu, X. Y.; Wang, P.; Su, W. K. Efficient and selective extraction of magnolol from Magnolia of f icinalis by mechanochemical extraction technique. Chem. Eng. Process. 2011, 50 (3), 325−330. (10) Zhu, X. Y.; Lin, H. M.; Chen, X.; Xie, J.; Wang, P. Mechanochemical-Assisted Extraction and Antioxidant Activities of Kaempferol Glycosides from Camellia oleifera Abel. Meal. J. Agric. Food Chem. 2011, 59 (8), 3986−3993. (11) Zhang, Y. H.; Sun, L. F.; Shi, W. L.; Wang, Q. C. Syringin content of Acanthopanax senticosus samples in Heilongjiang different zones measuring by HPLC method. Bull. Botanical Res. 2006, 26, 123− 126. (12) Song, Y. Y.; Li, Y.; Zhang, H. Q. Therapeutic effect of syringin on adjuvant arthritis in rats and its mechanism. J. Acta Pharm. Sin. 2010, 45, 1006−1011 (In Chinese). (13) Choi, J.; Shin, K. M.; Park, H. J.; Jung, H. J.; Kim, H. J.; Lee, Y. S.; Rew, J. H.; Lee, K. T. Anti-inflammatory and antinociceptive effects of sinapyl alcohol and its glucociside syringin. Planta Med. 2004, 70, 1027−1032. (14) Van, H. T.; Piel, G.; Evard, B.; Otte, X.; Thunus, L.; Delattre, L. Application of supercritical carbon dioxide for the preparation of a piroxican-B cyclodextrin inclusion compound. Pharm. Res. 1999, 16, 1864−870. (15) Van, H. T.; Evrand, B.; Piel, G.; Delattre, L. Inclusion of piroxicam into β-cylodextrin by means of supercritical carbon dioxide. J. Pharm. Belg. 2000, 55, 30−31. (16) Tang, K.; Cai, J.; Zhang, P. Equilibrium and Kinetics of Reactive Extraction of Ibuprofen Enantiomers from Organic Solution by Hydroxypropyl-β-cyclodextrin.Kewen Tang, Jian Cai, and Panliang Zhang. Ind. Eng. Chem. Res. 2012, 51 (2), 964−971. (17) Shi, Y.; Ding, J.; Tan, S. L. H.; Hu, Z. Ni/Fe2O3 Magnetic Composite Synthesized by Mechanical Alloying. J. Magn. Magn. Mater. 2003, 256, 13−19. (18) Kim, C. W.; Park, J. S.; Lee, K. S. Effect of Fe2P on the Electron Conductivity and Electrochemical Performance of LiFePO4 Synthesized by Mechanical Alloying Using Fe3+ Raw Material. J. Power Sources 2006, 163, 144−150. (19) Lee, J.; Zhang, Q. W.; Saito, F. Mechanochemical Synthesis of Lanthanum Oxyfluoride by Grinding Lanthanum Oxide with Poly (vinylidene fluoride). Ind. Eng. Chem. Res. 2001, 40 (22), 4785−4788. (20) Paneque, A.; Fernández-Bertran, J.; Reguera, E.; Yee-Madeira, H. Mechanochemical Synthesis of Hemin-Imidazole Complexes. Trans. Met. Chem. 2001, 26, 76−80. (21) Wang, J.; Lu, J. F.; Zhang, Q. W.; Saito, F. Mechanochemical Sulfidization of Nonferrous Metal Oxides by Grinding with Sulfur and Iron. Ind. Eng. Chem. Res. 2003, 42 (23), 5813−5818. (22) Onoda, H.; Ohta, T.; Kojima, K. Mechanochemical Reforming of Nickel Pyrophosphate. Mater. Chem. Phys. 2006, 98, 363−367. (23) Lu, J.; Ng, K. M.; Yang, S. Efficient, One-Step Mechanochemical Process for the Synthesis of ZnO Nanoparticles. Ind. Eng. Chem. Res. 2008, 47 (4), 1095−1101. (24) Solihin; Zhang, Q. W.; Tongamp, W.; Saito, F. Mechanochemical Route for Synthesizing KMgPO4 and NH4MgPO4 for Application as Slow-Release Fertilizers. Ind. Eng. Chem. Res. 2010, 49 (5), 2213− 2216. (25) Kokorevics, A.; Gravitis, J. Cellulose Depolymerization to Glucose and Other Water Soluble Polysaccharides by Shear Deformation and High Pressure Treatment. Glycoconjugate J. 1997, 14, 669−676. (26) Yarmukhametova, E. G.; Altunina, L. K.; Tikhonova, L. D. Preparation of Cellulose Ether from Rice Husks. In Proceedings of the 5th Korea-Russia International Symposium on Science and Technology, KORUS 2001, Tomsk, Russia, June 26−July 3, 2001; Vol. 2, pp 150− 153. (27) Tanaka, Y.; Zhang, Q. W.; Saito, F. Mechanochemical Decomposition of an Aromatic Polyamide Film. Ind. Eng. Chem. Res. 2003, 42 (21), 5018−5023.
4. CONCLUSION The effects of various parameters on the efficiency of mechanochemical assisted extraction for eleutheroside B extraction were studied and optimized. The optimum parameters were 23% (w/w) HP-β-CD content, a 40 °C circulating water temperature, and D95 ≤ 37 μm for particle size. The results of mass spectrometry analysis indicate the chemical structure of eleutheroside B is not altered by the extraction process. The mechanochemical assisted extraction process produced a higher eleutheroside B extraction yield, using a shorter extraction time and a greatly simplified process compared with traditional heat-reflux extraction. Moreover, the technique used water as the solvent making mechanochemical assisted extraction, a less expensive and eco-friendly technique. This study suggests that mechanochemical assisted extraction may be an effective way of extracting eleutheroside B from E. senticosus.
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AUTHOR INFORMATION
Corresponding Author
*E-mail:
[email protected]. Phone: 86 411 84706359. Fax: 86 411 84706359. Notes
The authors declare no competing financial interest.
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ACKNOWLEDGMENTS
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REFERENCES
This study was supported by the “863” Program, the HighTech Research and Development Program of China (2006AA10Z412), the National Natural Science Foundation of China (31001053) and the National Outstanding Youth Foundation of China (30125034). The work was also partly supported by the National Innovation Fund for Small Technology-Based Firms of China (06C26222120113). The authors gratefully thank Professor Philip A. Thacker from the University of Saskatchewan for his valuable suggestions and for revising the manuscript.
(1) Liu, Y.; Jin, L. J.; Xu, Y. P. Application of mechanochemical pretreatment to aqueous extraction of isofraxidin from Eleutherococcus Senticosus. Ind. Eng. Chem. Res. 2007, 46 (20), 6584−6589. (2) Lin, Q. Y.; Jin, L. J.; Cao, Z. H.; Li, H. Q.; Xu, Y. P. Protective effect of Acanthopanax senticosus extract against endotoxic shock in mice. J. Ethnopharmacol. 2008, 118 (3), 495−502. (3) Li, H. Q.; Jin, L. J.; Wu, F. F.; Li, X. Y.; You, J. S.; Cao, Z. H.; Li, D.; Xu., Y. P. Effect of curcumin on proliferation, cell cycle, and caspases of MCF-7 cells. Afr. J. Pharm. Pharmacol. 2012, 6 (12), 864− 870. (4) Cao, Z. H.; Gu, D. H.; Lin, Q. Y.; Xu, Z. Q.; Huang, Q. C.; Rao, H.; Liu, E. W.; Jia, J. J.; Ge, C. R. Effect of pu-erh tea on body fat and lipid profiles in rats of diet-induced obesity. Phytother Res. 2011, 25 (2), 234−238. (5) Li, H. Q.; Jin, L. J.; Li, X. Y.; Wu, F. F.; Cao, Z. H.; You, J. S.; Xu, Y. P. The research progress of antibiotics substituted by capsaicin in dietary. China Feed 2011, 451 (23), 23−25 (In Chinese). (6) Boldyrev, V. V.; Tkácǒ vá, K. Mechanochemistry of solids: Past, present, and prospects. J. Mater. Synth. Process. 2000, 8 (3), 121−132. (7) Korolev, K. G.; Lomovskii, O. I.; Rozhanskaya, O. A.; Vasil'ev, V. G. Mechanochemical preparation of water-soluble forms of triterpene acids. Chem. Nat. Compd. 2003, 39, 366−372. (8) Lomovsky, O.; Korolyov, K.; Kwon, Y. S. Mechanochemical solubilization and mechanochemically assisted extraction of plant bioactive substances In Proceedings of the 7th Korean-Russian 10700
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(28) Cao, G.; Doppiu, S.; Monagheddu, M.; Orrù, R.; Sannia, M.; Cocco, G. Thermal and Mechanochemical Self-Propagating Degradation of Chloro-organic Compounds: The Case of Hexachlorobenzene over Calcium Hydride. Ind. Eng. Chem. Res. 1999, 38 (9), 3218−3224. (29) Inoue, T.; Miyazaki, M.; Kamitani, M.; Kano, J.; Saito, F. Dechlorination of Polyvinyl Chloride by Its Grinding with KOH and NaOH. Adv. Powder Technol. 2005, 16, 27−34.
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