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. 2014 Jul 7;19(7):9689-711.
doi: 10.3390/molecules19079689.

Ionic liquid-based vacuum microwave-assisted extraction followed by macroporous resin enrichment for the separation of the three glycosides salicin, hyperin and rutin from Populus bark

Fengli Chen  1 , Kailin Mo  2 , Zhaizhi Liu  3 , Fengjian Yang  4 , Kexin Hou  5 , Shuangyang Li  6 , Yuangang Zu  7 , Lei Yang  8
Affiliations

Ionic liquid-based vacuum microwave-assisted extraction followed by macroporous resin enrichment for the separation of the three glycosides salicin, hyperin and rutin from Populus bark

Fengli Chen et al. Molecules. .

Abstract

An effective ionic liquid vacuum microwave-assisted method was developed for extraction of the thermo- and oxygen-sensitive glycosides salicin, hyperin and rutin from Populus bark due to the strong solvating effects of ionic liquids on plant cell walls. In this study, [C4mim]BF4 solution was selected as the extracting solution for extraction of the target analytes. After optimization by single factor experiments and response surface methodology, the optimum condition parameters were achieved, which included 1.0 M [C4mim]BF4, 2 h soaking time, -0.08 MPa vacuum, 20 min microwave irradiation time, 400 W microwave irradiation power and 25 mL/g liquid/solid ratio. Under the optimum conditions, higher extraction yields of salicin (35.53 mg/g), hyperin (1.32 mg/g) and rutin (2.40 mg/g) were obtained. Compared with other extraction methods, the developed method provided higher yields of the three target components after a relatively shorter extraction time (20 min). No obvious degradation of the target analytes was observed under the optimum conditions in performed stability studies and the proposed method had a high reproducibility. Meanwhile, after adsorption and desorption on macroporous D101 resin, the target analytes can be effectively separated from the [C4mim]BF4 ionic liquid extraction solution and the yields of salicin, hyperin and rutin were 89%, 82% and 84%, respectively. The recovered [C4mim]BF4 ionic liquid presented a good extraction effect on the three analytes after recycling five times.

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Conflict of interest statement

The authors declare that there is no conflict of interests regarding the publication of this paper.

Figures

Figure 1
Figure 1
Effect of anion (a) and carbon chain length of cation (b) on the extraction yields of target analytes. All experiments were performed in triplicate.
Figure 2
Figure 2
Optimization of salicin, hyperin and rutin extraction using a factorial design. Effects of ionic liquid concentration (a), soaking time (b), vacuum microwave irradiation power (c), vacuum microwave irradiation time (d), vacuum drgree (e) and liquid/solid ratio (f) on the extraction yields of target analytes. All experiments were performed in triplicate.
Figure 3
Figure 3
Optimization of salicin, hyperin and rutin extraction using BBD. Response surface plots showing the effects of variables on total extraction yield of target analytes. (a) Interaction of vacuum microwave irradiation time and power; (b) Interaction of vacuum microwave irradiation time and liquid/solid ratio; (c) Interaction of vacuum microwave irradiation power and liquid/solid ratio. All experiments were performed in triplicate.
Figure 4
Figure 4
Dynamic desorption curves of ionic liquid and target analytes on a column packed with D101 macroporous resin.
Figure 5
Figure 5
The performance of the recovered [C4mim]BF4 on the yields of salicin, hyperin and rutin.
Figure 6
Figure 6
Scanning electron microscopy images of bark of Poplus alba × P. berolinensis: (a) untreated sample; (b) ILVMAE; (c) ILMAE; (d) ILHRE.
Figure 7
Figure 7
Schematic diagram of the experimental apparatus.
Figure 8
Figure 8
HPLC profile of target analytes in an extract obtained using 1 M C4mimBF4 as extraction solvent.
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