Development
of Circulating Ultrasounic-Assisted Online
Extraction Coupled to Countercurrent Chromatography and Centrifugal
Partition Chromatography for Simultaneous Extraction and Isolation
of Phytochemicals: Application to Ligusticum chuanxiong Hort
- Publication date
- Publisher
Abstract
Circulating
ultrasonic-assisted extraction (CUAE) was developed
as a novel method for extraction of medicinal herbs, and the method
was validated. In addition, the novel hyphenated technique comprising
CUAE coupled with countercurrent chromatography (CCC) and centrifugal
partition chromatography (CPC) was developed and applied to the continuous
extraction and online isolation of chemical constituents from Ligusticum chuanxiong Hort. The optimum extraction
parameters, including the extraction time of 30 min, extraction temperature
of 45 °C, ultrasound power of 300 W, and the liquid–solid
ratio of 10 mL/g were determined by response surface methodology.
Furthermore, a schematic and the mechanism of online CUAE coupled
with CCC and CPC were presented. Three lactones, levistolide A (52.2
mg), Z-ligustilide (48.3 mg), and wallichilide (118.2 mg), with respective
purities of 95.8, 96.7, and 96.2%, were obtained from 500 g of the L. chuanxiong raw material using CUAE/CCC. In contrast,
senkyunolide A (26.2 mg), levistolide A (34.2 mg), and wallichilide
(95.1 mg), with respective purities of 96.2, 95.3, and 96.1%, were
obtained from 500 g of the L. chuanxiong raw material by using CUAE/CPC employing the two-phase solvent system
comprising <i>n</i>-hexane–ethyl acetate–methanol–water
in a volume ratio of 4:3:4:2 (v/v). Compared with reference extraction
methods, scientific and systematic extraction and isolation of natural
products was achieved with the instrumental setup, and this system
has great prospects for industrial application, where the combined
use of CCC and CPC can enhance the separation efficiency