Yuan Gao,Yutong Shi,Na Miao,Wenxin Xing,Cholil Yun,Shengfang Wang,Wenjie Wang,Huimei Wang
In this study, a green and efficient ultrasound-assisted enzymatic extraction (UAEE) method was established for total polyphenols (TPP) extraction from E. nigrum aerial parts. Fractional Factorial design (FFD) was initially implemented for the selection of significant parameters affecting TPP yield and then Box-Behnken design-response surface methodology (BBD-RSM) was employed to optimize the parameters. The optimum extraction conditions for UAEE were as follows: incubation temperature of 38.39 ℃, incubation time of 3.39 h, tannase of 386.53 U/g of sample (U/g), and cellulase of 224.42 U/g. Under the optimum conditions, the TPP yield was 52.17 ± 0.39 mg/g, which was 1.62 and 1.73 times those of the methods of ultrasound-assisted extraction (UAE) and enzyme-assisted extraction (EAE), respectively. The crude extract was purified by HPD-600 microporous resin, and the purity was improved from 8.11% to 22.56%. In addition, the results of antioxidant and antibacterial activity assays showed that the purified extract has stronger bioactivities in contrast with the crude extract. This study indicated that UAEE was an effective technique for the extraction of TPP from the aerial parts of E. nigrum , and TPP extracted by this extraction method could be applied in pharmaceuticals, cosmetics, and food industries.
Freeze-ultrasonic thawing extraction (FUTE) is a novel, green, and effective method for extracting bioactive compounds from plants, and the Gemini surfactant had the excellent properties especially for extracting hydrophobic and hydrophilic molecules. Therefore, the purpose of this study was to establish an effective method of synthetic Gemini surfactant aqueous system coupled with FUTE to extract the main individual polyphenols from the aerial parts of Empetrum nigrum. Based on identification of the polyphenols in the aerial parts of E. nigrum by ultra-high-performance liquid chromatography (UHPLC)–time of flight (TOF)–mass spectrometry (MS)/MS, the Gemini surfactant– N , N ʹ-bis(dodecyldimethyl)-1,4-butane dibromide (BBD)–FUTE technology was applied to extract the six main individual polyphenols. Under the optimum conditions, the extraction yields of neochlorogenic acid, catechin, rutin, hyperoside, quercetin, and guaijaverin were 8.48, 0.33, 4.23, 2.19, 1.12, and 0.32 mg/g, respectively, which were 1.01–1.96 and 1.15–2.39 times to those of ultrasonic-assisted extraction and freeze-thawing extraction methods, respectively. After cloud-point extraction, a preconcentration factor of 9.1 was obtained. All the results indicated that BBD-FUTE was a green and efficient method in the extraction of polyphenols from the aerial parts of E. nigrum . Therefore, it was suggested that the BBD-FUTE technology can be used as an alternative innovation method to effectively extract bioactive compounds from plant materials.