scholarly journals Extraction and purification of ustiloxin A from rice false smut balls by a combination of macroporous resin and high-speed countercurrent chromatography

2020 ◽  
Vol 2 (1) ◽  
Author(s):  
Gang Wang ◽  
Dan He ◽  
Fengchun Zhao ◽  
Junqiang Hu ◽  
Yin-Won Lee ◽  
...  

Abstract Rice false smut is an emerging plant disease worldwide. Ustiloxin A (UstA) is the major mycotoxin found in rice false smut balls, which are fungal colonies in rice florets. In this study, a new method consisting of macroporous resin column chromatography and high-speed countercurrent chromatography (HSCCC) was developed for UstA separation. UstA was extracted by a 3.81% HCOOH solution and adsorbed by XAD-4 resin. UstA was then eluted by a 40% methanol solution supplemented with 0.1% trifluoroacetic acid (TFA). Further purification was achieved by HSCCC using a two-phase solvent system consisting of n-butanol/TFA/H2O (1/0.05/1, v/v/v). Under the optimized conditions, 225 mg of UstA was obtained with a purity of 97.39% in a single run, with a final recovery of 65.2%. An inhibitory effect on seed germination of wheat and maize caused by UstA was observed in a preliminary phytotoxicity assay. Graphical abstract

2019 ◽  
Vol 57 (8) ◽  
pp. 738-744 ◽  
Author(s):  
Li-Tao Wang ◽  
Ming-Zhu Gao ◽  
Qing Yang ◽  
Qi Cui ◽  
Yue Jian ◽  
...  

Abstract Morus alba L. is a medicinal plant that contains a high amount of caffeoylquinic acids such as 3-caffeoylquinic acid (3-CQA), 5-caffeoylquinic acid (5-CQA) and 4-caffeoylquinic acid (4-CQA). This study aimed to establish a fast and efficient method for separating caffeoylquinic acids from mulberry leaves by using high-speed countercurrent chromatography coupled with macroporous resin. D101 resin showed better adsorption and desorption capacity for three caffeoylquinic acids among six macroporous resin adsorbents. The contents of 3-CQA, 5-CQA and 4-CQA reached for 4.77%, 18.95% and 9.84% through one cycle of D101 resin, which were 3.13-fold, 4.57-fold and 4.78-fold more than those in crude extracts, respectively. With a two-phase solvent system of ethyl acetate-water (1:1, V/V), >93% purity of target compounds were obtained in one cycle during 150 min with the recovery yields of 80.59%, 99.56% and 94.21% for 3-CQA, 5-CQA and 4-CQA, respectively. The structural identification of target compounds was carried out by ESI-MS, 1H NMR and 13C NMR spectra. The present result represented an easy and efficient separation strategy for the utilization of mulberry resource.


Author(s):  
Zhizhou Zhang ◽  
Yongchao Zhang ◽  
Yichao Wu ◽  
Yongxiang Xu ◽  
Yuanyuan Jiang ◽  
...  

Abstract Background Secoisolariciresinol di glucoside (SDG) is a natural antioxidant generally extracted from flaxseed, which is one of the most important oil crops in China, the by-product of the flaxseed oil, i.e., flaxseed meal, still contains a lot of lignans. However, flaxseed meal is generally treated as waste, resulting in a huge waste of resources. Objective To establish an efficient and convenient method for extraction and purification of lignans from flaxseed meal. Methods First, we used response surface methodology (RSM) to optimize the extraction conditions of the ultrasonic-assisted aqueous two-phase system (UAATPS), and we obtained the purified extracts by macroporous resin purification (MRP). Second, the antioxidant ability of the extracts was studied in vitro. Results The best extraction conditions obtained were as follows: 9.0 wt% sodium hydroxide, 30.0 wt% isopropanol, extraction time 39 min, liquid-to-solid ratio of 52.0 mL/g, ultrasonic wave 560 W, and extraction temperature 40 °C. Under the optimal conditions, the purity of crude extracts (SDG-APTS-C) reached 21.5%. The desorption conditions of MRP were as follows: eluting 3 BV with ultrapure water, and then eluting with 25% ethanol at 2 BV/h to collect eluents. The purified extracts (SDG-ATPS-P) had a purity quotient of 73.9%, 52.4% higher than that of SDG-ATPS-C. Additionally, experiments conducted in this paper revealed that SDG-ATPS-C and SDG-ATPS-P could effectively remove DPPH, ABTS, and hydroxyl free radicals in vitro. Conclusions The method was validated for extracting SDG from flaxseed meal, thus achieving the reuse of flaxseed meal. Highlights This research provides some references for the application of UAATPS combined with MRP in natural products.


Molecules ◽  
2019 ◽  
Vol 24 (21) ◽  
pp. 3956 ◽  
Author(s):  
Lu ◽  
Cui

Capsaicin, which mainly comes from pepper, exhibits anticancer, antioxidant, and anti-obesity properties. This work aims to construct a comprehensive technology for the extraction and purification of capsaicin from capsicum oleoresin. The tunable aqueous polymer phase impregnated HZ816 resins were selected in extraction step. In the extraction process, 3 g of impregnated HZ816 macroporous resin was employed per system. The results showed that a higher molecular weight of Polyethylene glycol (PEG) and 1-ethyl-3-methyl imidazolium acetate ([Emim] [OAc]) are more beneficial to the improvement of the yield of capsaicin. Screening experiment using fractional factorial designs indicated that the amount of sample loading, pH, and concentration of [Emim] [OAc] and PEG 6000 significantly affect the yield of capsaicin. Mathematical models of capsaicin yield in tunable aqueous polymer-phase impregnated resins were established and optimum condition was obtained using response surface methodology. The optimum impregnated phase was the polymer phase of an aqueous two-phase system which contained 18.5% (w/w) PEG6000, 15% (w/w) sodium citrate, and 10% (w/w) [Emim] [OAc] at pH 6.5. Under the optimal conditions, the yield of capsaicin reached 95.82% when the extraction system contains 0.25 g capsicum oleoresin. Ultimately, capsaicinoids extract was purified by reverse-phase resin (SKP-10-4300) chromatographic column. The capsaicin recovery and purity achieved 85% and 92%, respectively.


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