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ANALYTICAL SCIENCES · 2025 · IF 2

Confirmation of radicals auto-generated in [Bmim][PF6]/[C16mim][PF6]/water reverse micelles and the radical quantification based on the 1,1-diphenyl-2-picrylhydrazine (DPPHH) spectroscopic probe

Wang Mengge,Chen Xiaofeng,Wang Zhigang,Li Ming

Ionic liquids (ILs) which belong to the molten salt of a high ionic environment exhibit a number of unique properties, including the formation of various heterogeneities in their microemulsion. We found that auto-generated radicals within a [Bmim][PF 6 ]/[C 16 mim][PF 6 ]/PBS reverse micelles (IL-RMs) and then the radicals were quantified in this study. For the radical confirmation, EPR spectroscopy with 5,5-dimethyl-1-pyrroline N-oxide (DMPO) free radical scavenger was carried out. A spectroscopic chemical probe of 1,1-diphenyl-2-picrylhydrazine (DPPHH) was employed to quantify the radicals in the IL-RM systems. The mechanism of the radical generation was also proposed. The DPPHH probe method is simple, rapid, and sensitive to quantify free radicals in the IL-RM systems. Finally, IL-RMs were successfully applied to degrade Rhodamine B (Rho-B) dye with low degradation cost, simple operation, short time consumption, and remarkable degradation effect. The results show a near 100% degradation rate for 10 μmol·L −1 Rho-B in the IL-RMs system with pH 7.4 PBS containing 1 mmol·L −1 chloroacetic acid as an aqueous phase. Graphical abstract

研究领域: 化学 · 环境科学 · 材料科学
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APPLIED BIOCHEMISTRY AND BIOTECHNOLOGY · 2014 ·Vol. 172 ·期 6 ·3287-3296 · IF 1.687

Effect of Chaotropes on Lipase Back Extraction Recovery in the Process of Reverse Micellar Extraction

Yu Tingting,Cao Xuejun

Chaotropes could significantly enhance lipase activity recovery in reverse micellar back extraction. However, the mechanism of chaotropes promoting the release of enzyme from reverse micelles was not clear. In this study, chaotropes were added in the process of lipase reverse micellar extraction, and back extraction recovery was improved. In back extraction, at 0.6 M urea in stripping solution, 94.60 % total extraction recovery was obtained. Meanwhile at 0.3 M guanidine hydrochloride, nearly 65 % lipases were released into the stripping solution. DLS and Karl Fischer method results showed that the presence of urea in stripping solution could weaken the electrostatic interaction between lipase and cetyltrimethylammonium bromide molecules, promoting lipase release from reverse micelles, and guanidine hydrochloride could stimulate lipase and free water molecules enwrapped in reverse micelle release into the stripping solution. These experimental results provide a clue for understanding the mechanism of chaotropes influencing on protein recovery in reverse micelle back extraction.

研究领域: 生物化学 · 酶工程
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FOOD CHEMISTRY · 2025 · IF 9.8

Effects of ferrous ions partitioning at the oil-water interface on the oxidative stability of Antarctic krill (Euphausia superba) oil: Reverse micelles alter the physical location of ferrous ions

Xinmiao Wang,Fawen Yin,Fujun Liu,Qian Wang,Xu Guo,Peiyong Tong,Xiaoyang Liu,Beiwei Zhu,Dayong Zhou

This study investigates the role of ferrous ion partitioning in promoting lipid oxidation in Antarctic krill oil (AKO) containing reverse micelles. Cryogenic transmission electron microscopy and small-angle X-ray scattering confirmed the presence of reverse micelles in AKO. AKO with ferrous sulfate (FeSO 4 , water-soluble iron) and ferrous fumarate (C 4 H 2 FeO 4 , oil-soluble iron) were stored at 60 °C. Interestingly, compared with oil-soluble Fe 2+ , water-soluble Fe 2+ significantly enhanced oxidation. Confocal laser scanning microscopy (CLSM) showed that water-soluble Fe 2+ and lipid hydroperoxides (LOOHs) concentrated at the oil-water interface of reverse micelles, whereas ferrous fumarate was distributed in the oil phase. Meanwhile, water-soluble Fe 2+ significantly promote the oxidation of phospholipids at the oil-water interface, leading to the formation of LOOHs and free radicals that entered the oil phase, triggering glyceride oxidation. Overall, this characterization of the spatial distribution and pro-oxidant effects of metal ions in AKO provides valuable insights into the development of novel antioxidant technologies.

研究领域: 食品科学 · 生物化学 · 材料科学
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CERAMICS INTERNATIONAL · 2019 · IF 3.45

Preparation of γ-Al2O3 membranes for ultrafiltration by reverse micelles-mediated sol-gel process

Hang Qin,Wenming Guo,Hanning Xiao

Sol-gel process was modified by reverse micelles (RMs) for the preparation of γ-Al 2 O 3 ultrafiltration (UF) membranes and their applications in the efficient rejection of methyl blue and bovine serum albumin were explored. The optimized boehmite sol with a narrower particle size distribution and better sphericity was synthesized by using cetyltrimethyl ammonium bromide RMs as microreactors and was dip-coated on α-Al 2 O 3 microfiltration substrates to prepare γ-Al 2 O 3 UF membranes. It was found that not only the sol particle size, it's distribution and morphology had also an important effect on the pore size, pore size distribution , porosity and pore volume of the membrane. Additionally, the as-prepared membranes with a MWCO of 8 kDa exhibited a narrow pore size distribution (4.8–6.8 nm), relatively high pure-water flux (30.4 L/(h m 2  bar)) and excellent rejection for bovine serum albumin and methyl blue with the maximum rejection rate of 96.2% and 96.8% respectively.

研究领域: 材料科学 · 环境工程
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DALTON TRANSACTIONS · 2020 ·Vol. 50 ·期 2 ·562-567 · IF 4.174

Fast and high-yield synthesis of thiolate Ag44 and Au12Ag32 nanoclusters via the CTAB reverse micelle method

Lubing Qin,Feng Zhang,Xiaoshuang Ma,Yun Tang,Guanyu Ma,Zhenghua Tang

To advance the development of atomically precise Ag and Ag-alloyed nanoclusters, it is critical to develop effective synthetic methods. Herein, we successfully extend the CTAB (cetyl trimethyl ammonium bromide) reverse micelle method to synthesize a high-purity Ag44(p-MBA)30 (p-MBA = para-mercaptobenzoic acid) nanocluster and its corresponding alloy cluster Au12Ag32(p-MBA)30 in a short time (15 min and 5 min), with a high yield of ∼83% and ∼85%, respectively. Furthermore, the mechanism regarding the reverse micelle method has been clearly elucidated. Through characterizing the reaction system by Raman spectroscopy and NMR spectroscopy techniques, it can be revealed that employing CTAB to form reverse micelles to construct a sealed chemical environment is critical for realizing the fast and high-yield synthesis.

研究领域: 材料科学 · 化学
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Scientific Reports · 2017 ·Vol. 7 ·期 1 ·1-9 · IF 4.259

A reverse micelle strategy for fabricating magnetic lipase-immobilized nanoparticles with robust enzymatic activity

Yi Shixiong,Dai Fangyin,Zhao Cunyi,Si Yang

Enzyme-immobilized nanoparticles that are both catalysis effective and recyclable would have wide applications ranging from bioengineering and food industry to environmental fields; however, creating such materials has proven extremely challenging. Herein, we present a scalable methodology to create Candida rugosa lipase-immobilized magnetic nanoparticles (L-MNPs) by the combination of nonionic reverse micelle method and Fe 3 O 4 nanoparticles. Our approach causes the naturally abundant and sustainable Candida rugose lipase to ordered-assemble into nanoparticles with high catalytic activity and durability. The resultant L-MNPs exhibit the integrated properties of high porosity, large surface area, fractal dimension, robust enzymatic activity, good durability, and high magnetic saturation (59 emu g −1 ), which can effectively catalyze pentyl valerate esterification and be easily separated by an external magnet in 60 second. The fabrication of such fascinating L-MNPs may provide new insights for developing functional enzyme-immobilized materials towards various applications.

研究领域: 生物工程 · 食品工业 · 环境科学
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APPLIED BIOCHEMISTRY AND BIOTECHNOLOGY · 2020 ·Vol. 192 ·期 2 ·392-414 · IF 2.277

Enzymatic Synthesis of β-Sitosterol Laurate by Candida rugosa Lipase AY30 in the Water/AOT/Isooctane Reverse Micelle

Chen Sunni,Li Jing,Fu Zejian,Wei Guohua,Li Hongyan,Zhang Bin,Zheng Liufeng,Deng Zeyuan

Phytosterols are regarded as compounds able to reduce total and low-density lipoprotein cholesterol in the blood, and their esterified derivatives could help to improve the effectiveness of this function. In the present study, the water/sodium 1,4-bis-2-ethylhexylsulfosuccinate (AOT)/isooctane reverse micelle (RM) system was set up as a reaction medium for Candida rugosa lipase AY30 (CRL AY30) to synthesize β-sitosterol laurate (β-SLE). The product was identified by TLC, FT-IR, and HPLC–APCI–QqQ–MS/MS and quantified by HPLC. Through stepwise optimization, it was found that CRL AY30 had the highest activity in the water/AOT/isooctane RM system where 50 mM PBS with a pH of 7.5 was adopted as water core to carry CRL AY30, and the proportion of [CRL AY30] (mg/mL), [water] (mM), and [AOT] (mM) was set in 3:375:25, respectively, in isooctane. After screened with single-factor experiments, the esterification reaction conditions in the CRL AY30–water/AOT/isooctane RM system were further optimized by the response surface method as follows: the mole ratio of β-sitosterol to lauric acid of 1:3.5 (25 mM β-sitosterol), the enzyme load of 18% (w/w total reactants), the reaction temperature of 47 °C, and the reaction time of 48 h. As a result, the maximum esterification rate was up to 88.12 ± 0.79%.

研究领域: 生物化学 · 食品科学 · 制药工程
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Polymer Chemistry · 2014 ·Vol. 5 ·期 18 ·5300-5309 · IF 5.368

Reverse micelles based on β-cyclodextrin-incorporated amphiphilic polyurethane copolymers for protein delivery

Xiaoxu Du,Nan Song,Ying-Wei Yang,Guolin Wu,Jianbiao Ma,Hui Gao

A series of amphiphilic polyurethane (PU) copolymers were synthesized by a condensation reaction of poly(ethylene glycol) (PEG) of different molecular weights and 1,6-hexamethylene diisocyanate (HDI), with/without end-capped heptakis(2,6-di-O-methyl)-β-cyclodextrin (DM-β-CD). Their chemical structures were characterized by Fourier transform infrared (FT-IR) spectroscopy and proton nuclear magnetic resonance (1H-NMR) spectroscopy. Their molecular weights, thermal properties and crystallization properties were investigated using gel permeation chromatography (GPC) and differential scanning calorimetry (DSC), respectively. A model protein, bovine serum albumin (BSA), was encapsulated into the PU reverse micelles (RMs) with/without DM-β-CD entities using an emulsification method in dichloromethane (DCM), and then further transferred in biocompatible oil, i.e., ethyl oleate. The diameter of RMs in DCM decreased from 180–480 nm to 100–280 nm upon heating, as determined by dynamic light scattering (DLS), and it was spherical in shape, as observed using a scanning electron microscope (SEM). The encapsulation efficiency (EE) and loading capacity (LC) of BSA in the RMs composed of DM-β-CD-containing PUs were much higher than those without DM-β-CD. In vitro release studies showed that the release rate of RMs of DM-β-CD-containing PUs was faster than their counter parts without DM-β-CD. Interestingly, among all the RMs in the present study, the RMs of DM-β-CD-containing PUs composed of the irregular segments of both PEG1000 and PEG2000 exhibited the highest EE and LC, and the fastest release rate of its cargo. These results highlight the ability of RMs of proper PU composition to act as carriers for protein in an oleous phase with good EE and proper release behavior, paving a new way for the application of PU-based RMs in protein or peptide delivery.

研究领域: 材料科学 · 生物医学工程 · 药剂学
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JOURNAL OF HAZARDOUS MATERIALS · 2019 · IF 7.65

Facile inverse micelle fabrication of magnetic ordered mesoporous iron cerium bimetal oxides with excellent performance for arsenic removal from water

Zhipan Wen,Jun Lu,Yalei Zhang,Gang Cheng,Shengnan Huang,Jin Chen,Rui Xu,Yin-an Ming,Yingru Wang,Rong Chen

In this study, magnetic ordered mesoporous Fe/Ce bimetal oxides (OMICs) were successfully synthesized via the modified sol-gel-based inverse micelle method. The textural/structure properties, surface chemistry and adsorption behavior of OMICs could be easily adjusted by using the calcination temperature. The sintering of samples would decrease the surface area, while expand the pore and crystallite size, which resulted in the formation of highly ordered inner-connected structure. Compared with pure mesoporous iron oxides (MI) and mesoporous cerium oxides (MC), this ordered mesoporous iron-cerium bimetal oxides (OMIC-3, 450 °C) exhibited remarkable arsenic adsorption performance. The maximum adsorption capacities of As(III) and As(V) for OMIC-3 were 281.34 and 216.72 mg/g, respectively, and both As(III)/As(V) adsorption kinetics were well described by the pseudo-second order. The ionic strength and coexisting ions (except SiO 3 2− and PO 4 3- ) did not affect arsenic removal, while humic acid (HA) significantly influenced on the arsenic removal even at a lower concentration. The adsorption mechanism study revealed that both the surface charge and surface M-OH groups of OMIC-3 were played the key roles in arsenic removal. The reusable property suggested that this magnetic OMIC-3 was a promising excellent adsorbent for decontamination of arsenic-polluted (especially As(III)-polluted) wastewater.

研究领域: 环境科学 · 材料科学
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HOLZFORSCHUNG · 2019 ·Vol. 74 ·期 5 ·513-521 · IF 2.579

Incorporation of nano lignin reverse micelles on the transparency, UV-blocking and rheological properties of high-density polyethylene films

Yijie Zhou,Yong Qian,Senyi Wu,Xiaowen Zhong,Jinhao Huang,Xueqing Qiu

Aiming to improve the poor miscibility between lignin and non-polar materials, alkali lignin (AL) was self-assembled into lignin reverse micelles (LRM) and blended with high-density polyethylene (HDPE) to fabricate composite films. The particle size of AL increased from 3.5 nm to 130 nm after forming LRM, showing a uniform spherical morphology. The water droplet contact angle increased from 54° to 89°. Optimal and rheological analysis revealed that composite films exhibited good transparency, ultraviolet (UV)-blocking performance and low viscoelasticity after adding the nano LRM. Under the optimal dosage of 5 wt% LRM, the composite film can screen 93% UV rays, and the apparent viscosities, complex viscosities, storage and loss modulus of the mixture were the lowest. Atomic force microscopy (AFM) was used to investigate the molecular interactions between lignin and HDPE. The average adhesion force between LRM and HDPE in dry air was 1.07 mN m −1 , while that between AL and HDPE was 0.77 mN m −1 . AFM experiments fundamentally demonstrated better compatibility between LRM and HDPE, which was beneficial for the improvement of UV-blocking, rheological properties, as well as their processability of LRM/HDPE films.

CAS / MDL: 26062-79-3
研究领域: 材料科学 · 化学工程
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TALANTA · 2018 · IF 4.244

“Inverse” cloud point extraction coupled with large volume injection ion-pair chromatography: A green route integrating extraction, challenging sample cleanup and on-column concentration into fast simple operation

Jiechun Yu,Jianhao Huang,Fei Long,Ande Ma,Jialiang Pan

The efficient isolation of trace hydrophilic compounds from complicated aqueous-rich samples remains a daunting challenge. Herein, to address the analytical bottleneck, a novel inverse cloud-point extraction (ICPE) strategy was proposed based on the extraction principle opposite to that used in traditional CPE. Then, an original large-volume injection ion-pair chromatography (LVI-IPC) method was developed and systematically investigated based on the retention mechanism of the dynamic ion-exchange model. The combined ICPE-LVI-IPC method integrated extraction, challenging sample cleanup, and (on-column) concentration in a fast, simple phase-separation and injection operation. This method was successfully applied to the determination of melamine in dairy samples, including milk, yogurt and milk powder. The organic-solvent-free and sorbent-free sample preparation process could be accomplished within 11 min, requiring only 1.2 mL of water solution per sample. As an efficient on-column concentration strategy, LVI significantly improved the sensitivity. The obtained limit of detection of 0.0028 mg kg −1 was far below the limits established by the Codex Alimentarius Commission . Good recoveries were obtained from samples spiked at four concentration levels (92.6–95.8%), with satisfactory intraday and interday precisions of 1.9–3.9% and 1.6–5.2%, respectively. Further evaluation of the accuracy, by analyzing a certified milk reference material gave a small relative error of 2.2%. Comparisons with a variety of efficient methods showed the superiority of the proposed method in terms of sensitivity, speed, sample and solvent consumption, practicability, and throughput.

CAS / MDL: 7647-14-5
研究领域: 分析化学 · 食品科学 · 色谱学 · 样品制备
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