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LANGMUIR · 2023 · IF 3.9

Preparation and Characterization of GX-50 and Vitamin C Co-encapsulated Microcapsules by a Water-in-Oil-in-Water (W1/O/W2) Double Emulsion–Complex Coacervation Method

Ruijuan Wang,Chunliu Ma,Haitao Yan,Pu Wang,Shuyan Yu,Tongyan Zhang,Zhigang Yin

Co-encapsulated xanthoxylin (GX-50) and vitamin C (Vc) microcapsules (GX-50-Vc-M) were prepared by the combination of a water-in-oil-in-water (W1/O/W2) double emulsion with complex coacervation. The W1/O/W2 double emulsion was prepared by two-step emulsification, and it has a uniform particle size of 8.388 μm and high encapsulation efficiencies of GX-50 (85.95%) and Vc (67.35%) under optimized process conditions. Complex coacervation occurs at pHs 4.0–4.7, which has the highest encapsulation efficiency of GX-50 and Vc at pH 4.5. The complex coacervate with tannic acid solidifying (namely, wet microcapsules) has better mechanical properties and also enhances the ability of co-encapsulation of active ingredients. The resulting microcapsules by freeze-drying of wet microcapsules were characterized by UV–vis absorbance spectroscopy (UV–vis), Fourier infrared spectroscopy (FI-IR), confocal laser scanning microscopy (CLSM), scanning electron microscopy (SEM), X-ray diffraction (XRD), 2,2-diphenyl-1-picrylhydrazyl (DPPH·) radical scavenging, and in vitro permeation measurements. Under optimal conditions, the encapsulation efficiency and drug loading of GX-50-Vc-M for GX-50 and Vc are, respectively, 78.38 ± 0.51 and 59.34 ± 0.56%, and 35.6 ± 0.68 and 29.8 ± 0.92%. A slight shift in the FTIR peak between single GX-50 or Vc and GX-50-Vc-M confirmed the successful co-encapsulation of GX-50 and Vc in microcapsules. GX-50-Vc-M has bridged irregular spherical aggregates, while GX-50 and Vc are, respectively, encapsulated in hydrophobic and hydrophilic cavities of microcapsules in an amorphous dissolved state. GX-50-Vc-M has the highest DPPH· radical scavenging rate of 62.51%, and the scavenging process of GX-50-Vc-M on DPPH· radicals is more in line with the pseudo-second-order kinetic equation model. Moreover, the in vitro permeation of GX-50 and Vc in GX-50-Vc-M can reach maximum values of 40 and 60%, respectively. This concludes that GX-50-Vc-M is a promising delivery system for the penetration of the antioxidant into the deeper layers of the skin for the antioxidant effect.

CAS / MDL: 9004-32-4 14263-94-6
研究领域: 药剂学 · 生物化学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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FOOD RESEARCH INTERNATIONAL · 2021 · IF 6.475

Preparation and drying of water-in-oil-in-water (W/O/W) double emulsion to encapsulate soy peptides

Xin Ying,Jiaxing Gao,Jing Lu,Changlu Ma,Jiaping Lv,Benu Adhikari,Bo Wang

Soy peptide solution (40%, w/w) was successfully encapsulated in a W 1 /O/W 2 double emulsion produced by a two-step emulsification process. Polyglycerol polyricinoleate (PGPR) was found to be an effective inner emulsifier compared to Span 60 and lecithin to produce stable W 1 /O primary emulsion. The primary emulsion was subsequently emulsified into an outer aqueous phase (W 2 ) containing octenyl succinic anhydride (OSA) starch and maltodextrin. The droplet size and encapsulation efficiency of the peptide solution in W 1 /O/W 2 emulsion were found to depend on the W 1 :O ratio, peptide concentration in the inner W 1 phase and homogenization condition of the secondary emulsification step. The double emulsion with the highest encapsulation efficiency (>80%) was prepared by: (i) using 40% (w/w) soy peptide solution as W 1 phase; (ii) controlling W 1 :O ratio at 3:7 (w/w) and (iii) homogenizing the emulsion at 10,000 rpm for 3 min. The freeze-dried microcapsule powder of W 1 /O/W 2 emulsion showed higher encapsulation efficiency (>70%) compared to spray-dried one. The freeze-dried microcapsule of W 1 /O/W 2 double emulsion developed in this study is a promising delivery matrix to encapsulate hydrophilic ingredients including peptides. Fourier-transform infrared spectroscopy (FTIR) spectra of the microcapsule powder indicated good compatibility between peptide and encapsulants.

研究领域: 食品科学 · 生物技术
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Analytical Methods · 2024 · IF 2.7

NIR light-triggered bursting of double-emulsion drop (DED) for micro-droplets generation

Zhaoze Lu,Jian Yu,Kaihua Wang,Wei Cheng,Likai Hou

Micro-droplets have significant applications in microbiologies, pharmaceuticals, cosmetics, and synthetic materials. Here, we present for the first time a near-infrared (NIR) light-triggered double-emulsion drop (DED) bursting method for generating a large number of micro-droplets in several micron. Under the irradiation of NIR light, the inner water phase of the DED containing a trace amount of Prussian blue (PB) rapidly heats up and evaporates rapidly to generate microbubbles due to the photothermal property of PB. By controlling the light intensity, the DED can inflate itself by coalescing these constant microbubbles to burst immediately and tear the middle oil phase to form a large number of micro-droplets. The performance of micro-droplets generated by NIR light-triggered DED bursting is investigated at different oil shell thickness (HO), oil phase viscosity (ηO) and oil type. HO and ηO are both key factors affecting the generation of micro-droplets. DED with lower HO and ηO can generate lower polydispersity and large quantity of micro-droplets by NIR-triggered DEDs bursting. The proportion of micro-droplets below 10 μm can reach up to 95%. Furthermore, camellia oil, as middle oil phase of DEDs, also can be used to generate lower polydispersity and large quantity of micro-droplets in several micron. The presented bursting method has a great potential to generate micro-droplets for micro/nano and biotechnology applications.

CAS / MDL: 38215-36-0
研究领域: 微生物学 · 药学 · 合成材料科学 · 生物技术
✓ 已验证 产品关联 DOI PubMed 高影响因子
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JOURNAL OF FOOD ENGINEERING · 2020 · IF 4.499

Microfluidic droplet formation in co-flow devices fabricated by micro 3D printing

Jia Zhang,Wenhua Xu,Fengying Xu,Wangwang Lu,Liuyun Hu,Jianlin Zhou,Chen Zhang,Zhuo Jiang

Droplet microfluidics offer many advantages for microscale droplet generation and have great application potential in food emulsion processing. To employ novel technique to develop microfluidic chips, new devices based on a co-flow regime were fabricated by microscale 3D printing via projection microstereoscopic lithography and were applied to produce single emulsion and double emulsion . The results showed that monodisperse water-in-oil (W/O) and oil-in-water (O/W) single emulsion could be produced in the same device with a coefficient of variation (CV) less than 3%. The parallelized microfluidic device has 5 droplet generators and can generate different types of single emulsions with a CV of approximately 3%. Furthermore, double emulsion droplets could be produced without surface treatment. The development of micro 3D printing provides a new way of microfluidics emulsion formation in food, especially for double emulsion formation, which has the great advantage of no surface treatment. These devices provide considerable support for further commercial application of droplet microfluidics.

研究领域: 食品科学 · 微流体技术 · 生物工程
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INDUSTRIAL & ENGINEERING CHEMISTRY RESEARCH · 2021 · IF 3.764

Toward Understanding the Effect of Solvent Evaporation on the Morphology of PLGA Microspheres by Double Emulsion Method

Wei Si,Qingqing Yang,Yuan Zong,Guobin Ren,Ling Zhao,Minghuang Hong,Zhong Xin

During the fabrication of poly(lactide-co-glycolic acid) (PLGA) microspheres by the water/oil/water (W1/O/W2) emulsion solvent evaporation method, water permeation coupled with dichloromethane (DCM) volatilization represents a critical process affecting the microsphere morphology. In this work, the mechanism of pore formation in PLGA through water permeation has been verified. By molecular simulations, the diffusion coefficients of water with different DCM contents were determined. The results showed that the diffusion coefficient decreased rapidly from 53.33 × 10–6 to 6.73 × 10–6 cm2/s after decreasing the DCM mass fraction from 94 to 63%. Furthermore, the higher stirring speed and lower volume of the external aqueous phase promoted the DCM volatilization. Two different mass transfer stages were identified for water permeation, and the first stage could be considered the main mass transfer window because of its high diffusion coefficient. The morphology of PLGA microspheres confirmed the existence of a relationship between water permeation and DCM volatilization.

CAS / MDL: 9002-89-5
研究领域: 材料科学 · 制药工程
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FOOD HYDROCOLLOIDS · 2025 · IF 12.4

Tethering pH-Induced Structural Modifications of Ovomucin to Stabilize W1/O/W2 Double Emulsions for Enhanced Protection of Companilactobacillus crustorum MN047

Bohan Sun,Youming Liu,Rui Sun,Wei Hu,Yi Hao,Yuanyuan Shan,Pengrui Wu,Charles S. Brennan,Gang Wu,Yanglei Yi,Xin Lü

Ovomucin (OVM) exhibits pH-responsive conformational changes, aggregating under acidic conditions and extending under alkaline conditions, making it a promising stabilizer for double emulsions (DEs) designed to protect probiotics in the gastrointestinal environment. This study presents an OVM-based DE system for the efficient encapsulation and delivery of Companilactobacillus crustorum MN047. The primary W 1 /O emulsion was formed by homogenizing olive oil with 4% PGPR and sodium chloride solution (8:2 ratio), followed by homogenization with 2.5% pH 9 OVM solution (3:7 ratio) to create the DE. Particle size, zeta potential, rheology, and interfacial tension analyses confirmed the stabilizing role of OVM under alkaline conditions, whereas CLSM and circular dichroism revealed the structural effects of OVM, resulting in increased α-helix and decreased β-sheet contents under acidic conditions. DE achieved an encapsulation efficiency of 93.55%, with protection rates of 82.26% in gastric fluid and 66.82% in intestinal fluid. In a dextran sulfate sodium-induced ulcerative colitis mouse model, OVM-encapsulated C. crustorum MN047 demonstrated enhanced effects in inflammation alleviation, intestinal barrier integrity, and gut microbiota regulation. This study underscores the potential of OVM-based DE systems for probiotic oral delivery and introduces an effective encapsulation approach for gastrointestinal applications.

CAS / MDL: 3326-32-7
研究领域: 食品科学 · 微生物学 · 生物化学
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FOOD HYDROCOLLOIDS · 2024 · IF 11

Protection and delivery of probiotics by degraded fucoidan-chitosan nanogel-based W1/O/W2 double emulsion incorporated in self-assembled hydrogel particles

Biyang Zhu,Siyu Guo,Peter Chi-Keung Cheung,Kseniya Hileuskaya,Lijun You

Probiotics as pharmaceutical and nutraceutical products are essential to human health, whereas maintaining their viability in adverse environments remains an obstacle. This study presents a well-designed W 1 /O/W 2 emulsion system incorporated in calcium-alginate hydrogel particles for the targeted delivery and sustained release of Lactobacillus bulgaricus in the gastrointestinal tract. Firstly, the degraded fucoidan (DF) with the highest carboxyl content (2.99%), prepared using UV/H 2 O 2 treatment, was more favorable for forming DF-CS nanogel through ionic cross-linking with chitosan (CS). The W 1 /O/W 2 double emulsion fabricated by 0.4 mg/mL DF-CS nanogel possessed the highest interface stability, as concluded from visual appearance, confocal laser scanning microscope (CLSM), droplet size distribution, and ζ-potential results. The double emulsion loaded in 2% alginate hydrogel showed desirable textural properties and swelling behavior, thereby offering a high encapsulation efficiency of Lactobacillus bulgaricus (74.5%). Additionally, the hydrogel delivery system not only achieved sustained release of Lactobacillus bulgaricus in the simulated gastrointestinal condition (>10 7  CFU/g) but also maintained at least 71.3% and 55.1% survival of probiotics at −20 °C and 4 °C, respectively, after 28 d of long-term storage. Overall, these W 1 /O/W 2 double emulsion-filled multilayer self-assembled hydrogel particles can be utilized for better protection and delivery of probiotics in the food and pharmaceutical industries.

研究领域: 食品科学 · 生物工程 · 药剂学
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REACTIVE & FUNCTIONAL POLYMERS · 2013 · IF 2.505

Multihollow nanocomposite microspheres with tunable pore structures by templating Pickering double emulsions

Shengwen Zou,Hao Liu,Yu Yang,Zengjiang Wei,Chaoyang Wang

Micrometer-sized dual nanocomposite polymer microspheres with tunable pore structures were fabricated using a simple and straightforward method based on Pickering double emulsions . First, a primary water-in-styrene (oil) emulsion (w 1 /o) was prepared using the hydrophobic silica nanoparticles as a particulate emulsifier without any molecular surfactants . Then, a water-in-styrene-in-water (w 1 /o/w 2 ) Pickering emulsion was produced by the emulsification of the primary w 1 /o emulsion into water using Fe 3 O 4 nanoparticles as external emulsifier. The big styrene droplets containing small water droplets were polymerized after the formation of the double emulsions. Nanocomposite polystyrene microspheres with a multihollow structure were obtained and their morphological structures were studied by scanning electron microscopy (SEM). The pore structure of the microspheres could be tuned by the volume ratio of the internal water phase to the medium oil phase (w 1 :o) of the primary emulsions. With increasing w 1 :o from 1:8 to 4:1, the amount of the pores in one microsphere increased gradually and the pore structures changed from close to interconnected. The resulting multihollow microspheres had a responsive ability to magnetic stimulus due to the existence of Fe 3 O 4 nanoparticles. This kind of multihollow hybrid polymer microspheres is expected to have a wide potential application in materials science and biotechnology.

CAS / MDL: 78-67-1
研究领域: 材料科学 · 生物技术
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FOOD RESEARCH INTERNATIONAL · 2022 · IF 7.425

Encapsulation of bitter peptides in diphasic gel double emulsions: Bitterness masking, sustained release and digestion stability

Yi Gao,Xiaoqing Li,Youfa Xie,Xin Huang,Ce Cheng,David Julian McClements,Lu Zhang,Xing Chen,Liqiang Zou,Liu Wei

Bitter peptides (BP) have been reported to exhibit beneficial physiological activities, but their bitter taste and digestive sensitivity currently limits their application in foods . In this study, W1/O/W2 double emulsions were prepared with bitter peptides in the inner water phase. The effects of gelling the inner and/or outer water phases, as well as crystallizing the oil phase, were then investigated. Aqueous phase gelation reduced the particle size of the double emulsions, improved their physical stability, increased their encapsulation efficiency for the bitter peptides, and reduced the bitterness of the peptides. After simulated oral and gastric digestion, the bitter peptide-loaded W1/O droplets in the double emulsions retained their structure, thereby preventing release of the peptides in the mouth and stomach. Our results suggest that gelled double emulsions may have great potential to create more palatable functional foods containing bitter peptides.

研究领域: 食品科学 · 生物技术 · 营养学
✓ 已验证 产品关联 DOI PubMed 高影响因子
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PHYSICS OF FLUIDS · 2023 ·Vol. 35 ·期 12 · IF 4.6

Interface coupling and droplet size under various flow-focusing geometry dimensions in double emulsion formation

Pang Yan,Li Lin,Ru Jiahe,Zhou Qiang,Wang Xiang,Liu Zhaomiao

The application performance of droplets, including the size and core-shell volumetric ratio of a double emulsion droplet, is investigated under various geometric sizes and flow rates in a flow-focusing capillary device. This study uses three-dimensional (3D) printing to create a novel substrate to assemble capillaries and make the inner dimension of the device tunable. Droplet generation is separated into two regions (uniform or non-uniform) based on the interface coupling shapes, where different generation modes are classified based on the rupture form of the multilayer interfaces. A map of the generation modes is established based on geometric size and flow conditions. In the dripping mode, interface coupling and its effect on generation are analyzed by the interface necking process for the two generation sub-modes (with/without a ball). The local capillary number of the double emulsion droplet is established for these sub-modes to analyze variations in the inner droplet volume, which helps propose the volume predictive model of inner and outer droplets.

研究领域: 微流控技术 · 材料科学 · 生物工程
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COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS · 2022 · IF 5.518

Exploration of stabilization mechanism of polyol-in-oil-in-water quercetin-loaded Pickering double emulsions

Rong Liang,Jiahui Yang,Chunhuan Liu,Cheng Yang

The low solubility of quercetin considerably decreases its loading efficiency in traditional water and oil-based emulsion systems, which has limited their applications. To find a solution to this issue, in this investigation, polyol consisting of dipropylene glycol and glycerol as a solvent was used to increase quercetin solubility. It was further incorporated in polyol-in-oil-in-water Pickering double emulsions stabilized by SiO 2 . The characterization of these Pickering double emulsions was performed by analyses of their microscopic structures, particle sizes, rheology, and storage stability. The rise in the concentration of quercetin from 0 to 0.60 wt% decreased the droplet size of these emulsions and increased their viscoelasticity and storage stability. The microstructure of the emulsions showed the presence of some quercetin on the water-oil interface, suggesting that this bioactive compound might have recrystallized from the internal polyol phase during the preparation and then acted as a particle stabilizer in synergy with SiO 2 . To test and validate this hypothesis, we examined the Pickering stabilization properties of the recrystallization quercetin and its interaction with SiO 2 . We found that the recrystallized quercetin interacted with SiO 2 through a hydrogen bond and co-stabilized the interface. Additionally, it also served as a thickener that was involved in the development of an intense entangled network structure that connected the droplets, which improved the emulsion stability. These results revealed an effective approach for the preparation of stable Pickering double emulsions with high quercetin loading.

研究领域: 食品科学 · 材料科学 · 生物化学
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CHEMICAL ENGINEERING JOURNAL · 2024 · IF 13.3

Double emulsion templates for efficient production of phase change microcapsules

Xuexue Xiang,Jing Gao,Fujun Wang,Lu Wang

The utilization of phase change materials (PCMs) in thermal storage technology exhibits great potential for various applications in thermal management and latent heat storage systems. However, leakage of organic PCMs hinders its practical application. Encapsulation of PCMs in microcapsules with polymer shells can prevent PCM leakage while improving heat transfer and stability. In this study, shell monomers were introduced as an immiscible third phase into the traditional o/w two-phase emulsion system, and the formed three-phase complex emulsion was dynamically reconfigured to exhibit a core–shell encapsulated conformation induced by interfacial tension, resulting in the formation of a thermodynamically stable double emulsion. Microcapsules with 1,6-hexanediol diacrylate (HDDA) shells were successfully prepared using this double emulsion as a template. The emulsion configuration is of significant advantage in promoting stable encapsulation of the phase change material in the shell material, resulting in fast and efficient encapsulation and improved utilization of the phase change material. Phase change microcapsules with different phase change temperatures were prepared and characterized using n-octadecane (C 18 ), methyl stearate (Mes), n-eicosane (C 20 ) and n-docosane (C 22 ) as phase change materials, respectively. Results show that the prepared microcapsules are spherically integrated, with smooth surfaces and obvious core–shell structures, and the enthalpies of phase transition of C 18 , Mes, C 20 and C 22 microcapsules are as high as 171.86, 122.37, 165.77 and 178.69 J/g, respectively. These microcapsules exhibit excellent thermal stability and durability and the encapsulation efficiencies exceed 99.7 % at different phase change temperatures. Furthermore, the potential applications of PCM microcapsules in the field of temperature regulation were also demonstrated. This double-emulsion template method provides a straightforward, rapid and scalable approach for the mass production of microcapsules with different core–shell compositions.

CAS / MDL: 57837-19-1 13048-33-4
研究领域: 材料科学 · 化学工程
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