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Large-scale synthesis of polydimethylsiloxane as vitreous replacement applications. 大规模合成聚二甲基硅氧烷作为玻璃体替代品的应用。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2025-01-08 eCollection Date: 2025-01-01 DOI: 10.1080/15685551.2024.2449442
Ajrina Nur Shabrina, Diba Grace Auliya, Risdiana, Lusi Safriani

Polydimethylsiloxane (PDMS) is a polymer that can be used as a vitreous substitute. To fulfill the need for PDMS on a large scale, synthesis of PDMS in a large number is also needed. Therefore, intensive research is needed to produce PDMS in large quantities. This study reported that the result of the synthesis of PDMS on a scale three and five times larger than the lab-scale using a ring-opening polymerization method with octamethylcyclotetrasiloxane (D4) as a monomer and hexamethyldisiloxane as a chain terminator by increasing the volume of raw materials and reactors. The viscosity of PDMS obtained is in the ranges of 1000-3700 mPa.s for lab-scale, 1130-3590 mPa.s for three times scale-up, and 1270-4320 for five times scale-up. The obtained refractive index ranges from 1.3982 to 1.4008 and the surface tension ranges from 20 to 21 mN/m. From FTIR measurements, the synthesized PDMS from lab-scale and scale-up had structural and functional groups similar to commercial PDMS, showing that PDMS has been successfully synthesized.

聚二甲基硅氧烷(PDMS)是一种可用作玻璃体替代物的聚合物。为了满足对 PDMS 的大规模需求,还需要大量合成 PDMS。因此,需要深入研究如何大量生产 PDMS。本研究报告了以八甲基环四硅氧烷(D4)为单体、六甲基二硅氧烷为链终止器的开环聚合法,通过增加原料和反应器的体积,合成出比实验室规模大三倍和五倍的 PDMS 的结果。实验室规模的 PDMS 粘度为 1000-3700 mPa.s,放大 3 倍的粘度为 1130-3590 mPa.s,放大 5 倍的粘度为 1270-4320 mPa.s。获得的折射率范围为 1.3982 至 1.4008,表面张力范围为 20 至 21 mN/m。通过傅立叶变换红外光谱测量,实验室规模和放大规模合成的 PDMS 具有与商用 PDMS 相似的结构和官能团,表明 PDMS 已成功合成。
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引用次数: 0
Mechanically stable polymer networks incorporating polymeric ionic liquids for enhanced conductivity in solid-state electrolytes. 结合聚合物离子液体的机械稳定聚合物网络,增强固态电解质的导电性。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2025-01-07 eCollection Date: 2025-01-01 DOI: 10.1080/15685551.2024.2449444
Sezer Özenler, Nataliya Kiriy, Upenyu L Muza, Martin Geisler, Anton Kiriy, Brigitte Voit

Enhancing both ionic conductivity and mechanical robustness remains a major challenge in designing solid-state electrolytes for lithium batteries. This work presents a novel approach in designing mechanically robust and highly conductive solid-state electrolytes, which involves ionic liquid-based cross-linked polymer networks incorporating polymeric ionic liquids (PILs). First, linear PILs with different side groups were synthesized for optimizing the structure. Molecular weights of the PIL samples, ranging from 30 to 40 kDa, were determined using a complimentary combination of thermal field-flow fractionation (ThFFF) and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) analysis. The aimed for networks were synthesized through the photo-initiated polymerization of a network-forming monomer and a cross-linker, in the presence of lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) and a PIL bearing quaternized imidazolium groups. The resulting cross-linked membranes - semi-interpenetrating networks - exhibit substantial mechanical strength, with a Young's modulus of 40-50 MPa, surpassing the threshold for solid-state battery separators, while maintaining high ionic conductivity in the range of 4 × 10-4 S·cm-1 at 60°C. Notably, the introduction of oligo(ethylene glycol) moieties into the PIL structure significantly enhances ionic conductivity and allows for incorporation of a larger amount of the lithium salt compared to the alkyl-substituted analogs. Moreover, although cross-linking often impairs ionic transport as a result of restricted segmental mobility of the polymer chains, incorporation into the network of highly conductive linear PILs circumvents this issue. This unique combination of properties positions the developed membranes as promising candidates for application in solid-state lithium batteries, effectively addressing the traditional trade-off in electrolyte design.

提高离子电导率和机械稳健性仍然是锂电池固态电解质设计的主要挑战。这项工作提出了一种设计机械坚固和高导电性固态电解质的新方法,该方法涉及基于离子液体的交联聚合物网络,其中包含聚合物离子液体(pil)。首先,为了优化结构,合成了具有不同侧基的线性pil;使用热场流分馏(ThFFF)和基质辅助激光解吸/电离飞行时间质谱(MALDI-TOF MS)分析的互补组合来测定PIL样品的分子量,范围从30到40 kDa。在双(三氟甲烷磺酰)亚胺锂(LiTFSI)和含季铵化咪唑基的PIL的存在下,通过光引发聚合合成了目标网络。所得到的交联膜-半互穿网络-表现出可观的机械强度,杨氏模量为40-50 MPa,超过固态电池隔膜的阈值,同时在60℃下保持4 × 10-4 S·cm-1的高离子电导率。值得注意的是,与烷基取代类似物相比,在PIL结构中引入低聚(乙二醇)基团显著提高了离子电导率,并允许掺入更大量的锂盐。此外,尽管交联通常由于聚合物链的节段迁移率受限而损害离子传输,但将其纳入高导电性线性pil网络中可以规避这一问题。这种独特的性能组合使所开发的膜成为固态锂电池应用的有希望的候选者,有效地解决了电解质设计中的传统权衡。
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引用次数: 0
Advances in bio-polymer coatings for probiotic microencapsulation: chitosan and beyond for enhanced stability and controlled release. 微胶囊益生菌用生物聚合物涂层的研究进展:壳聚糖及壳聚糖外膜增强稳定性和控释。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-12-31 eCollection Date: 2025-01-01 DOI: 10.1080/15685551.2024.2448122
Great Iruoghene Edo, Alice Njolke Mafe, Nawar F Razooqi, Ebuka Chukwuma Umelo, Tayser Sumer Gaaz, Endurance Fegor Isoje, Ufuoma Augustina Igbuku, Patrick Othuke Akpoghelie, Rapheal Ajiri Opiti, Arthur Efeoghene Athan Essaghah, Dina S Ahmed, Huzaifa Umar, Dilber Uzun Ozsahin

This review paper analyzes recent advancements in bio-polymer coatings for probiotic microencapsulation, with a particular emphasis on chitosan and its synergistic combinations with other materials. Probiotic microencapsulation is essential for protecting probiotics from environmental stresses, enhancing their stability, and ensuring effective delivery to the gut. The review begins with an overview of probiotic microencapsulation, highlighting its significance in safeguarding probiotics through processing, storage, and gastrointestinal transit. Advances in chitosan-based encapsulation are explored, including the integration of chitosan with other bio-polymers such as alginate, gelatin, and pectin, as well as the application of nanotechnology and innovative encapsulation techniques like spray drying and layer-by-layer assembly. Detailed mechanistic insights are integrated, illustrating how chitosan influences gut microbiota by promoting beneficial bacteria and suppressing pathogens, thus enhancing its role as a prebiotic or synbiotic. Furthermore, the review delves into chitosan's immunomodulatory effects, particularly in the context of inflammatory bowel disease (IBD) and autoimmune diseases, describing the immune signaling pathways influenced by chitosan and linking gut microbiota changes to improvements in systemic immunity. Recent clinical trials and human studies assessing the efficacy of chitosan-coated probiotics are presented, alongside a discussion of practical applications and a comparison of in vitro and in vivo findings to highlight real-world relevance. The sustainability of chitosan sources and their environmental impact are addressed, along with the novel concept of chitosan's role in the gut-brain axis. Finally, the review emphasizes future research needs, including the development of personalized probiotic therapies and the exploration of novel bio-polymers and encapsulation techniques.

本文综述了近年来用于益生菌微胶囊化的生物聚合物涂层的研究进展,重点介绍了壳聚糖及其与其他材料的协同复合。益生菌微胶囊对于保护益生菌免受环境压力、增强其稳定性和确保有效地递送到肠道至关重要。本文首先概述了益生菌微胶囊技术,强调了微胶囊技术在益生菌加工、储存和胃肠道运输过程中保护益生菌的重要性。探讨壳聚糖基包封的进展,包括壳聚糖与其他生物聚合物如海藻酸盐、明胶和果胶的整合,以及纳米技术和创新包封技术的应用,如喷雾干燥和分层组装。详细的机制见解整合,说明壳聚糖如何通过促进有益菌和抑制病原体影响肠道微生物群,从而增强其作为益生元或合成菌的作用。此外,本综述深入探讨了壳聚糖的免疫调节作用,特别是在炎症性肠病(IBD)和自身免疫性疾病的背景下,描述了壳聚糖影响的免疫信号通路,并将肠道微生物群的变化与全身免疫的改善联系起来。最近的临床试验和人体研究评估壳聚糖包被益生菌的功效,同时讨论了实际应用和体外和体内研究结果的比较,以突出现实世界的相关性。讨论了壳聚糖来源的可持续性及其对环境的影响,以及壳聚糖在肠-脑轴中的作用的新概念。最后,综述了未来的研究需求,包括个性化益生菌疗法的开发以及新型生物聚合物和封装技术的探索。
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引用次数: 0
Fabrication and in vitro evaluation of pH/thermo dual responsive hydrogels as controlled ibuprofen sodium in situ depot. 控制布洛芬钠原位库pH/热双响应水凝胶的制备及体外评价。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-12-30 eCollection Date: 2025-01-01 DOI: 10.1080/15685551.2024.2442118
Samiullah Khan, Abdur Rehman, Syed Faisal Badshah, Gamal A Shazly, Amira Metouekel, Fakhreldeen Dabiellil

Ibuprofen sodium (IBP) is a commonly used NSAID for multiple pain conditions. However, despite its extensive use, it is associated with multiple GIT adverse effects after oral administration. In the present study, we have fabricated thermoresponsive gel depot using Poly (N-vinylcaprolactam) and sodium alginate as polymers. The designed formulations are intended to be used as IBP depot after being administered subcutaneously. The sol-gel phase transition temperature and gelation time of gel samples were optimized by tube inversion, rheological exploration and optical transmittances. Temperature sweep experiments confirmed that optimized gel samples have sol-gel transition between 32°C and 37°C. Swelling and in vitro drug release displayed that optimized gels have maximum swelling and IBP release at pH 7.4 and at 35°C confirming their pH/thermo sensitivity. The degradation profile of hydrogels displayed controlled degradation for 6 days that with increasing contents. MTT assay showed L929 cells displayed more than 90% cell viability against blank and IBP-loaded PNVCL/NaAlg hydrogels at optimized concentrations. Fourier transform infrared spectroscopy confirmed the polymer blend hydrogels structure formation. Thermogravimetric analysis confirmed the presence of thermoresponsive moieties and thermal stability of polymer blend hydrogel sample. While scanning electron microscopy showed that hydrogel has channels in structure that might facilitate the diffusion of solvent. Results concluded that PNVCL/NaAlg hydrogels can be utilized as IBP sustained depot following subcutaneous application invivo and GIT adverse effects could be avoided associated with its oral administration.

布洛芬钠(IBP)是一种常用的非甾体抗炎药,用于治疗多种疼痛。然而,尽管其广泛使用,口服给药后仍与多种GIT不良反应相关。在本研究中,我们以聚(n -乙烯基己内酰胺)和海藻酸钠为聚合物制备了热敏凝胶库。所设计的制剂在皮下给药后用作IBP储存库。通过试管反演、流变学探测和光学透射率等方法对凝胶样品的溶胶-凝胶相变温度和凝胶化时间进行了优化。温度扫描实验证实,优化后的凝胶样品在32℃~ 37℃之间发生溶胶-凝胶转变。溶胀和体外药物释放表明,优化后的凝胶在pH 7.4和35°C时溶胀和IBP释放量最大,证实了其pH/热敏性。随着水凝胶含量的增加,水凝胶在6天内呈现出可控的降解特征。MTT实验显示,在最佳浓度下,L929细胞对空白和负载ibp的PNVCL/NaAlg水凝胶的细胞存活率超过90%。红外光谱傅里叶变换证实了聚合物共混水凝胶的结构形成。热重分析证实了聚合物共混水凝胶样品的热响应部分的存在和热稳定性。扫描电镜显示,水凝胶在结构上具有通道,可能有利于溶剂的扩散。结果表明,PNVCL/NaAlg水凝胶可作为体内皮下应用的IBP持续储存库,且可避免口服引起的胃肠道不良反应。
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引用次数: 0
Synthesis and properties of bio-based semi-aromatic heat-resistant copolymer polyamide 5T-co-6T. 生物基半芳香族耐热共聚物聚酰胺 5T-co-6T 的合成与性能。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-08-11 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2390700
Xiangcheng Bian, Liqun Ma, Chen Yang, Fuchun Zhang, Shuo Zhang, Yuan Li, Kai Gao, Bingxiao Liu, Zhongqiang Wang

Herein, poly(pentanediamine terephthalamide) (PA5T) homopolymer was synthesized via a salt-forming reaction+solid state polycondensation method using bio-based 1,5-pentanediamine and terephthalic acid as the primary raw materials. To address the issue of its narrower processing window, poly(hexamethylene terephthalamide)(PA6T), which also cannot be melt processed due to the processing window is negative, was introduced into its molecular chain to synthesize poly (pentanediamine/hexanediamine terephthaloyl) (PA5T-co-6T) copolymers. The structures were investigated by Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance carbon spectroscopy (13C-NMR). Furthermore, the melting temperature, crystallization temperature, thermal stability, and crystal growth mode of the polymer were tested and analyzed using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and wide-angle x-ray diffraction (WAXD), respectively. The results demonstrate that the crystal growth mode gradually changes from three-dimensional spherical growth to two-dimensional disk-like or three-dimensional spherical growth with the increase of 6T chain segment content. Simultaneously, the crystallization temperature, melting temperature, and crystallization rate of the polymer all showed a trend of decreasing first and then increasing, which was due to the combined effects of the increase in the content of 6T chain segments on the molecular-chain structure and crystal structure of the polymer. Bio-based PA5T-co-6T has excellent heat resistance and a wider processing window than PA5T and PA6T, which possesses great application prospects in the fields of automotive, electronic appliances, and LED optics.

本文以生物基 1,5-戊二胺和对苯二甲酸为主要原料,通过成盐反应+固态缩聚法合成了聚对苯二甲酰对苯二胺(PA5T)均聚物。为了解决其加工窗口较窄的问题,在其分子链中引入了因加工窗口为负值而同样不能熔融加工的聚对苯二甲酰对苯二甲酰胺(PA6T),合成了聚(戊二胺/对苯二甲酰己二胺)(PA5T-co-6T)共聚物。傅立叶变换红外光谱(FTIR)和核磁共振碳谱(13C-NMR)对其结构进行了研究。此外,还分别使用差示扫描量热法(DSC)、热重分析法(TGA)和广角 X 射线衍射法(WAXD)对聚合物的熔化温度、结晶温度、热稳定性和晶体生长模式进行了测试和分析。结果表明,随着 6T 链段含量的增加,晶体生长模式从三维球形生长逐渐转变为二维盘状或三维球形生长。同时,聚合物的结晶温度、熔融温度和结晶速率均呈现先降低后升高的趋势,这是由于 6T 链段含量的增加对聚合物的分子链结构和晶体结构产生了综合影响。与 PA5T 和 PA6T 相比,生物基 PA5T-co-6T 具有优异的耐热性和更宽的加工窗口,在汽车、电子电器和 LED 光学等领域具有广阔的应用前景。
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引用次数: 0
Progress in synthesis, modification, characterization and applications of hyperbranched polyphosphate polyesters. 超支化聚磷酸酯的合成、改性、表征和应用进展。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-07-26 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2376842
Dongyan Hao, Xiaoxiao Guo, Xing Zhu, Chao Wei, Lanchang Gao, Xuechuan Wang

Hyperbranched polyphosphate polyesters (HPPs) as a special class of hyperbranched polymers have attracted increased interest and have been intensively studied, because of peculiar structures, excellent biocompatibility, flexibility in physicochemical properties, biodegradability, water soluble, thermal stability, and mechanical properties. HPPs can be divided into phosphates as monomers and phosphates as end groups. In this article, the classification, general synthesis, modifications, and applications of HPP are reviewed. In addition, recent developments in the application of HPP are described, such as modified or functionalized by end capping and hypergrafting to improve the performances in polymer blends, coatings, flame retardant, leather. Furthermore, the modifications and application of HPPs in biomedical materials, such as drug delivery and bone regeneration were discussed. In summary, the hyperbranched polymer enlarges its application range and improves its application performance compared with conventional polymer. In the future, more new HPPs composite materials will be developed through hyperbranched technique. This review of HPPs will provide useful theoretical basis and technical support for the development of new hyperbranched polymer material.

超支化聚磷酸酯(HPPs)作为一类特殊的超支化聚合物,因其奇特的结构、优异的生物相容性、灵活的理化性质、生物降解性、水溶性、热稳定性和机械性能,引起了越来越多的关注和深入研究。HPPs 可分为作为单体的磷酸盐和作为端基的磷酸盐。本文综述了 HPP 的分类、一般合成、改性和应用。此外,还介绍了 HPP 的最新应用发展,如通过端基封端和超接枝进行改性或功能化,以提高其在聚合物共混物、涂料、阻燃剂和皮革中的性能。此外,还讨论了 HPP 在生物医学材料中的改性和应用,如药物输送和骨再生。总之,与传统聚合物相比,超支化聚合物扩大了应用范围,提高了应用性能。未来,通过超支化技术将开发出更多新型 HPPs 复合材料。本文对 HPPs 的综述将为新型超支化聚合物材料的开发提供有益的理论依据和技术支持。
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引用次数: 0
The effect of polycarboxylate superplasticizer on the strength and hydration performance of alkali slag building materials. 聚羧酸盐超塑化剂对碱渣建材强度和水化性能的影响。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-07-06 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2376780
Guide Liu, Xin Zheng, Guoliang Xie, Gongliang Liu

To explore the effect of polycarboxylate superplasticizers on the strength and hydration performance of alkali slag building materials, this study prepared cross-linked polycarboxylate superplasticizers with different ratios of hydrogen peroxide, methyl allyl alcohol polyoxyethylene ether, acrylic acid, polyethylene glycol diacrylate, monomer aqueous solution, reducing agent, chain transfer agent, etc. according to certain ratios, and tested their effects on the hydration performance and strength of alkali slag building materials. Through experimental analysis, it was found that the higher the proportion of cross-linked polycarboxylate based high-efficiency water-reducing agents, the lower the initial flowability of building material slurry; The addition of cross-linked polycarboxylate water-reducing agent will prolong the initial and final setting time of alkali slag building materials, delaying the hydration time of building materials; Cross linked polycarboxylate superplasticizers can reduce the electrical conductivity of alkali slag building material slurry, delaying its hydration rate; Different ratios of water-reducing agents have a significant impact on the water reduction rate of alkali slag building materials, with V2 water-reducing agent having the highest water-reduction rate of 28.6%; Cross linked polycarboxylate superplasticizers can increase the flexural and compressive strength of alkali slag building materials. Therefore, cross-linked polycarboxylate water-reducing agents have shown great potential in regulating the properties of alkali slag building materials.

为探讨聚羧酸系超塑化剂对碱渣建材强度和水化性能的影响,本研究将过氧化氢、甲基烯丙基醇聚氧乙烯醚、丙烯酸、聚乙二醇二丙烯酸酯、单体水溶液、减水剂、链转移剂等按一定比例配制成交联聚羧酸系超塑化剂,并测试了其对碱渣建材水化性能和强度的影响。通过实验分析发现,交联聚羧酸系高效减水剂的配比越高,建材浆体的初始流动性越低;交联聚羧酸系减水剂的加入会延长碱渣建材的初凝和终凝时间,延缓建材的水化时间;交联聚羧酸盐超塑化剂可降低碱渣建材浆体的导电性,延缓其水化速度;不同配比的减水剂对碱渣建材的减水率有显著影响,其中V2减水剂的减水率最高,为28.6%;交联聚羧酸盐超塑化剂可提高碱渣建材的抗折和抗压强度。因此,交联聚羧酸盐减水剂在调节碱渣建筑材料性能方面显示出巨大潜力。
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引用次数: 0
Ionic Organic Network-based C3-symmetric@Triazine core as a selective Hg+2 sensor. 基于离子有机网络的 C3 对称@三嗪核心作为选择性 Hg+2 传感器。
IF 1.8 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-06-18 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2360746
Maha A Alshubramy, M M Alam, Khalid A Alamry, Abdullah M Asiri, Mahmoud A Hussein, Mohammed M Rahman

The C3-symmetry ionic polymer PPyTri has been designed with multi-walled carbon nanotubes (MWCNTs) or graphene nanoplatelets (GNPs) and studied as an ultrasensitive electrochemical sensor for trace Hg(II) detection. The synthesis approach incorporated attaching three pyridinium cationic components with chloride anions to the triazine core. The precursors, BPy, were synthesized using a condensation process involving 4-pyridine carboxaldehyde and focused nicotinic hydrazide. The polymer PPyTri was further modified with either MWCNTs or GNPs. The resulting ionic polymer PPyTri and its fabricated nanocomposites were characterized using infrared (IR), nuclear magnetic resonance (NMR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and powder X-ray diffraction (XRD). The analysis revealed that both the polymer and its nanocomposites have semi-crystalline structures. The electroactivity of the designed nanocomposites toward Hg + 2 ions revealed that among the nanocomposites and bare copolymer, the glassy carbon electrode (GCE) adapted with the PPyTri GNPs-5% exhibited the greatest current response over a wide range of Hg + 2 concentrations. The nanocomposite-modified electrode presented an excellent sensitivity of 83.33 µAµM - 1 cm - 2, a low detection limit of 0.033 nM, and a linear dynamic range of 0.1 nM to 0.01 mM (R2 = 0.9945).

我们设计了具有多壁碳纳米管(MWCNTs)或石墨烯纳米片(GNPs)的 C3 对称性离子聚合物 PPyTri,并将其作为痕量汞(II)检测的超灵敏电化学传感器进行了研究。合成方法包括在三嗪内核上附加三个带有氯阴离子的吡啶阳离子成分。前体 BPy 是通过 4-吡啶甲醛和烟酸酰肼的缩合过程合成的。聚合物 PPyTri 进一步使用 MWCNTs 或 GNPs 进行改性。利用红外线(IR)、核磁共振(NMR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和粉末 X 射线衍射(XRD)对制备的离子聚合物 PPyTri 及其纳米复合材料进行了表征。分析表明,聚合物及其纳米复合材料都具有半晶体结构。所设计的纳米复合材料对 Hg + 2 离子的电活性表明,在纳米复合材料和裸共聚物中,使用 PPyTri GNPs-5% 的玻璃碳电极(GCE)在 Hg + 2 浓度范围内的电流响应最大。经纳米复合材料改性的电极灵敏度极高,达到 83.33 µAµM - 1 cm - 2,检测限低至 0.033 nM,线性动态范围为 0.1 nM 至 0.01 mM(R2 = 0.9945)。
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引用次数: 0
Cyclodextrin-grafted redox-responsive hydrogel mediated by disulfide bridges for regulated drug delivery. 由二硫桥介导的环糊精接枝氧化还原反应水凝胶用于调节药物输送。
IF 1.6 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-05-30 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2358581
Xin Xu, Jinku Xu, Zeyuan Sun, Derkach Tetiana

In this paper, a novel mono-methacrylated β-cyclodextrin (β-CD) monomer mediated by disulfide bond was synthesized, and then thermal copolymerized with HEMA monomer in the presence of a little crosslinker to prepare redox-responsive hydrogel for regulated drug delivery. The structure of the monomer was confirmed by FTIR, 1H NMR, 13C NMR spectroscopy. The substitution degree of polymerizable methacrylated group grafted onto β-CD was about 1 by calculating by1H NMR (0.987) and element analysis (0.937). The mono-methacrylated β-CD monomer can well copolymerize with 2-hydroxyethyl methacrylate (HEMA) monomer with gel fraction over 80%. The hydrogel shows low cytotoxicity, and copolymerization of the mono-methacrylated β-CD monomer in the hydrogels increases its equilibrium swelling degree (ESD) and tensile strength, while its transmittance slightly decreases. Drug loading and release rate are dependent on the β-CD content. The hydrogel with high β-CD content of 13.83 wt% shows 1.8 and 8.5 folds puerarin (PUE) and curcumin (CUR) loading than pure pHEMA hydrogel, respectively. The incorporation of β-CD sustained drug release, especially CUR release was prolonged more than 24 h from 5 h of pure pHEMA hydrogel (80% release). The hydrogels are highly sensitive to reduced glutathione (GSH), and low concentration of GSH of 3 mM can significantly accelerate drug release rate. The higher of β-CD content, the more sensitive the hydrogels to GSH, resulting in rapider drug release rate.

本文合成了一种以二硫键为介导的新型单甲基丙烯酸酯化β-环糊精(β-CD)单体,然后在少量交联剂存在下与HEMA单体热共聚,制备出氧化还原反应型水凝胶,用于调节药物输送。傅立叶变换红外光谱、1H NMR、13C NMR 光谱证实了单体的结构。通过 1H NMR(0.987)和元素分析(0.937)计算,接枝到 β-CD 上的可聚合甲基丙烯酸酯基团的取代度约为 1。单甲基丙烯酸酯化的 β-CD 单体能很好地与甲基丙烯酸 2-羟乙基酯(HEMA)单体共聚,凝胶率超过 80%。水凝胶的细胞毒性较低,单甲基丙烯酸酯化β-CD单体在水凝胶中的共聚增加了水凝胶的平衡膨胀度(ESD)和拉伸强度,但透光率略有下降。药物负载量和释放速率与 β-CD 含量有关。与纯 pHEMA 水凝胶相比,β-CD 含量高(13.83 wt%)的水凝胶的葛根素(PUE)和姜黄素(CUR)负载量分别增加了 1.8 倍和 8.5 倍。掺入β-CD后,药物释放持续时间延长,尤其是姜黄素的释放时间从纯pHEMA水凝胶的5小时延长到24小时以上(释放率为80%)。水凝胶对还原型谷胱甘肽(GSH)高度敏感,3 mM 的低浓度 GSH 可显著加快药物释放速度。β-CD含量越高,水凝胶对GSH越敏感,药物释放速度越快。
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引用次数: 0
A new polyazomethine-based pyrazole moiety and its reinforced nanocomposites @ ZnO for antimicrobial applications. 一种新型聚氮甲基吡唑分子及其增强纳米复合材料 @ ZnO 用于抗菌应用。
IF 1.6 4区 化学 Q3 POLYMER SCIENCE Pub Date : 2024-05-15 eCollection Date: 2024-01-01 DOI: 10.1080/15685551.2024.2352897
Aqilah A Hakami, Hajar S Alorfi, Thoraya A Farghaly, Mahmoud A Hussein

A new class of biologically active polyazomethine/pyrazole and their related nanocomposites, polyazomethine/pyrazole/zinc oxide nanoparticles, have been successfully synthesized through the polycondensation technique in the form of polyazomethine pyrazole (PAZm/Py4-6) and polyazomethine/pyrazole/zinc oxide nanoparticles (PAZm/Py/ZnOa-c). The polymeric nanocomposites were prepared with a 5% loading of zinc oxide nanofiller using the same preparation technique, in addition to the help of ultrasonic radiation. The characteristics of the new polymers, such as solubility, viscometry, and molecular weight, were examined. All the polymers were completely soluble in the following solvents: concentrated sulfuric acid, formic acid, dimethylformamide, dimethyl sulfoxide, and tetrahydrofuran. Furthermore, the weight loss of the polyazomethine pyrazole (4, 5, and 6) at 800 °C was 67%, 95%, and 86%, respectively, which indicates the thermal stability of these polymers. At 800 °C, the polyazomethine/pyrazole/zinc oxide nanoparticles (a, b, and c) lost 74%, 68%, and 75% of their weight, respectively. This shows that adding zinc oxide nanoparticles made these compounds more stable at high temperatures. The X-Ray diffraction pattern of the polyazomethine pyrazole (PAZm/Py4-6) shows a number of sharp peaks with varying intensities. The polymers that were studied had straight crystal structures. Furthermore, the measurements of polyazomethine/pyrazole/zinc oxide nanoparticles (PAZm/Py/ZnOa-c) indicate a good merging of zinc oxide nanoparticles into the matrix of polymers. The antimicrobial activity of polymers and polymer nanocomposites was tested against some selected bacteria and fungi. The synthesized polymer (c) shows the highest activity against the two types of gram-negative bacteria selected. Most tested compounds were found to be effective against gram-positive bacteria except polyazomethine pyrazole (PAZm/Py5) and polyazomethine pyrazole (PAZm/Py6), which do not exhibit any activity. The synthesized polymers and their related nanocomposites were tested for their ability to kill the chosen fungi. All of them were effective against Aspergillus flavus, but only polyazomethine pyrazole (PAZm/Py4) and polyazomethine/pyrazole/zinc oxide (PAZm/Py/ZnOc) were effective against Candida albicans.

通过缩聚技术,成功合成了具有生物活性的新型聚氮甲胺/吡唑及其相关纳米复合材料--聚氮甲胺/吡唑/氧化锌纳米颗粒,即聚氮甲胺吡唑(PAZm/Py4-6)和聚氮甲胺/吡唑/氧化锌纳米颗粒(PAZm/Py/ZnOa-c)。使用相同的制备技术,并在超声波辐射的帮助下,制备了含有 5% 氧化锌纳米填料的聚合物纳米复合材料。对新聚合物的溶解度、粘度和分子量等特性进行了检测。所有聚合物都能完全溶于以下溶剂:浓硫酸、甲酸、二甲基甲酰胺、二甲亚砜和四氢呋喃。此外,聚氮甲基吡唑(4、5 和 6)在 800 ℃ 时的失重率分别为 67%、95% 和 86%,这表明了这些聚合物的热稳定性。800 °C 时,聚氮甲基吡唑/氧化锌纳米颗粒(a、b 和 c)的重量损失分别为 74%、68% 和 75%。这表明添加纳米氧化锌使这些化合物在高温下更加稳定。聚氮甲基吡唑(PAZm/Py4-6)的 X 射线衍射图样显示出一些强度不同的尖锐峰。所研究的聚合物具有平直的晶体结构。此外,聚氮甲基吡唑/氧化锌纳米颗粒(PAZm/Py/ZnOa-c)的测量结果表明,氧化锌纳米颗粒与聚合物基质的结合良好。测试了聚合物和聚合物纳米复合材料对一些特定细菌和真菌的抗菌活性。合成的聚合物 (c) 对所选的两种革兰氏阴性菌的活性最高。除了聚氮甲基吡唑(PAZm/Py5)和聚氮甲基吡唑(PAZm/Py6)没有表现出任何活性外,大多数测试化合物都对革兰氏阳性细菌有效。对合成的聚合物及其相关纳米复合材料杀死所选真菌的能力进行了测试。所有聚合物都对黄曲霉菌有效,但只有聚氮甲基吡唑(PAZm/Py4)和聚氮甲基/吡唑/氧化锌(PAZm/Py/ZnOc)对白色念珠菌有效。
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引用次数: 0
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Designed Monomers and Polymers
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