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Journal of Orthopaedic Translation · 2017 · IF 0

Quantitative determination of residual 1,4-dioxane in three-dimensional printed bone scaffold

Ling Li,Jing Long,Long Li,Huijuan Cao,Tingting Tang,Xinghua Xi,Ling Qin,Yuxiao Lai,Xinluan Wang

Summary Background/Objective A novel porous scaffold poly (lactide- co -glycolide) and tricalcium phosphate (PLGA/TCP) was developed by three-dimensional printing technology for bone defect repair. As a Class 2 solvent with less severe toxicity, content of residual 1,4-dioxane in this newly developed scaffold should be rigorously controlled when it is translated to clinical use. In this study, a headspace gas chromatography-mass spectrometric (HS-GC-MS) method and related testing protocol were developed for quantitative determination of 1,4-dioxane in the PLGA/TCP composite scaffolds. Methods Matrix effect analysis was used to optimise the pretreatment method of the scaffolds. Then, the procedure for testing 1,4-dioxane using HS-GC-MS was set up. The accuracy, precision, and robustness of this newly developed quantitative method were also validated before quantification of 1,4-dioxane in the scaffolds with different drying procedures. Results Dimethyl formamide (DMF) was the optimal solvent for dissolving scaffolds for GC-MS with proper sensitivity and without matrix effect. Then, the optimised procedure was determined as: the scaffolds were dissolved in DMF and kept at 90°C for 40 minutes, separated on a HP-5MS column, and detected by mass spectroscopy. Recovery experiments gave 97.9–100.7% recovery for 1,4-dioxane. The linear range for 1,4-dioxane was determined as 1–40 ppm with linear correlation coefficient ≥ 0.9999. Intraday and interday precision was determined as being within relative standard deviation of below 0.68%. The passable drying procedure was related to lyophilising (−50°C, 50 Pa) the scaffolds for 2 days and drying in vacuum (50 Pa) for 7 days. Conclusion This is the first quantitative method established to test 1,4-dixoane in a novel scaffold. This method was validated with good accuracy and reproducibility, and met the methodological requirements of the Guideline 9101 documented in the Chinese Pharmacopoeia 2015 Edition. The translational potential of this article This quantitative method for determination of residual 1,4-dioxane in the novel scaffolds is a key technical method during its translation into clinical use because this method is an important and indispensable file in the enterprise standard when the porous scaffold is registered as a Class III implanted medical device for bone defect repair, which is used to guarantee the safety of the scaffolds. It is also applied to optimise the drying process of scaffolds and to monitor the quality of scaffolds in the industrialisation process. Further, this method provides references for other solvents quantitative determination in porous scaffolds or materials.

研究领域: 生物材料学 · 分析化学 · 医学工程
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MACROMOLECULAR BIOSCIENCE · 2026 ·Vol. 26 ·期 9 ·e70245 · IF 4.2

Functionalized 3D-Printed PCL/β-TCP Scaffolds with ZnO for Enhanced Bone Healing

Ayijiamila Mohetaer,Shan Rong,Zhang Jing,Wang Yuxin,Wan Xiaofei,He Qian,Ma Chunquan,Liu Bin,Song Fuxiang

Alveolar ridge deficiency remains a significant clinical challenge in dental implantology, often necessitating bone augmentation procedures. While autogenous bone grafting is considered the gold standard, its limitations, including donor site complications and limited availability, have prompted the development of alternative bone graft materials. In this study, we fabricated a novel polycaprolactone (PCL)/β-tricalcium phosphate (β-TCP)@zinc oxide (ZnO) composite scaffold via direct ink writing (DIW) three-dimensional (3D) printing. The scaffold integrates a biomimetic porous architecture with a controlled ion-release strategy to enhance osteogenic performance. The characterization of the material confirmed excellent chemical stability, hydrophilicity, and tunable degradation behavior. The incorporation of ZnO facilitated the sustained release of bioactive ions (Ca 2+ , PO 4 3− , and Zn 2+ ), significantly improving the scaffold's bioactivity. In vitro assessments revealed that the scaffold with 2% ZnO (PTZ-2) exhibited optimal cytocompatibility and osteogenic differentiation capacity, promoting alkaline phosphatase activity and mineralized nodule formation in MC3T3-E1 cells. In a rat cranial defect model, the PTZ-2 scaffold achieved approximately 95% new bone area after 12 weeks. Histological analysis further confirmed the presence of continuous, highly mineralized bone matrix with excellent osseointegration capability. These findings collectively indicate that the 3D-printed PCL/β-TCP@ZnO composite scaffold has great potential for clinical translation in bone defect regeneration.

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Journal of Applied Biomaterials & Functional Materials · 2026 · IF 2.9

Preparation and characterization of PCL@β-TCP composite antibacterial scaffolds by additive manufacturing

Chen Zhang,Yi Qi,Binying Dai,Runyi Lin,Jinchao You,Yaomei Wang,Shunxue Xing,Yuansong Ye,De-Jing Li

Poly(ε-caprolactone) (PCL) and β-tricalcium phosphate (β-TCP) are promising materials for bone tissue engineering due to their complementary biodegradability and osteoconductivity. However, their individual limitations hinder clinical application. In this study, PCL@β-TCP composite scaffolds containing 5%, 10%, and 20% β-TCP were fabricated via fused deposition modeling (FDM). The effects of β-TCP content on the physicochemical, mechanical, and antibacterial properties of the scaffolds were systematically investigated. Results showed that increasing β-TCP content enhanced hydrophilicity (contact angle reduced from 89.1° to 66.9°), accelerated biodegradation (higher weight loss after 103 days in PBS), and improved antibacterial activity, as evidenced by larger inhibition zones against E. coli and S. aureus. These findings demonstrate that β-TCP incorporation effectively enhances the bioactivity and antibacterial performance of PCL scaffolds, highlighting their potential for bone tissue engineering applications, particularly in non-load-bearing contexts.

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COLLOIDS AND SURFACES A-PHYSICOCHEMICAL AND ENGINEERING ASPECTS · 2015 · IF 2.752

Factors affecting the physicochemical properties of the modified core/shell NH2–SiO2@NZVI nanoparticles

Zeyu Guan,Yajie Shu,Yongwen Ma,Jinquan Wan

A novel core–shell amino-functionalized silica coated nanoscale zero valent iron (NH 2 –SiO 2 @NZVI) was prepared by the combination of liquid phase reducing method and improved Stöber method. The surface, structure and characteristics of the nanoparticles (NPs) were investigated by transmission electron microscope (TEM), scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and the elemental analysis. It was found that the appropriate dropping rate of NaBF 4 and the proper usage of 3-aminopropyl trimethoxysilane (APTMS) were the crucial and key step for the formation of highly uniform and desirable NH 2 –SiO 2 @NZVI particles. SEM, XRD results showed that the obtained NH 2 –SiO 2 @NZVI NPs has a good dispersibility and antioxidant capacity with the particle size around 120   nm, BET surface area around 123.38   m 2 /g when NaBH 4 dropping speed was 1   ml/min and the usage of APTMS was 0.3   ml/ml tetraethyl orthosilicate (TEOS). NH 2 –SiO 2 @NZVI particles can effectively adsorb TCP with the first-order rate constant k obs of 0.0204   h −1 in 18   h and remove with a removal efficiency of 45.62% in 48   h.

研究领域: 材料科学 · 环境科学
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JOURNAL OF ALLOYS AND COMPOUNDS · 2017 · IF 3.133

PVB modified spherical granules of β-TCP by spray drying for 3D ceramic printing

Yue Ben,Le Zhang,Shuai Wei,Tianyuan Zhou,Zheng Li,Hao Yang,Yun Wang,Farida A. Selim,Chingping Wong,Hao Chen

Monodispersed and spherical β-TCP granules for 3D printing were prepared by spray drying with the surface modification of PVB . Modifier PVB attached to the particle surface to form the crosslinked network structure and keep them combine with each other into aggregates. The morphology, size, forming performance and crushing behavior of granules as well as the microstructure and density of as-fabricated β-TCP ceramics were used to optimize the PVB contents. Promising results could be expected that PVB contents were 1.0 wt.% and the average particle size of granules was 37.36 μm. The modified granules exhibited excellent forming performance with monodispersed and spherical aggregates for 3D printing . They could be completely crushed under 80 MPa without obvious inter-granules void. These granules with 1.0 wt.% PVB had defined strengths for ceramic forming. The good dispersity and flowability assured the high density and uniform porous structure of β-TCP ceramics, which were used as biological ceramic materials and completely met the standard for bone tissue engineering .

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ACS Applied Bio Materials · 2026 · IF 4.7

Digitally Customized 3D PCL/β-TCP Scaffold for Precise Reconstruction of Alveolar Crest Defects

Lei Kang,Chunquan Ma,Xiajie Hu,Xudong Wu,Rong Shan,Fuxiang Song

Bone tissue engineering scaffolds are used to repair dimensional alveolar crest defects resulting from etiologies such as trauma, infection, or tumor resection, thereby enabling a more accurate, efficient, and predictable dental diagnosis and treatment. In this study, cone beam computed tomography (CBCT) data from patients with alveolar crest defects were utilized to design a personalized scaffold. Subsequently, the 3D PCL/β-TCP scaffold was successfully fabricated based on this design using 3D printing technology. In parallel, a comprehensive series of assays were conducted to evaluate the properties of the 3D PCL/β-TCP scaffold, including its ability to promote MC3T3-E1 cell adhesion and proliferation in vitro. Furthermore, its capacity to induce bone formation was assessed in an in vivo animal model. The results demonstrated that the scaffold exhibited excellent biocompatibility, as evidenced by CCK-8 and live/dead (AM/PI) fluorescence staining assays, and significantly facilitated the adhesion and proliferation of MC3T3-E1 cells. Additionally, ALP and Alizarin Red staining experiments indicated that the 3D PCL/β-TCP scaffold significantly enhanced ALP expression and calcified nodule formation. Finally, the in vivo experiments in rats with skull defects confirmed that the 3D PCL/β-TCP scaffold contributed to accelerated bone formation. In summary, owing to numerous favorable properties such as personalized customization, biomimetic porous architecture, and excellent osteogenic ability, the 3D PCL/β-TCP scaffold was confirmed to be an advantageous candidate, offering ideas and effective methods for the precise repair of the alveolar crest.

CAS / MDL: 7758-87-4 75-09-2
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JOURNAL OF BIOMATERIALS SCIENCE-POLYMER EDITION · 2025 · IF 3.6

3D printing of methacrylated hyaluronic acid/α-TCP composite scaffold for bone defect repair

Minjie Shen,Haoran Liu,Zhijia Shen,Yajie Wang,Xiexing Wu,Chunyang Fan,Yongkang Deng,Jinlong Zhang,Liang Hu,Huilin Yang,Chun Liu

Bone defects can occur due to various reasons, such as trauma, infection, congenital disorders, or surgical interventions like tumor removal. This study presents the development and characterization of a novel 3D printable composite ink integrating α-tricalcium phosphate (α-TCP) with a photocuring polymer hyaluronic acid methacrylyol (HAMA) for bone defect repair. The composite bioink was formulated to address the limitations of traditional bioinks and to harness the benefits of α-TCP’s osteoconductivity and the mechanical stability provided by photocuring polymers. The resulting HAMA/α-TCP scaffolds were evaluated for their rheological properties, biocompatibility, mechanical strength, and osteogenic potential both in vitro and in vivo. The study demonstrated that the incorporation of α-TCP into the HAMA matrix significantly enhanced the scaffold’s mechanical properties and osteogenic differentiation capacity. In vivo studies using a rat skull defect model confirmed the superior bone regenerative potential of the HAMA/α-TCP scaffolds compared to controls. The findings suggest that the HAMA/α-TCP composite scaffolds offer a promising approach for bone defect repair, highlighting their potential for clinical translation in orthopedic applications.

CAS / MDL: 60-00-4 760-93-0
研究领域: 生物材料学 · 再生医学 · 骨科
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CHEMOSPHERE · 2019 · IF 5.108

Photochemical reaction of tricresyl phosphate (TCP) in aqueous solution: Influencing factors and photolysis products

Shibin Sun,Jingqiu Jiang,Hongxia Zhao,Huihui Wan,Baocheng Qu

Organophosphate triesters (OPEs) have caused great concern as a class of emerging environmental contaminants due to their widespread use and their toxicity to organisms. However, the phototransformation behavior of OPE is still not fully understood, which is important for understanding their environmental fate . In the present study, the photodegradation of tricresyl phosphate (TCP), one of the most widely detected OPEs in aqueous environments, was investigated including the direct photolysis and in the presence of several natural water factors, NO 2 − , Fe 3+ and humic acid . The degradation process followed the pseudo-first-order kinetics, with rate constant increasing slightly with increasing initial TCP concentration. The presence of NO 2 − and Fe 3+ was observed to promote the photochemical loss of TCP, while humic acid played a negative role on TCP transformation. Electron spin resonance (EPR) analysis showed that carbon-centered radical was produced in the photolysis process of TCP, and hydroxyl radical contributed to the promotion of rate constant for Fe 3+ and NO 2 − . Four photolysis products were tentatively identified by HPLC-LTQ-Orbitrap MS analysis, and the possible degradation pathways of TCP were proposed. These findings provide a meaningful reference for the fate and transformation of OPEs in natural water.

研究领域: 环境科学 · 毒理学
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RSC Advances · 2012 ·Vol. 2 ·期 32 ·12378-12383 · IF 0

Singlet oxygen photogeneration and 2,4,6-TCP photodegradation at Pt/TiO2 under visible light illumination

Xuefeng Hu,Huanhuan Ji,Lei Wu

Pure and Pt nanoparticle-modified rutile TiO2 were synthesized via hydrolysis of TiCl4 in the absence or presence of Pt nanoparticles. HRTEM, XRD, and SEM were used to characterize the structure of the prepared catalysts. The resulting modified TiO2 catalysts show extended visible light absorbance. Photodegradation of 2,4,6-trichlorophenol (2,4,6-TCP) over these photocatalysts was investigated under visible light illumination. The Pt nanoparticles facilitate the separation of photogenerated electron–hole pairs at low Pt content, then enhances the photodegradation rate of 2,4,6-TCP. 0.18Pt–TiO2 achieved the best photocatalytic activity among the tested catalysts. It was found that singlet oxygen rather than ˙OH acts as the main oxidative species for the degradation of 2,4,6-TCP according to the experimental results. The degradation intermediates of 2,4,6-TCP were identified and the degradation pathway was proposed. Pt nanoparticles on TiO2 significantly enhance O2 adsorption and the formation of ˙O2−. The rutile surface is a favorable condition for stabilizing ˙O2−. These properties of the Pt nanoparticle-modified rutile TiO2 facilitate the formation of 1O2via the reaction of superoxide anions with holes.

CAS / MDL: 88-06-2
研究领域: 环境科学 · 材料科学 · 光催化技术
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MATERIALS LETTERS · 2012 · IF 2.307

Fabrication and characterization of porous HA/β-TCP scaffolds strengthened with micro-ribs structure

Quan Wu,Xianglin Zhang,Bin Wu,Wei Huang

The minimal demands for scaffolds include a guaranteed strength over time. In this study, a novel porous HA/β-TCP bioceramic scaffold with micro-ribs structure was fabricated by extrusion deposition technique and microwave sintering. Micro-ribs were placed at the center and corners of scaffold along the direction of load. Mechanical behaviors were studied to verify the strengthening effect of micro-ribs. Compared to the scaffold without micro-ribs, the average compressive strength of newly developed scaffold was remarkably improved from 28.3   MPa to 45.6   MPa under the porosity of 50%. Moreover, it also exhibited more stable and longer lasting mechanical strength during degradation in vitro. The effectiveness of micro-ribs on improving the mechanical performance of scaffolds provided a structural design reference for bone tissue engineering.

CAS / MDL: 9004-65-3 111-87-5
研究领域: 生物材料学 · 骨组织工程
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TALANTA · 2024 · IF 5.6

A cocatalytic nanozyme based on metal-organic framework-embedded iron porphyrin for the sensitive detection of Salmonella typhimurium in milk

Hong Duan,Dongmei Li,Jiali Wang,Yumin Shen,Lingyan Zheng,Xiaolin Huang

The nanozyme, acting as the signal labeling reporter, is widely employed in colorimetric immunoassays due to its exceptional catalytic activity and reliable performance. Nonetheless, when immobilized on the nanozyme's surface, there is a decline in catalytic activity, which hinders its ability to meet the escalating demand for advanced colorimetric immunoassays. Herein, we introduce a novel MILL-88@TcP nanozyme, formed by encapsulating iron porphyrins (TcP) within metal-organic frameworks (MILL-88), where the catalytic activity of TcP is fully preserved through ethanol-induced release. Leveraging the superior encapsulation capacity and enzyme-mimicking characteristics of MILL-88, the MILL-88@TcP nanozyme demonstrates a remarkable colorimetric performance, 1430-fold higher than that of MILL-88 alone. Furthermore, we developed the MILL-88@TcP nanozyme-based Enzyme-Linked Immunosorbent Assay (N-ELISA) for enhanced sensitivity in detecting Salmonella typhimurium , achieving a detection limit of 1.68 × 10 2  CFU/mL, approximately 500-fold enhancement compared to the traditional HRP-based ELISA (8.35 × 10 4  CFU/mL). Notably, the average recoveries ranged from 91.50 % to 108.50 % with a variation of 3.53 %–10.41 %, indicating high accuracy and precision. Collectively, this study highlights that the MILL-88@TcP nanozyme, with its superior catalytic performance and anti-interference capabilities, holds promise as a colorimetric labeling reporter to enhance the detection efficacy of colorimetric immunoassays and has the potential to establish a more stable and sensitive colorimetric assay platform.

CAS / MDL: 7722-84-1 207738-08-7
研究领域: 生物化学 · 食品科学 · 纳米技术 · 免疫学
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CATALYSIS TODAY · 2013 · IF 2.98

Simultaneous photocatalytic Cr(VI) reduction and 2,4,6-TCP oxidation over g-C3N4 under visible light irradiation

Xuefeng Hu,Huanhuan Ji,Fei Chang,Yongming Luo

In this study, a rapid reduction of Cr(VI) and degradation of 2,4,6-trichlorophenol (2,4,6-TCP) in a simultaneous manner was reported through the catalysis of g-C 3 N 4 under visible light ( λ   >   420   nm) irradiation. The effects of initial concentration of reactants, dissolved O 2 and pH value were investigated systematically. It indicated that, under the optimized concentration, the Cr(VI) reduction and 2,4,6-TCP oxidation could be accomplished in couple of hours in the presence of g-C 3 N 4 . And also, the O 2 involvement and low pH value were able to significantly improve the removal rate of Cr(VI) and 2,4,6-TCP. In addition, the reaction mechanism was investigated through monitoring the reduced states of Cr(VI) and active oxygen intermediates formed during photoreaction by ESR and XPS, as well as determining the degradation products of 2,4,6-TCP by HPLC–MS. The results supported that the redox reactions of Cr(VI) and 2,4,6-TCP can be performed simultaneously via a synergistic oxidation–reduction mechanism in the presence of g-C 3 N 4 under visible light irradiation.

研究领域: 环境科学 · 光催化材料
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