含硅磷酸钙骨水泥的理化性质及体外细胞毒性

用共沉淀反应法制备硅酸三钙(C3S),将所制备的硅酸三钙(C3S)加入到磷酸钙系骨水泥(CPC)中,制备了一种新型的硅磷酸钙骨水泥(CPSC).研究了该复合骨水泥的理化性质和体外细胞毒性.与CPC骨水泥相比,硅磷酸钙骨水泥(CPSC)的固化时间延长,添加适量的C3S可提高CPC的抗压强度;在模拟体液(SBF)浸泡设定时间后,硅磷酸钙骨水泥(CPSC)降解率增加,并且在浸泡初期,SBF的pH增加.体外细胞毒性实验结果显示:复合C3S骨水泥浸提液能促进成纤维细胞的增殖,表明硅磷酸钙骨水泥有良好的生物相容性.含C3S的磷酸钙骨水泥可作为骨组织再生的生物材料使用.     

钙磷物质的量比对磷酸钙骨水泥性能的影响

本研究通过在磷酸钙骨水泥(calcium phosphate cement,CPC)固相配方中添加不同量的氯化钙(CaCl2),制备不同钙磷物质的量比的CPC,研究不同钙磷物质的量比对CPC性能的影响。测试CPC的初、终凝时间。将CPC体外模拟浸泡3d和7d,研究模拟生理条件下CPC的性能,分别利用X-射线衍射(XRD)、力学性能实验机、扫描电镜(SEM)等研究CPC相成分、抗压强度和断面微观形貌。通过化学滴定测定浸泡液中氯离子浓度。结果表明:提高钙磷物质的量比不会显著延长CPC凝结时间;模拟浸泡液中的氯离子浓度处于正常生理条件的范围内;随钙磷物质的量比的增加,水化后CPC的抗压强度显著提高,而经过体外模拟浸泡后,钙磷物质的量比为1.67和1.80的CPC的抗压强度明显下降;具有较高钙磷物质的量比的CPC体外模拟浸泡后,形成多孔结构、弱结晶类骨磷灰石的终产物。     

N掺杂TiO2对聚乙烯复合薄膜的光催化降解研究

以快速溶胶-凝胶法制备了具有不同N掺杂量的TiO2光催化剂,在室温光照240 h条件下,用于固相光催化降解碳酸钙填充聚乙烯复合材料薄膜;采用X射线光电子能谱仪(XPS)、X射线衍射仪(XRD)、紫外-可见光漫反射仪(UV-Vis)、傅立叶变换红外光谱仪(FTIR)、扫描电子显微镜(SEM)等手段分析了催化剂和薄膜的形貌...     

锰铝层状双金属氢氧化物活化过一硫酸盐降解橙黄Ⅱ

通过水热法制备MnAl层状双金属氢氧化物(MA),采用扫描电镜(SEM)、傅里叶红外光谱仪(FTIR)、X射线衍射仪(XRD)和比表面积分析仪(BET)对其进行表征,并用其活化过一硫酸盐(PMS)降解偶氮染料橙黄Ⅱ。实验结果表明,当温度为25℃,溶液初始pH为7,0.1 g/LMA,1 mmol/LPMS,反应90分钟后20mg/L橙黄Ⅱ降解率为85.2%。橙黄Ⅱ的降解率随着PMS浓度、溶液初始pH值和温度升高而增大。MA投加量有最优值。水中常见离子Cl^-、NO₃^-、HCO₃^-、HPO₄^-、HA都对降解有一定的抑制。自由基猝灭实验结果表明体系中的主要氧化物种为¹O₂。经过5次循环使用后,橙黄Ⅱ的降解率还可达到38.2%。在实际水体应用中,橙黄Ⅱ的降解率可达53.8%。     

基于新型硼酸固相萃取柱的多巴胺色谱分析方法

用"点击化学"方法,将炔基化3-氨基苯硼酸与叠氮化硅胶反应,制备了新型硼酸固相萃取吸附剂。采用固相萃取(SPE)对样品进行前处理,反相高效液相色谱分离,紫外检测,建立了一种快速、高效、灵敏的多巴胺分析方法。固相萃取的最优条件为:对200 mg吸附剂装填的萃取柱,用甲醇活化,磷酸盐缓冲溶液(pH 8.0)平衡,再分别用1 mL水和2 mL 20%甲醇淋洗,3 mL 1 mol/L醋酸甲醇溶液洗脱。采用C18反相色谱柱,50 mmol/L磷酸二氢钠-乙腈-甲醇流动相(7∶2∶1,V/V)和检测波长280 nm的色谱条件,对洗脱液进行色谱分析。结果表明,该吸附剂对顺式邻羟基化合物有良好的识别能力。在最优萃取条件下,多巴胺的回收率达90%以上。多巴胺分析的线性范围为0.1～100 mg/L,检出限为0.0001 mg/L,相对标准偏差(RSD)<10.6%。在实际样品分析中,大鼠空白血加标液的回收率均高于97%,相对标准偏差为4.30%。     

基于多巴胺的黏合水凝胶的制备及表征

以1-(3-二甲氨基丙基)-3-乙基碳二亚胺/N-羟基琥珀酰亚胺(EDC/NHS)为催化剂, 将多巴胺通过酰胺化反应连接到氧化海藻酸钠上, 制得含邻苯二酚结构的氧化海藻酸钠(COA), 将COA与胶原(COL)复合, 制得具有黏合性能的COA-COL水凝胶, 通过紫外-可见光谱(UV-Vis)、 傅里叶变换红外光谱(FTIR)和核磁共振波谱(¹H NMR)方法表征了COA的结构, 用扫描电子显微镜、 体外膨胀降解、 万能电子拉力机和噻唑蓝(MTT)法分别表征了COA-COL水凝胶的形貌结构、 平衡溶胀率、 降解率、 黏合强度和细胞毒性. 研究结果表明, 多巴胺已引入到氧化海藻酸钠上, 取代度分别为12.5%, 18%和22%; COA-COL水凝胶的内部形成了典型的海绵体多孔网状结构, 平衡溶胀率随着多巴胺取代度的提高先减小后增大, 降解率随着取代度的提高依次减小, COA-COL水凝胶的黏合强度从未经多巴胺改性时的(20.43±4.21) kPa提高到多巴胺取代度为22%时的(29.91±6.10) kPa, 而且具有良好的生物相容性.     

介孔硅基干凝胶的降解性及其生物相容性研究

本研究利用改进的溶胶-凝胶工艺合成了介孔硅基干凝胶。通过差热-热重(DTA-TG)、X-射线衍射(XRD)、红外光谱(FTIR)和N₂等温吸附-脱附测试分析,以及扫描电镜(SEM)、透射电镜(TEM)观察,表征了硅基干凝胶的热效应、相态、结构、形貌特征,并对合成的硅基干凝胶进行了体外降解与细胞培养实验研究。测试结果表明：合成的硅基干凝胶为平均孔径3nm左右、最大比表面积901 m²·g^-1的介孔结构。体外模拟体液(Simulated body fluid,SBF)降解结果显示,低温处理的材料在42 d内完全降解,直线拟合符合一级反应动力学方程。通过添加钙磷成分或高温煅烧处理可以调控干凝胶的降解速率,使硅基干凝胶的降解呈现直线式匀速降解的特征。体外细胞培养表明：硅基干凝胶可促进C2C12细胞(C3H小鼠肌原细胞)的分化和繁殖,证明材料的生物相容性良好。     

聚丁二酸丁二酯/纳米高岭土共混体系结晶及力学性能研究

用熔融共混法制备聚丁二酸丁二酯(PBS)/纳米高岭土(nano kaolin)复合降解材料,利用FTIR、DSC、万能拉力机和SEM对其微观结构、结晶、力学性能及分散性进行研究.FTIR光谱分析结果表明,改性剂与nano kaolin发生了化学键合作用;DSC结果表明,在PBS中加入nano kaolin,提高了结晶起...     

Lys调节PLGA纳米纤维的体外降解产物酸度的研究

采用向PLGA纳米纤维中添加碱性氨基酸——赖氨酸(Lys)的方法来降低降解产物的集酸程度.用电纺丝技术制备载Lys的PLGA/Lys复合纳米纤维,并用SEM、DSC、及力学测试等表征手段对该复合纳米纤维的形貌、热学性质以及力学性质等方面进行表征;研究PLGA/Lys复合纳米纤维中Lys的释放特性;对PLGA与PLGA/Lys纳米纤维进行体外降解实验,评价纤维降解过程中的形貌和降解液pH值;用已降解8周的纳米纤维降解液对血管平滑肌细胞进行培养,MTT检测细胞毒性.结果表明,在电压为12 kV,注射速率1.0mL/h,温度23℃,湿度20%,接收距离14 cm时可以纺出形貌较好的PLGA/Lys复合纳米纤维,Lys含量越多,复合纳米纤维的直径越细.纳米纤维中Lys的含量影响Lys的释放特性.Lys促进PLGA的降解并对改善其降解产物的酸度有一定的缓解作用,含2%Lys的纳米纤维降解8周后可以使降解液pH维持在7.4~6.7之间.降解的酸性产物不利于平滑肌细胞生长,但含Lys降解液的培养基中细胞生长状态良好,这可能是由于Lys能减轻酸性降解产物对细胞功能的影响,同时也能为细胞增殖提供营养物质.     

Mg-Al-CO3水分散液的稳定性及流变性

以n(Mg):n(AI)=3的层状双金属氢氧化物（LDH）作为研究对象,考察了其水分散液的稳定性及流变性。发现其水分散液的稳定性依赖于含固量及LDH的结构完整性。LDH水分散液的流变性与其特殊的层状结构密切相关,LDH水分散液具有剪切变稀作用且是可逆的,同时还具有触变性能。利用XRD表征LDH晶体结构,SEM及TEM考察了水分散液中LDH的晶粒形态。     

Electrochemical Preparation and Characterization of Neodymium Hexacyanoferrate and Its Application

A novel route for the fabrication of neodymium hexacyanoferrate (NdHCF) modified glassy carbon electrodes (GCE) was proposed. The morphological characterization of NdHCF was examined by scanning electron microscopy (SEM) and Fourier transform infrared spectra (FTIR). The performances of the NdHCF/GCE were characterized with cyclic voltammetry and differential pulse voltammograms (DPV). The modified electrode showed excellent electrocatalytic effect and high stability toward the electrochemical oxidation of dopamine (DA) in phosphate buffer solution (pH 5.5) with a diminution of the anodic overpotential of 155 mV. The anodic peak currents increased linearly with the concentration of DA from 5.0×10^?7 to 6.0×10^?4 M with a detection limit of 1.0×10^?8 M (S/N=3). The most important is that the modified electrode could be used for the determination of DA in the presence of an ascorbic acid concentration as large as 100‐fold that of DA. The proposed method was used to determine DA in DA‐hydrochloride injection and showed excellent sensitivity and recovery. The ease of fabrication, high stability, and low cost of the modified electrode are the promising features of the proposed sensor.     

Organic/Inorganic bioactive materials Part III: in vitro bioactivity of gelatin/silicocarnotite hybrids

In this work we present our experimental results on synthesis, structure evolution and in vitro bioactivity assessment of new gelatin/silicocarnotite hybrid materials. The hybrids were obtained by diluting gelatin (G) and silicocarnotite (S) ceramic powder with G:S ratios of 75:25 and 25:75 wt.% in hot (40°C) water. The hybrids were characterized using XRD, FTIR, SEM/EDS and XPS. FTIR depicts that the “red shift” of amide I and COO⁻ could be attributed to the fact that the gelatin prefers to chelate Ca²⁺ from S. The growth of calcium phosphates on the surface of the hybrids synthesized and then immersed in 1.5 SBF for 3 days was studied by using of FTIR, XRD and SEM/EDS. According to FTIR results, after an immersion of 3 days, A and B-type CO₃HA can be observed on the surface. XRD results indicate the presence of hydroxyapatite with well defined crystallinity. SEM/EDS of the precipitated layers show the presence of CO₃HA and amorphous calcium phosphate on the surface of samples with different G/S content when immersed in 1.5 SBF. XPS of the G/S hybrid with 25:75 wt.% proved the presence of Ca-deficient hydroxyapatite after an in vitro test for 3 days.     

Exploiting micellar environment for simultaneous electrochemical determination of ascorbic acid and dopamine

A simple and reliable method for simultaneous electrochemical determination of ascorbic acid (AA) and dopamine (DA) is presented in this work. It was based on the use of the cationic surfactant cetylpyridinium chloride (CPC) that enables the separation of the oxidation peaks potential of AA and DA. Cyclic voltammetry (CV) as well as pulse differential voltammetry (PDV) were used in order to verify the voltammetric behaviour in micellar media. In the cationic surfactant CPC, a remarkable electrostatic interaction is established with negatively charged AA, as a consequence, the oxidation peak potential shifted toward less positive potential and the peak current increased. On the other hand, the positively charged DA is repelled from the electrode surface and the oxidation peak potential shifts toward more positive potential in comparison to the bare electrode. Therefore, the common overlapped oxidation peaks of AA and DA can be circumventing by using CPC. Parameter that affects the E_pa and I_pa such as CPC concentration and pH were studied. Under optimised conditions, the method presented a linear response to AA and DA in the concentration range from 5 to 75 μmol L⁻¹ and 10 to 100 μmol L⁻¹, respectively. The proposed method was successfully applied to the simultaneous determination of AA and DA in dopamine hydrochloride injection (DHI) samples spiked with AA.     

Synthesis,characterization, and in vitro degradation of liquid‐crystalline terpolyesters of 4‐hydroxyphenylacetic acid/3‐(4‐hydroxyphenyl)propionic acid with terephthalic acid and 2,6‐naphthalene diol

Melt‐processable liquid‐crystalline terpolyesters of 4‐hydroxyphenylacetic acid (HPAA) and 3‐(4‐hydroxyphenyl)propionic acid (HPPA) with terephthalic acid and 2,6‐naphthalene diol were synthesized by one‐step acidolysis melt polycondensation followed by postpolymerization and were characterized with viscosity studies, Fourier transform infrared (FTIR) and NMR spectroscopy, differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), polarized light microscopy, and wide‐angle X‐ray diffraction. The melting behaviors and liquid‐crystalline transition temperatures of the terpolyesters were dependent on the composition of the HPAA/HPPA content. The transition temperatures of the polyesters could be effectively reduced by the introduction of an even number of built‐in short methylene spacers in combination with the 2,6‐naphthalene offset structure. A terpolyester with an HPPA content of 33% (NTP33) showed optimum properties for the glass‐transition temperature, around 71 °C, and the melting temperature, near 240 °C, with a Schlieren nematic texture. The polymer showed excellent flow behavior in a Brabender plasticorder. It was also thermally stable up to 400 °C. NTP33 showed 2.5% in vitro hydrolytic degradation in buffer solutions of pH 10 at 60 °C after 540 h. Considerable enzymatic degradation was also observed with porcine pancreas lipase/buffer solutions in comparison with Candida rugosa lipase after 60 days. The degradation was also followed with FTIR, DSC, and TGA. Apart from the temperature and pH of the buffer solution, several structural parameters, such as the aromatic content, crystallinity percentage, and composition of the polymer, affected the degradation behavior. FTIR studies indicated the involvement of chain scission during degradation. Scanning electron microscopy studies further showed that surface erosion also played a major role in the degradation. © 2002 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 40: 1845–1857, 2002     

Selective enrichment of catecholamines using iron oxide nanoparticles followed by CE with UV detection

This study examines the use of unmodified magnetite nanoparticles (Fe₃O₄ NPs) for selective extraction and enrichment of the catecholamines dopamine (DA), noradrenaline (NE), and adrenaline (E), prior to analysis using capillary electrophoresis with UV detection. Coordination between Fe³⁺ on‐the‐surface Fe₃O₄ NPs and the catechol moiety of catecholamines enables Fe₃O₄ NPs to capture catecholamines from an aqueous solution. We obtained maximum loading of catecholamines on the NP surface by adjusting the pH of the solution to 7.0. In addition, catecholamine loading on the Fe₃O₄ NPs increased in conjunction with NP concentrations. H₃PO₄ was found to be efficient for the removal of adsorbed catecholamines on the NP surface. Adding 1.2% poly(diallyldimethylammonium chloride) to the background electrolyte resulted in a baseline separation of the liberated catecholamines within 20 min. Under optimal extraction and separation conditions, the limit of detections at a S/N ratio of 3 for E, NE, and DA were 9, 8, and 10 nM, respectively. Significantly, the combination of a phenylboronate‐containing spin column and the proposed method was successfully applied to the determination of NE and DA in human urine and NE in Portulaca oleracea L. leaves.     

<Emphasis Type="Italic">In vitro</Emphasis> bioactivity of 70 wt.% SiO<Subscript>2</Subscript> — 30 wt.% CaO sol-gel glass,doped with 1, 3 and 5 wt.% NbF<Subscript>5</Subscript>

The 70SiO₂-30CaO (wt.%) sol-gel glasses doped with 1, 3 and 5 NbF₅ (wt.%) were prepared via polystep sol-gel route. The synthesized glasses were characterized by XRD, FTIR and SEM. Changes in 1.5 SBF solutions were measured by ICP-AES. XRD of the glasses stabilized at 700°C for 6 hours proved the presence of niocalite. FTIR was consistent with XRD data. The in vitro bioactivity study of all glasses prepared were carried out by soaking in 1.5 simulated body fluid (1.5 SBF) at 37°C for 6 and 12 days in static conditions. The FTIR reveals the formation of A-type and B-type carbonate containing hydroxyapatite (CO₃HA) layer. Changes in 1.5 SBF solutions, after 6 days of soaking, show that the Ca concentration increased significantly, compared to the initial Ca content in the 1.5 SBF solution before in vitro test. After 12 days of immersion, the Ca concentration decreased, i.e., the formation of HA phase consumed Ca from 1.5 SBF solution. For all soaking times, the concentration of P is much lower than that the used 1.5 SBF. Based on these results we suggest that Ca and P play an active role in the future of the glasses. SEM depicts that the different morphology of hydroxyapatite can be formed as a function of soaking time.     

Synthesis and characterization of novel brush copolymers with biodegradable polyphosphoester side chains for gene delivery

A novel kind of pH‐sensitive brush copolymer [poly(2‐hydroxyethyl methacrylate)‐graft‐poly(ethylethylene phosphate)]‐block‐poly[2‐(dimethylamino)ethyl methacrylate] [(PHEMA‐g‐PEEP)‐b‐PDMAEMA] with biodegradable polyphosphoester as the side chains, and its self‐assembled aggregates were developed for nonviral gene delivery. The brush copolymers were synthesized via a combination of single‐electron transfer living radical polymerization and ring‐opening polymerization. The chemical structures of these brush copolymers were characterized by FTIR, ¹H NMR, and ³¹P NMR measurements. The critical aggregation concentration values of (PHEMA‐g‐PEEP)‐b‐PDMAEMA in pH 7.4 buffer solution were determined by the fluorescence probe technique. The interaction of (PHEMA‐g‐PEEP)‐b‐PDMAEMA and DNA was studied by agarose gel retardation assay, and the formed complexes were further investigated by means of zeta potential, dynamic light scattering, and transmission electron microscopy measurements. In addition, the in vitro cytotoxicity and transfection tests indicated that these brush copolymers showed low toxicity and favorable transfection efficiency to HeLa cells. All these results demonstrated that these biocompatible brush copolymers may be a promising candidate as nonviral polymeric gene vector. © 2013 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2013     

Comparative isoconversional thermal analysis of Artemisia vulgaris hydrogel and its acetates; a potential matrix for sustained drug delivery

Abstract

Artemisia vulgaris hydrogel (AVH) was acetylated (AAVH) and characterized by FTIR, CP/MAS ¹³C-NMR spectroscopic techniques and thermogravimetric analysis. Flynn–Waal–Ozawa model was used to investigate thermal degradation kinetics. Energy of activation (Ea) values of first and major thermal degradation steps were found to be 128.14 and 116.85 kJmol^?1 for AVH and AAVH, respectively. Thermodynamic triplet, order of degradation reaction, integral procedural decomposition temperature (IPDT) and comprehensive index of intrinsic thermal stability (ITS) were also taken into account. In vitro caffeine release from AVH-based matrix tablets indicates potential of AVH for the development of oral delivery systems for sustained drug release.     

Fabrication of Fe3O4 Nanoparticles Modified Electrode and Its Application for Voltammetric Sensing of Dopamine

Magnetic nanoparticles of Fe₃O₄ approximately 5nm in size were synthesized and characterized by XRD and TEM. A novel gold electrode modified with Fe₃O₄ nanoparticles was then constructed and was characterized by electrochemical impedance spectroscopy (EIS) and cyclic voltammetry (CV). The modified electrode exhibited strong promoting effect and high stability toward the electrochemical oxidation of dopamine (DA), which gave reversible redox peaks with a formal potential of 0.192 V (vs. Ag/AgCl) electrode in pH 7.0 phosphate buffer solution (PB). The anodic peak currents (measured by constant potential amperometry) increased linearly with the concentration of dopamine in the range of 1.5×10^?7 to 4.0×10^?4 M. The detection limit (S/N=3) obtained was 3.0×10^?8 M. The relative standard deviation (RSD) of 8 successive scans was 3.41% for 1.5×10^?6 M DA. The interference of ascorbic acid (AA) could be eliminated efficiently. The proposed method showed excellent sensitivity and recovery.     

Biodegradability of conducting chitosan-g-polycaprolactone/polypyrrole conduits

Conducting chitosan-g-polycaprolactone(CPC)/polypyrrole(PPy) conduits were fabricated for potential applications in nerve repair. Their mechanical and conducting properties as well as in vitro and in vivo degradation behaviors were mainly examined. It was found that some CPC/PPy conduits showed significantly stronger tensile and lateral compressive strength in the wet state, and notably higher conductivity in the overall tested PPy-load range, in comparison with chitosan/PPy conduits. After being consecutively exposed to PBS systems for various periods up to 10 weeks, the CPC/PPy conduits exhibited relatively slow degradation compared to chitosan/PPy conduits, and their degradation behaviors were measurably mediated by the composition of CPCs. The pH values of media corresponding to some selected CPC/PPy conduits did not significantly deviate from the initial pH value due to the buffering effect of chitosan component. After being implanted into rabbits for various periods, it was observed that the explanted chitosan/PPy conduits could only sustain a very low compressive load after 6-week degradation, and most of them were partially or fully collapsed after 8-week or longer degradation and showed very low conductivity. In contrast to these observations, some explanted CPC/PPy conduits were able to maintain enough strong mechanical strength in the wet state for the required period, and still showed acceptable conducting properties after 10-week in vivo degradation. Results suggested that some CPC/PPy conduits having proper compositional proportions could serve as desirable candidates to bridge nerve gaps in vivo.