Use of a liquid chromatograph-ion trap mass spectrometer for end-group characterization of various polyethoxylate materials

The separation and detection properties of various ethoxylated polymers were investigated with atmospheric pressure ionization liquid chromatography/mass spectrometry (LC/MS). Interesting chromatographic elution behavior based on functionality was noted. LC/MS using in-source CID (collision-induced dissociation) and tandem mass spectrometry (MS/MS) detection was compared for end-group identification. Excellent end-group identification was achieved when the end-group molecular weight (MW) was greater than 100 Da and the average MW of the polymer was less than 400 Da by both MS/MS and in-source CID. In cases where the end-group MW was less than 100 Da, because of the low mass cut-off in a quadrapole ion trap analyzer, in-source CID produced the only characteristic end-group ions. The use of a dual scan function allowed investigation of the oligomeric distribution followed by a narrow low-mass scan using in-source CID to generate end-group information. This approach is applicable on instruments without MS/MS capability.     

Ti600合金的高温氧化行为研究

研究了Ti600合金在600~750℃下的高温氧化行为。采用连续氧化增重的方法及氧化速度常数、氧化活度等理论计算了合金氧化的热力学和动力学规律;用XRD、SEM、EDS等手段研究保护膜的表面相结构和表面形貌以及截面元素分布。结果表明:Ti600合金在700℃以下均有较好的抗氧化性能,其连续氧化动力学曲线基本符合抛物线规律;在750℃,氧化较严重,其连续氧化动力学曲线近似符合抛物线-直线规律。氧化层由金红石型的TiO2氧化物和少量的Al2O3组成。Al2O3能阻止氧的渗入,降低氧化速度。     

Miscibility of polymethylmethacrylate and polyethyleneglycol blends in tetrahydrofuran

The miscibility of polymethylmethacrylate (PMMA) and polyethyleneglycol (PEG) blends in tetrahydrofuran (THF) has been investigated by viscosity, density, refractive index, and ultrasonic velocity studies. Various interaction parameters such as polymer–solvent and blend–solvent interaction parameters and heat of mixing have been calculated using the viscosity, density, and ultrasonic velocity data. The results indicated the existence of positive interactions in the blend polymer solutions and that they are miscible in THF in the entire composition range. The study also revealed that variation in the temperature does not affect the miscibility of PMMA and PEG blends in THF significantly. The presence of hydrogen bonding in the blends in the solid state has also been indicated by FTIR studies. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Encapsulation of diclofenac sodium with acidic copolymer hydrogels based on PEG/poly(N‐isopropylacrylamide‐co‐2‐acrylamido‐2‐methyl‐1‐propanesulfonic acid) semi‐interpenetrating network using in situ loading technique

A pH‐ and temperature‐responsive semi‐interpenetrating copolymer PEG6000/poly(NIPA‐co‐AMPS) (PEG/AMPS‐co‐NIPA SIPN), for short PEG SIPN, was made by ammonium persulfate‐initiated suspension copolymerization of N‐isopropylacrylamide, 2‐acrylamido‐2‐methylpropanesulphonic acid, and N,N′‐methylene‐bis‐acrylamide (MBAA; crosslinker) in the presence of PEG6000. The PEG SIPN copolymer matrices containing nanostructures made in the high‐temperature copolymerization resulted in channels for PEG and facile migration of drugs. In drug encapsulation or drug‐loading process, one can easily ignore or pay less attention to the interaction between a drug and its encapsulation materials; however, the ignored interactions may induce problems in drug properties or the release behavior in use. Sodium diclofenac (DFNa) precipitates as the carboxylic acid form in an acidic environment, and it is challenging to encapsulate sodium diclofenac in such an acidic matrix without precipitation of the sparingly soluble acid form of DFNa on the surface of the polymer substrate. To avoid bulky precipitation in drug loading, an in situ loading technique was developed for producing gel spheres with DFNa uniformly distributed in the polymer matrix. The technique is based on fast polymerization of spherical droplets of a pregel solution in which the drug is dissolved. Diffusion‐loading prodrugs were made in comparison with in situ loading prodrugs in thermal, release kinetics, and release behavior. Drug release profiles (in pH 7.4 phosphate buffer) show that the new drug loading technique gives controlled release during a period of about 7 days at 37°C. By contrast, gel spheres loaded with sodium diclofenac using the conventional diffusion technique produced almost total release of the drug within about 24 h. The thermal stability of sodium diclofenac, the PEG/AMPS‐co‐NIPA SIPN, and the prodrugs made with the SIPN and sodium diclofenac was studied. A near zero‐order release kinetics was found in the in vitro release of sodium diclofenac with in situ loading PEG SIPN prodrug. We have, for the first time, studied sodium diclofenac release behavior from the PEG SIPN hydrogel systems. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

集成干扰素突变体的构建、表达及纯化

目的构建高效且可供单甲氧基聚乙二醇马来酰亚胺(mPEG-MAL)定点修饰的集成干扰素突变体(IIFNm108),并进行表达、纯化及鉴定。方法采用同源序列对比、空间结构模拟并结合α干扰素与受体结合的特点设计突变位点。用重叠延伸PCR法,扩增IIFNm108基因,与pET-23b载体连接,构建重组表达质粒pET-23b-IIFNm108,转化E.coli BL21(DE3),IPTG诱导表达,所得包涵体经变性、复性、DEAE阴离子交换及凝胶过滤两步层析纯化后,进行各项鉴定。结果重组表达质粒经双酶切及测序鉴定证明构建正确。目的蛋白的表达量占菌体总蛋白的30%以上,主要以包涵体形式存在。纯化的IIFNm108蛋白纯度大于95%,比活性约为(2.08±0.17)×108IU/mg,N-端、C-端氨基酸序列与理论一致,相对分子质量为19500,可与mPEG-MAL成功交联。结论已获得一种高效且可供mPEG-MAL定点修饰的集成干扰素突变体IIFNm108。     

傅立叶变换红外光谱法研究马来酸酐与聚乙二醇酯化反应

利用傅立叶变换红外光谱法跟踪监测马来酸酐与聚乙二醇的酯化反应,根据酯化产物在不同反应时间上的特征红外吸收峰面积的变化半定量的作出酯化反应动力学曲线,并考察了催化剂、反应温度等对酯化反应动力学曲线的影响,找出获得单酯产物的最佳反应条件。     

Preparation and conductivity of substituted germanic heteropoly acids polyethylene glycol hybrid materials

In this work, the polyethylene glycol (PEG) hybrid materials composited with substituted germanic heteropoly acids were prepared. Infrared (IR) spectra revealed that the Keggin structure characteristic of the GeM₁₁VO₄₀^5? anion were present in the hybrid materials. At room temperature (20°C), the conductivity of the products is 4.07 × 10^?3 S cm^?1 and 2.12 × 10^?3 S cm^?1, respectively. The results indicated that the conductivity of substituted germanic heteropoly acids PEG hybrid materials is higher than that of the corresponding pure substituted germanic heteropoly acids. According to the experimental results, we proposed a possible mechanism of the proton conduction of the hybrid materials. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

聚乙二醇-600对酸性Zn-Ni合金的电沉积行为及镀层耐蚀性影响的研究

采用循环伏安(CV)曲线研究了聚乙二醇-600 (PEG-600)在酸性Zn-Ni合金基础镀液中对Zn-Ni合金电沉积行为的影响;采用电化学阻抗谱(EIS)、动电位极化曲线与表面形貌分析方法研究了酸性Zn-Ni合金基础镀液中,聚乙二醇-600的浓度对Zn-Ni合金镀层表面微观形貌及耐蚀性的影响.结果 表明,PEG-60...     

增韧酚醛泡沫塑料的制备及填料对其性能的影响

以甲阶段酚醛树脂（PF）为基体,聚乙二醇（PEG）和玻璃纤维（GF）为增韧剂,通过抗冲击测试、SEM分析及红外光谱分析（IR spectra）,研究了PEG和GF对改性酚醛泡沫塑料性能的影响。通过综合性能比较得出GF与PEG复合增韧效果最好。结果表明：采用100份酚醛树脂、12份聚乙二醇、0.5份玻璃纤维,温度为80℃,反应时间为30 min,可制备出增韧酚醛泡沫塑料,冲击强度为5.54 kJ/m^2,泡孔细小均匀,粉化率降低7.43%。