Optical study of the formation of pyrrolo[2,3-d]pyrimidine-based fluorescent nanoaggregates

Pyrrolo[2,3-d]pyrimidine derivatives possessing different sterically-hindered end-groups at position 7 of the heterocycle were studied and compared with respect to nanoaggregate formation ability by the reprecipitation method in aqueous solutions. The emergence of nanoaggregates with an increasing water fraction in THF/water mixture was traced by observing sudden changes in spectral and transient fluorescence dynamics accompanied by fluorescence efficiency turn-on. The aggregation induced emission with a maximal 20-fold emission efficiency enhancement was obtained. Tuning of the nanoaggregates sizes from about 50 nm to 600 nm by increasing the THF/water ratio was revealed by electron microscopy. Almost perfect spherical shapes of the nanoaggregates and their structureless fluorescence bands similar to those of their neat amorphous films suggested an amorphous-like nature of the pyrrolo[2,3-d]pyrimidine-based nanoparticles.     

Kinetic Study of the Degradation of PAC-1 and Identification of a Degradation Product in Alkaline Condition

A selective and validated stability-indicating LC method was developed for the kinetic study of the degradation of PAC-1, which was carried out in aqueous solutions at 37, 60, 80 and 100 °C with pH 1.5–9.0. Separation was performed on a Kromasil C₁₈ column with acetonitrile–water–fomic acid (30:70:0.1, v/v/v) as mobile phase with a flow rate of 1.0 mL min⁻¹ at 281 nm. The degradation rate obtained indicated a first-order reaction law and the activation energy (E _a) was calculated. The results showed that temperature and pH values were significant factors affecting the degradation of PAC-1. An unknown degradation product in alkaline condition was isolated using a reverse-phase semi-preparative LC system. The structure of the degradation product is identified as 2-hydroxy-3-(2-propenyl)-[[2-hydroxy-3-(2-propenyl)phenyl]methylene]hydrazone utilizing the ¹H NMR, ¹³C NMR, IR and Q-TOF-MS techniques.

     

Improved microhardness and microtribological properties of bismaleimide nanocomposites obtained by enhancing interfacial interaction through carbon nanotube functionalization

Through the functionalization of multiwalled carbon nanotubes (MWCNTs) by 0,0′‐diallylbisphenol A (DBA), the interface situation between MWCNTs and bismaleimide (BMI) was improved, as detected by scanning electron microscope (SEM) and dynamic mechanical analysis (DMA). The improved interface situation was considered to be the main reason for the huge increased microhardness value and greatly improved the microtribological property of MWCNTs/BMI composites. Besides, the wear mechanism for the composite was also believed to be related to the interfacial situation. The rough wavelike worn surface of pure BMI resin is attributed to its poor load capacity. The smoother waterfall‐shape worn surface of MWCNTs/BMI is related to the interface formed by the addition of MWCNTs while the ultrasmooth worn surface of DBA modified MWCNTs/BMI is due to the greatly improved interfacial interaction of the composite. Copyright © 2008 John Wiley & Sons, Ltd.     

季铵型阳离子蔗渣纤维素对甘蔗清汁的澄清研究

利用新型的季铵型阳离子蔗渣纤维素作为澄清剂,对甘蔗清汁进行吸附脱色研究.本实验在单因素试验结果的基础上,分别选取纯度提高率和色值降低率作为考查指标,利用SPSS软件进行正交试验的设计和数据分析.通过最佳工艺参数的优化试验,得出如下结论:反应温度为80℃、蔗汁中阳离子蔗渣纤维素复合物的加入量为0.4g/100mL甘蔗清汁、接触时间为40min、pH值8.     

对迈克尔逊干涉仪测量波长实验中几个常见问题的分析

本文分析了迈克尔逊干涉仪测量波长实验中经常遇到的几个问题，并对其产生的原因进行了探讨。     

海螺状碳酸钙的可控合成与荧光性能

采用液相沉淀法,以硝酸铋[Bi(NO_3)_3]为添加剂来调控碳酸钙晶体的形状与大小,制备了海螺状碳酸钙粒子.通过扫描电子显微镜(SEM)、X射线衍射仪(XRD)、热重分析仪(TGA)、原子荧光光谱仪(AFS)等对产物的结构和性能进行了表征.结果表明,在60℃条件下,添加20 mL浓度为2 g/L的Bi(NO_3)_3溶液可得到海螺状球霰石型碳酸钙粒子,且其荧光性明显增强.在碳酸钙的成核过程中,Bi~(3+)的加入起到了显著的调控作用.     

EFFECT OF POLYETHYLENEIMINE ON THE PROPERTIES OF CONCENTRATED SUSPENSIONS OF TITANIUM DIOXIDE MICROBEADS

The effect of polyethyleneimine (PEI) concentration on the properties of titanium dioxide (TiO2) suspensions is studied with or without the addition of an electrolyte (barium acetate). Measurements of the apparent viscosity and the stability of TiO2 suspensions showed that PEI is an effective dispersant for TiO2 particles in suspension in the absence of an electrolyte, not only reducing the viscosity of the suspension but also increasing its stability. In the presence of an electrolyte, however, small quantities of polyethyleneimine could neither disperse the TiO2 particles nor de-crease the viscosity of the TiO2 suspensions; only PEI concentrations beyond saturation adsorption could perceptively improve the stabilitv of TiO2 suspensions.     

Determination of antibacterials in animal feed by pressurized liquid extraction followed by online purification and liquid chromatography-electrospray tandem mass spectrometry

A fully automated method has been developed for analysis of eighteen antibacterial compounds, including penicillins, cephalosporins and sulfonamides, in animal feed with limits of quantification in the range 0.25–5.79 μg kg⁻¹. The method is based on pressurized liquid extraction of 3 g homogenized feed with water and online clean-up of 500 μL of the extract with C₁₈HD cartridges. The purified sample was directly analysed by liquid chromatography–electrospray tandem mass spectrometry (SPE–LC–ESI-MS–MS). Chromatographic separation was achieved within 10 min by use of a C₁₂ Phenomenex Hydro-RP reversed-phase analytical column and a mobile phase gradient (water + 0.1% formic acid–methanol + 0.1% formic acid). The method was validated, revealing capability for detection of concentrations as low as 0.09 μg kg⁻¹, decision limits (CCα) and detection capabilities (CCβ) in the range 10–174 μg kg⁻¹ and 22–182 μg kg⁻¹, respectively, and inter-day precision ranging from 0.7 to 8.3%. Recovery, with internal standard correction, was in the range 93–134% for all analytes. The method was then applied to analysis of fifteen feed samples, nine of which contained at least one antimicrobial at concentrations between 0.006 and 1.526 mg kg⁻¹. The performance data and results from the method were compared with those from a previous method developed by our group, using offline SPE, by analyzing the same set of samples by both methods. The online SPE approach resulted in slightly improved sensitivity, with LODs of 0.09–2.12 μg kg⁻¹ compared with 0.12–3.94 μg kg⁻¹ by the offline approach. In general, better recovery was achieved by use of online purification (for 72% of the analytes) and the correlation between the two methods was good. The main advantages of the new online method are rapid and automated sample pre-treatment, and reduction of sample manipulation, enabling high-throughput analysis and highly accurate results. Because of all these characteristics, the proposed method is applicable and could be deemed necessary within the field of food control and safety.