Novel sponge-like molecularly imprinted mesoporous silica material for selective isolation of bisphenol A and its analogues from sediment extracts

Bisphenol A (BPA) imprinted sponge mesoporous silica was synthesized using a combination of semi-covalent molecular imprinting and simple self-assembly process. The molecularly imprinted sponge mesoporous silica (MISMS) material obtained was characterized by FT-IR, scanning electron microscopy, transmission electron microscopy, and nitrogen adsorption–desorption measurements. The results show that the MISMS possessed a large specific surface area (850.55 m² g⁻¹) and a highly interconnected 3-D porous network. As a result, the MISMS demonstrated a superior specific adsorption capacity of 169.22 μmol g⁻¹ and fast adsorption kinetics (reaching equilibrium within 3 min) for BPA. Good class selectivity for BPA and its analogues (bisphenol F, bisphenol B, bisphenol E and bisphenol AF) was also demonstrated by the sorption experiment. The MISMS as solid-phase extraction (SPE) material was then evaluated for isolation and clean-up of these bisphenols (BPs) from sediment samples. An accurate and sensitive analytical method based on the MISMS–SPE coupled with HPLC–DAD has been successfully established for simultaneous determination of five BPs in river sediments with detection limits of 0.43–0.71 ng g⁻¹ dry weight (dw). The recoveries of BPs for lyophilizated sediment samples at two spiking levels (50 and 500 ng g⁻¹ dw for each BP) were in the range of 75.5–105.5% with RSD values below 7.5%.     

Lasing of a DCM dye layer in carbazole-based films

We have studied the spectral and lasing properties of 4-dicyanomethylene-2-methyl-6-(p-dimethylaminostyryl)-4H-pyran (DCM) in polyepoxypropylcarbazole (PEPK), polybutylcarbazole (PBK), and polyvinylcarbazole (PVK) films when excited by emission from a XeCl laser (λ = 308 nm) and the second harmonic of a YAGNd laser (λ = 532 nm). Stimulated emission was excited without an external cavity in the traveling wave mode in films of thickness 0.5–0.8 μm, obtained by the centrifuging method. __________ Translated from Zhurnal Prikladnoi Spektroskopii, Vol. 73, No. 2, pp. 177–181, March–April, 2006.     

脉冲序列控制电流断续模式Buck变换器的动力学建模与边界碰撞分岔

通过建立一个开关周期内输出电容电荷变化量对应的输出电压变化量, 建立了工作于电感电流断续模式(discontinuous conduction mode, DCM)的脉冲序列(pulse train, PT)控制Buck变换器的近似离散时间模型, 研究了负载电阻及输入电压变化时PT控制DCM Buck变换器的边界碰撞分岔行为. 通过构造相应的迭代映射曲线, 分别分析了不同负载电阻时PT控制DCM Buck变换器的周期1、周期2和周期3运行轨迹的不动点稳定性, 揭示了PT控制DCM Buck变换器在不同周期态时的边界碰撞分岔的形成机理. 研究结果表明, 随参数变化, PT控制DCM Buck变换器始终运行在不同的周期态, 各周期态的切换由边界碰撞分岔引起, 李雅谱诺夫指数始终小于零. 利用PSIM电路仿真软件, 给出了不同负载电阻时的时域波形和相轨图. 实验结果验证了理论分析和仿真结果的正确性, 同时说明了本文动力学建模的可行性.     

Analysis of questioned documents: A review

During the last years (2000–2014), many publications concerning the forensic analysis of questioned documents have been published, and new techniques and methodologies are nowadays employed to overcome forensic caseworks. This article reviews a comprehensive collection of the works focused on this issue, including dating studies, the analysis of inks from pens and printers, the analysis of paper, the analysis of other samples related to questioned documents and studies on intersecting lines. These sections highlight the most relevant analytical studies by a wide range of analytical techniques. Separation and spectrometric techniques are critically discussed and compared, emphasizing the advantages and disadvantages of each one. Finally, concluding remarks on the research published are included.     

Monitoring of progestins: Development of immunochemical methods for purification and detection of levonorgestrel

A polyclonal antibody (Ab) for the progestin levonorgestrel (LNG) was generated, and immunochemical assays for its detection, clean-up and concentration were developed. A highly specific microplate diagnostic assay for the detection of LNG was developed that used the enzyme linked immunosorbent assay (ELISA) method. The LNG ELISA developed was sensitive and reproducible; it exhibited I₅₀ and I₂₀ values of 3.3 ± 1.8 ng mL⁻¹ and 0.6 ± 0.4 ng mL⁻¹, respectively, and the Abs did not cross react with any of the tested steroid hormones. The above Abs were used to develop a sol-gel-based immunoaffinity purification (IAP) method for concentration and clean-up of LNG that is compatible with subsequent immunochemical or instrumental chemical analytical procedures, such as liquid chromatography followed by mass spectrometry (LC-MS/MS). Development of the columns included successful entrapment of Abs within a tetramethoxysilane (TMOS)-based SiO₂ polymer network. The Abs could bind the free analyte from solution, and the bound analyte could be easily eluted from the sol-gel matrix at high recoveries. The Ab selectivity towards the antigen was high, in both ELISA and the sol-gel columns, but the entrapped Abs cross-reacted with two other steroid hormones - ethynylestradiol (EE2) and nortestosterone (NT) - which share similar epitopes with LNG, despite the lack of cross reactivity in the ELISA. The validity of the method was investigated by LC-MS/MS and a good analytical correlation was obtained.     

An overview of sample preparation and extraction of synthetic pyrethroids from water,sediment and soil

The latest developments in sample preparation and extraction of synthetic pyrethroids from environmental matrices viz., water, sediment and soil were reviewed. Though the synthetic pyrethroids were launched in 1970s, to the best of authors’ knowledge there was no review on this subject until date. The present status and recent advances made during the last 10 years in sample preparation including conservation and extraction techniques used in determination of synthetic pyrethroids in water, sediment and soil were discussed. Pre- and post-extraction treatments, sample stability during extraction and its influence upon the whole process of analytical determination were covered. Relative merits and demerits including the green aspects of extraction were evaluated. The current trends and future prospects were also addressed.     

Pure red emission of dye-doped organic molecules from microcavity organic light emitting diode

Organic red emitting diode was fabricated by using 4-dicyanomethylene-2-methyl-6-[2-(2,3,6,7-tetrahydro-1 H,5H-benzo[ij]quinolizin-8-yl)vinyl]-4H-pyran (DCM)-doped tri-(8-quinolitolato) aluminum (Alq₃) as emitter with the structure of G/ITO/NPB(25 nm)/DCM:Alq₃(55 nm)/Alq₃(20 nm)/LiF (1.2 nm)/Al(84 nm), (glass/indium–tin-oxide/4,4-bis-[N-(1-naphthyl)-N-phenyl-amino]biphenyl, G/ITO/NPB), the wavelength of the maximal emission of which is 615 nm. By introducing cavity to Organic light emitting diode (OLED), we got pure red emitting diode with wavelength of the maximal emission of 621 nm and full-width at half-maximum (FWHM) of 27 nm. As far as we know, it is the best result in the dye-doped organic red emitting diode. We also made a device of G/ITO/NPB(25 nm)/DCM:Alq₃(29 nm)/DCM:PBD(26 nm)/Alq₃(20 nm)/LiF(1.2 nm)/Al(84 nm), in order to compare the performance of Alq₃ with that of 2-(4-biphenylyl)-5-(4-t-butylphenyl)-1,3,4-oxadiazole (PBD) as host material. It was found that the performance of device A is better than that of C both in brightness and color purity,as well as in EL efficiency.     

N-alkylpyridinium quaternization combined with liquid chromatography–electrospray ionization-tandem mass spectrometry: A highly sensitive method to quantify fatty alcohols in thyroid tissues

A highly sensitive method was developed for the identification and quantification of fatty alcohols in biological tissues. In the presence of pyridine-d₀ and triflic anhydride (Tf₂O), fatty alcohols were converted into permanently charged N-alkylpyridinium ions. Stable isotope-labeled derivatives were generated by pyridine-d₅ and added as internal standard (IS). The mixture was analyzed by liquid chromatography coupled to positive electrospray ionization tandem mass spectrometry (LC–ESI-MS/MS). This method was optimized and validated in terms of reaction time, derivatization efficiency, stability, desalting, and ion suppression effect. Besides, fatty alcohols exhibited good linear relationship (r² > 0.993) over the concentration range of 10 ng mL⁻¹–1 μg mL⁻¹. The limits of detection (LODs) were lowered from previously reported 0.1 ng mL⁻¹ to 0.25 pg mL⁻¹. Precision (RSD% < 15.6%), accuracy (93.0–107.2%), matrix effect, and recovery (in thyroid tissues) were validated as well. Finally, this method was applied for the analysis of ten even carbon-numbered fatty alcohols (C₈–C₂₄) in human thyroid carcinoma and para-carcinoma tissues, revealing a significant decrease of fatty alcohols (free and esterified) in thyroid carcinoma tissues (p < 0.05).