Rapid determination of volatile constituents of Michelia alba flowers by gas chromatography-mass spectrometry with solid-phase microextraction

The volatile constituents of Michelia alba flowers, including fresh flowers, frozen flowers and withered flowers, were investigated by GC-MS. The volatiles in a simulated natural environment were sampled by solid-phase microextraction (SPME), with a 100 microm polydimethylsiloxane fiber at 25+/-5 degrees C for 4 h. The fibers were desorbed in a GC injection liner at 250 degrees C for 3 min. With headspace SPME-GC-MS analysis, 61 peaks were separated. The main compounds in headspace of fresh Michelia alba flowers included alpha-myrcene, (S)-limonene, (R)-fenchone, linalool, camphor, caryophyllene, germacrene D, etc., a greater number of compounds than for frozen flowers and withered flowers. At the same time, the biomarkers of fresh flowers were compared with the frozen flowers and withered flowers. In this study, headspace SPME-GC-MS afforded a simple and more sensitive sampling method for fresh Michelia alba flowers and other fresh flowers.     

Stochastic resonance is applied to quantitative analysis for weak chromatographic signal of glyburide in plasma

Based on the theory of stochastic resonance, a new method carried on the quantitive analysis to weak chromatographic signal of glyburide in plasma, which was embedded in the noise background and the signal-to-noise ratio (SNR) of HPLC-UV is enhanced remarkably. This method enhances the quantification limit to 1 ng ml⁻¹, which is the same as HPLC-MS, and makes it possible to detect the weak signal accurately by HPLC-UV, which was not suitable before. The results showed good recovery and linear range from 1 to 50 ng ml⁻¹ of glyburide in plasma and the method can be used for quantitative analysis of glyburide.     

基于三维静电势参数研究C60溶解性的构效关系

在量子化学从头算基础上,对一系列溶剂化合物分子进行了结构优化和三维静电势参数计算,运用多元线性回归分析和神经网络方法对C60在121种不同溶剂的溶解性与计算的结构参数进行了构效关系研究.用建立起来的QSPR 关系式对15种不同结构类型溶剂进行了预测,并阐述了C60溶质与不同溶剂之间的相互作用,获得了满意的结果.     

Effect of the sixth axial ligand in CS-ligated iron(II)octaethylporphyrinates: structural and Mössbauer studies

The effect of a sixth ligand in a series of low-spin thiocarbonyl-ligated iron(II)octaethylporphyrinates has been investigated. Six-coordinate complexes have been synthesized and characterized by M?ssbauer and infrared spectroscopy and single-crystal X-ray structure determinations. The results are compared with the five-coordinate parent complex. The crystal structures of [Fe(OEP)(CS)(1-MeIm)] and [Fe(OEP)(CS)(Py)] are reported and discussed. The 1-methylimidazole and pyridine derivatives exhibit Fe-C(CS) bond distances of 1.703(4) and 1.706(2) A that are significantly longer than the 1.662(3) A reported for five-coordinate [Fe(OEP)(CS)] (Scheidt, W. R.; Geiger, D. K. Inorg. Chem. 1982, 21, 1208). The trans Fe-N(ligand) distances of 2.112(3) and 2.1550(15) A observed for the 1-methylimidazole and pyridine complex are approximately 0.13 A longer than those observed for analogous bis-ligated complexes and are consistent with a significant structural trans effect for the CS ligand. M?ssbauer investigations carried out for five- and six-coordinate thiocarbonyl derivatives with several different sixth axial ligands reveal interesting features. All derivatives exhibit very small isomer shift values, consistent with a very strong interaction between iron and CS. The five-coordinate derivative has delta(Fe) = 0.08 mm/s, and the six-coordinate complexes exhibit delta(Fe) = 0.14 to 0.19 mm/s at 4.2 K. The five-coordinate complex shows a large quadrupole splitting (DeltaE(q) = 1.93 mm/s at 4.2 K) which is reduced on coordination of the sixth ligand (DeltaE(q) = 0.42-0.80 mm/s at 4.2 K). Addition of a sixth ligand also leads to a small decrease in the value of nu(CS). Correlations in structural, IR, and M?ssbauer results suggest that the sixth ligand effect is primarily induced by changes in sigma-bonding. The structure of [Fe(OEP)(CS)(CH(3)OH)] is briefly reported. Crystal data: [Fe(OEP)(CS)(1-MeIm)] crystallizes in the monoclinic system, space group P2(1)/n, Z = 4, a = 9.5906(5) A, b = 16.704(4) A, c = 23.1417(6) A, beta = 100.453(7) degrees. [Fe(OEP)(CS)(Py)] crystallizes in the triclinic system, space group P1, Z = 5, a = 13.9073(6) A, b = 16.2624(7) A, c = 22.0709(9) A, alpha = 70.586(1) degrees, beta = 77.242(1) degrees, gamma = 77.959(1) degrees. [Fe(OEP)(CS)(CH(3)OH)] crystallizes in the triclinic system, space group P1, Z = 1, a = 9.0599(5) A, b = 9.4389(5) A, c = 11.0676(6) A, alpha = 90.261(1) degrees, beta = 100.362(1) degrees, gamma = 114.664(1) degrees.     

A novel neutral receptor for selective recognition of H2PO 4 −

A new urea-based receptor was designed to selectively recognize H₂PO₄⁻ among other anions (such as F^-, Cl^-, Br^-, I^-, OH^-, AcO^-) in organic solvent (DMSO) through intermolecular hydrogen bonding. Addition of anions to the receptor caused changes in UV–vis spectrum which provided the first indication of its anion binding ability. Electronic supplementary material The online version of this article (doi:) contains supplementary material, which is available to authorized users.     

Shift-full-rank matrices and applications in space-time trellis codes for relay networks with asynchronous cooperative diversity

To achieve full cooperative diversity in a relay network, most of the existing space-time coding schemes require the synchronization between terminals. A family of space-time trellis codes that achieve full cooperative diversity order without the assumption of synchronization has been recently proposed. The family is based on the stack construction by Hammons and El Gamal and its generalizations by Lu and Kumar. It has been shown that the construction of such a family is equivalent to the construction of binary matrices that have full row rank no matter how their rows are shifted, where a row corresponds to a terminal (or transmit antenna) and its length corresponds to the memory size of the trellis code on that terminal. We call such matrices as shift-full-rank (SFR) matrices. A family of SFR matrices has been also constructed, but the memory sizes of the corresponding space-time trellis codes (the number of columns of SFR matrices) grow exponentially in terms of the number of terminals (the number of rows of SFR matrices), which may cause a high decoding complexity when the number of terminals is not small. In this paper, we systematically study and construct SFR matrices of any sizes for any number of terminals. Furthermore, we construct shortest (square) SFR (SSFR) matrices that correspond to space-time trellis codes with the smallest memory sizes and asynchronous full cooperative diversity. We also present some simulation results to illustrate the performances of the space-time trellis codes associated with SFR matrices in asynchronous cooperative communications.     

The Pharmacokinetics in Mice and Cell Uptake of Thymus Immunosuppressive Pentapeptide Using LC-MS/MS Analysis

Thymus immunosuppressive pentapeptide (TIPP) is a novel anti-inflammatory peptide with high efficacy and low toxicity. This study aims to establish a selective LC-MS/MS method for analyzing the analyte TIPP in biological samples, laying the foundation for further PK and PD studies of TIPP. Protein precipitation was conducted in acetonitrile supplemented with 2% formic acid and 25 mg/mL dithiothreitol as a stabilizer, which was followed by backwashing the organic phase using dichloromethane. The chromatographic separation of TIPP was achieved on a C18 column with a gradient elution method. During positive electrospray ionization, TIPP was analyzed via multiple-reaction monitoring. The linear relationships between the concentration of TIPP and peak area in murine plasma cell lysates, supernatants, and the final cell rinse PBS were established within the ranges of 20–5000 ng/mL, 1–200 ng/mL, 10–200 μg/mL, and 0.1–20 ng/mL, respectively (r² > 0.99). Validated according to U.S. FDA guidelines, the proposed method was proved to be acceptable. Such a method had been successfully applied to investigate the pharmacokinetics of TIPP in mice via subcutaneous injection. The plasma half-life in mice was 5.987 ± 1.824 min, suggesting that TIPP is swiftly eliminated in vivo. The amount of TIPP uptake by RBL-2H3 cells was determined using this method, which was also visually verified by confocal. Furthermore, the effective intracellular concentration of TIPP was deduced by comparing the intracellular concentration of TIPP and degrees of inflammation, enlightening further investigation on the intracellular target and mechanism of TIPP.     

分析宽频带、双极化、恒束宽四脊喇叭的混合方法

介绍了作为反射面天线馈源的宽频带、双极化、恒波束四脊喇叭，运用有限元和模式匹配相结合的混合法详细且计算了四脊喇叭的广义散射矩阵。然后运用口面积分计算了四脊喇叭的辐射远场，给出了四脊喇叭和用四脊喇叭做馈源的反射面天线的实测结果。     

红外焦平面阵列非均匀性自适应校正算法研究

在分析红外焦平面阵列非均匀性校正现行算法的基础上,提出了一种具有自适应性能的新算法。该算法以小波变换中的滤波器理论为基础,通过将图像序列在时间域的尺度分解和相庆统计量计算,获得在红外焦平面校正中起影响的偏置和增益系数。模拟实验结果验证了其有效性和先进性。     

光纤传感器对混凝土结构钢筋腐蚀监测的研究

本文报道了光纤传感器用于混凝土结构钢筋腐蚀监测的实验研究结果。该传感方案基于用Fe-C合金膜局部取代光纤介质包层,构成腐蚀敏感膜,从而获取金属腐蚀信息。为了监测钢筋在实际混凝土结构中的腐蚀行为。本文提出了可以埋入到结构中的光纤腐蚀传感器（FOCS）,并对埋入工艺进行研究,通过人造裂缝将防冰盐（NaCl）溶液加入到混凝土结构钢筋处并进行加速腐蚀,用紧贴钢筋铺设的FOCS监测钢筋腐蚀过程中输出光功率的变化,结果表明FOCS输出光功率变化和腐蚀介质的pH值变化有良好的对应关系,并与腐蚀电化学理论描述相一致,证实了所提传感器方案的可行性。