泡塑富集-硫脲解脱电感耦合等离子体质谱法快速测定化探样品中痕量金的条件优化

针对化探样品中痕金的电感耦合等离子体质谱法快速测试方法,探讨了吸附酸度、解脱时间、吸附温度等对测试结果的影响。确立了电感耦合等离子体质谱法测定的最佳条件。方法检出限为:0.035 ng/g,准确度△lgC(n=12)为0.01～0.05,精密度RSD（n=12）为4.50～9.64。很好的解决金的快速测定问题,对地矿部门日益增多的化探任务,提高了测试速度,缩短了测试周期,值得推广。     

微型集成化色谱仪

用微制造技术和色谱原理结合，以全新的概念和设计思维研制色谱仪一微型集成化色谱仪。这种仪器的整个色谱部分在基片上制成。集微型进样器，细内径毛细管柱和微型固体检测器于一体，功耗不过几瓦，重不过几百克，而分析速度比现有仪器提高近一个数量级，检测灵敏度可达１０＾－６Ｖ／Ｖ。这种仪器的制作过程类似半导体器件，能大批量，性能高度重复可靠、而成本极为低廉地制造出来，彻底改变传统色谱仪器的生产方式。本文给出这种仪     

α—氨基酸的快原子轰击质谱

本文研究了１８种α－氨基酸的快原子轰击质谱，发现添加三氟乙酸溶液能显著提高灵敏度，改善谱图。特征碎片主要有中性丢失ＣＯ２Ｈ２，Ｈ２Ｏ，ＮＨ３的离子以及Ｒ＾＋离子。侧链的性质决定了碎片的产生和离子的强弱。     

Fast Capillary Gas Chromatography: Comparison of Different Approaches

Savings in analysis time in capillary GC have always been an important issue for chromatographers since the introduction of capillary columns by Golay in 1958. In laboratories where gas chromatographic techniques are routinely applied as an analytical technique, every reduction of analysis time, without significant loss of resolution, can be translated into a higher sample throughput and hence reduce the laboratory operating costs. In this contribution, three different approaches for obtaining fast GC separations are investigated. First, a narrow-bore column is used under conventional GC operating conditions. Secondly, the same narrow-bore column is used under typical fast GC conditions. Here, a high oven temperature programming rate is used. The third approach uses a recent new development in GC instrumentation: Flash-2D-GC. Here the column is placed inside a metal tube, which is resistively heated. With this system, a temperature programming rate of 100°/s is possible. The results obtained with each of these three approaches are compared with results obtained on a column with conventional dimensions. This comparison takes retention times as well as plate numbers and resolution into consideration.     

QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留

采用QuEChERS方法结合在线凝胶色谱-气相色谱-质谱（GPC-GC-MS）系统,建立了大米、黍子和小麦中34种中高毒农药的快速筛查方法。研究了称样量、萃取剂、净化吸附剂种类对大米样品提取净化效果的影响并考察了基质效应和分析保护剂的使用效果,采用选择离子监测（SIM）模式,外标法定量。结果表明,34种农药在大米、黍子和小麦中的检出限分别为0.0281~5.30、0.0282~4.82、0.0273~5.13 μg/kg;在0.05 μg/g添加水平的平均回收率分别为94.5%~117.1%、83.1%~121.7%、93.1%~120.2%;相对标准偏差（RSD,n=6）分别为2.6%~14.5%、3.4%~15.1%、3.5%~15.2%。该方法消耗试剂少,分析成本低,符合绿色化学的理念,具有操作便捷、快速、通用性强等特点,适用于大米、黍子和小麦中34种农药残留的快速筛查与检测。     

High-Field Detection of Biomarkers with Fast Field-Cycling MRI: The Example of Zinc Sensing

Many smart magnetic resonance imaging (MRI) probes provide response to a biomarker based on modulation of their rotational correlation time. The magnitude of such MRI signal changes is highly dependent on the magnetic field and the response decreases dramatically at high fields (>2 T). To overcome the loss of efficiency of responsive probes at high field, with fast-field cycling magnetic resonance imaging (FFC-MRI) we exploit field-dependent information rather than the absolute difference in the relaxation rate measured in the absence and in the presence of the biomarker at a given imaging field. We report here the application of fast field-cycling techniques combined with the use of a molecular probe for the detection of Zn²⁺ to achieve 166 % MRI signal enhancement at 3 T, whereas the same agent provides no detectable response using conventional MRI. This approach can be generalized to any biomarker provided the detection is based on variation of the rotational motion of the probe.     

High‐energy collision‐induced dissociation of [M+Na]+ ions desorbed by fast atom bombardment of ceramides isolated from the starfish Distolasterias nipon

Ten ceramides and four cerebrosides were extracted from the starfish Distolasterias nipon by solvent extraction, silica gel column chromatography and reversed‐phase high‐performance liquid chromatography. Structural identification was conducted using tandem mass spectrometry of monosodiated ions desorbed by fast atom bombardment. The complete structures of four cerebrosides were determined by a previously reported method. The high‐energy collision‐induced dissociation (CID) spectral characteristics of ceramides with various structures depend on the number and positions of double bonds on both the N‐acyl and sphingoid chains, the presence of a hydroxyl group or a double bond at the C‐4 position of the sphingoid chain and the presence of an α‐hydroxy group on the N‐acyl chain. The high‐energy CID of the monosodiated ion, [M+Na]⁺, of each ceramide molecular species generated abundant ions, providing information on the composition of the fatty acyl chains and sphingoid long‐chain bases. Each homologous ion series along the fatty acyl group and aliphatic chain of the sphingoid base was used for locating the double‐bond positions of both chains and hydroxyl groups on the sphingoid base chain. The double‐bond positions were also confirmed by the m/z values of abundant allylic even‐ and odd‐electron ions, and the intensity ratio of the T ion peak relative to the O ion peak. This technique could determine the complete structures of ceramides and cerebrosides in an extract mixture and has great potential for determining other sphingolipids isolated from various biological sources. Copyright © 2013 John Wiley & Sons, Ltd.     

A tin-containing liquid crystalline polymer with two glass temperatures

A tin-containing liquid crystalline side group polymer was synthesized and characterized. Two glass transitions were detected by calorimetric investigations. The X-ray pattern corresponds to a smectic C order of the side groups and a disordered isotropic main chain. Dielectric measurements show two relaxation ranges which are influenced by the glass transitions and a fast local process. The low frequency mechanism can be related to the reorientation of the side groups and the higher glass transition temperature. The second is connected with the α-relaxation of the main chain and freezes in at lower temperatures.     

Fast switching of vertically aligned negative liquid crystals by optically hidden relaxation

We propose a method for fast switching of vertically aligned (VA) negative liquid crystals (LCs) by hiding the relaxation process of LCs. During the turn-off process, a strong in-plane electric field is applied for a short duration of time instead of relying solely on the slow relaxation of LCs. The LC molecules are rotated to the transmission axis of one of the polarisers by the applied in-plane electric field, resulting in turn-off switching that is 5.8 times faster than that of a conventional VA cell. By applying an overdriving scheme, we experimentally obtained a total response time of 3.3 ms.     

Fast polarisation-insensitive optical shutter supported by backflow in dichroic dye-doped dual-frequency liquid crystal

This paper describes a novel implementation of a dual-frequency liquid crystal optical shutter of the guest–host type. The transmissive state of the filter is obtained by applying a low-frequency electric field that brings the dichroic dye in a homeotropic orientation. The light-absorbing state is realised by a twisted planar configuration for which the absorption is quasi-independent of the polarisation. Switching between the two states occurs in about 1 ms and the devices show no scattering for wavelengths inside or outside the absorption band of the dichroic dye. Simulations and experiments reveal how a twisted state is obtained through the backflow phenomenon.