Applications of coupled LC-GC: A review

Although coupled liquid chromatographygas chromatography (LC-GC) was first demonstrated ten years ago, only in the last few years has there been a sudden surge of interest in the technique. Approximately 70% of the total number of LC-GC applications have been published in the last two years (1987–88) alone. This review categorizes LC-GC publications into four main application areas: fossil fuels, foods, environmental samples, biologiical/pharmaceutical samples, and miscellaneous samples. Multidimensional separations carried out using other coupled-column chromatographic techniques (such as supercritical fluid chromatography (SFC) with GC, and on-line trace enrichment-GC) have also been included in this review.     

火焰原子吸收光谱法测定生物样品中锌、铜和锰

生物样品经消化处理后,用火焰原子吸收光谱法测定样品中锌、铜和锰的含量,平均加标回收率为97.3%-102.4%,相对标准偏差(RSD)为0.65 %-1.40%.锌、铜和锰在给定范围内呈现良好的线性关系,相关系数分别为0.9994、0.9994和0.9983,方法简便,快速,结果可靠.     

色质联用技术在毒物分析中的应用

从生物样品中检测未知物,一直以来是毒物分析中的一个难点。如何有效地提取目标化合物,并选择适合的检测手段将未知物筛选出来,GC-MS方法是快速筛选多种毒物和药物的一个简便、可靠的手段。随着MS技术的不断发展,更灵敏、更准确的特性将使其成为药物和毒物分析中必不可少的一门技术。     

生物检材中氯敌鼠的LC-MS分析

氯敌鼠(chlorophacinone)为第一代抗凝血杀鼠剂,主要是拮抗维生素K1的活性,阻碍凝血酶原的合成,损害微血管,降低血液凝固能力,因而造成皮下出血和内脏大量出血而引起死亡。中毒潜伏期3～5天,死亡高峰为4～6天。氯敌鼠由于中毒潜伏期长,体内检测有一定难度,特别是经过抢救以后,体内含量降低,因此需要高灵敏度的方法进行检验。生物检材中氯敌鼠的分析,国内外均有报道,检测方法多用有机溶剂提取,HPLC法和紫外导数法分析。中国刑警学院谭家镒等人,采用GDX101大孔树脂提取,紫外导数法进行测定。有关用硅胶柱提取,LC-MS测定的方法未见报道。     

Long range one-dimensional ordering of lead phthalocyanine monolayer on InSb(1 0 0) (4 × 2)/c(8 × 2)

Sub-monolayer and monolayer of lead phthalocyanine deposited on InSb(1 0 0) (4 × 2)/c(8 × 2) surface have been investigated by scanning tunneling microscopy and low energy electron diffraction. Molecules first adsorb on the indium rows of the (4 × 2)/c(8 × 2) structure in the [1 1 0] direction and diffuse at the surface in order to form two-dimensional islands. The molecule-substrate interaction stabilizes the PbPc molecules on the In rows. It weakens the interaction between molecules located in adjacent rows resulting in numerous gliding planes between the molecular chains, in the direction parallel to the rows. At monolayer completion, a long-range one-dimensional order is adopted by the molecules in the [1 1 0] direction.     

Experimental identification of physical parameters of fluid-filled pipes using acoustical signal processing

A method is formulated for the identification of an unknown physical parameter of a fluid-filled pipe using the measurement of sound speed in the pipe. The method uses a simple formula which provides the relationship between the sound speed and a few physical parameters of the pipe: thickness, diameter, wall material constants and fluid constants. Once the sound speed in the pipe is measured, the simple formula can be used to extract one of the unknown parameters providing the remaining ones are known.The sound speed in the pipe is measured using a 3-transducer array. In order to demonstrate the potential of the technique the results of several measurements obtained in a water-filled steel pipe are presented.The required accuracy of the measurement of sound speed and of the specification of known parameters is analysed. The accuracy depends on the unknown parameter which is to be identified. For example, if the pipe thickness is the unknown parameter, the other parameters have to be known within a very narrow margin of error. On the contrary, if the fluid properties have to be identified the needed accuracy of known parameters gets much lower.     

Utilization of carbohydrates by radiation processing

Upgrading and utilization of carbohydrates such as chitosan, sodium alginate, carrageenan, cellulose, pectin have been investigated for recycling these bio-resources and reducing the environmental pollution. These carbohydrates were easily degraded by irradiation and various kinds of biological activities such as anti-microbial activity, promotion of plant growth, suppression of heavy metal stress, phytoalexins induction, etc. were induced. On the other hand, some carbohydrate derivatives, carboxymethylcellulose and carboxymethylstarch, could be crosslinked under certain radiation condition and produce the biodegradable hydrogel for medical and agricultural use.     

Structure of enantiopure and racemic alanine adlayers on Cu(1 1 0)

Plane wave density functional theory has been employed to analyze the structure of alanine adlayers on the Cu(1 1 0) surface. Alanine forms (3 × 2) adlayers on Cu(1 1 0) that are closely related to the structures of glycine on the same surface. There is essentially no energy difference between the most stable racemic and enantiopure alanine adlayers. This observation implies that adsorption of racemic alanine on Cu(1 1 0) will result in a pseudoracemate adlayer.     

Gamma-rays from Mössbauer sources: a low-dose approach to cancer therapy

Summary A new approach to cancer treatment using low-energy gamma-rays is discussed. Cultures of bone marrow mononuclear cells collected from normal donors and patients with chronic myelogenous leukaemia have been studied after the addition of hematin, at different concentrations, and irradiation by a M?ssbauer gamma-ray source. Growth stimulation has been observed when hematin is added to normal bone marrow cultures, while growth inhibition is observed when hematin is added to leukaemic cultures. The effect becomes then more pronounced when hematin is used in combination with M?ssbauer gamma-rays.     

Scanning probe microscopy characterization of gold-chemisorbed poplar plastocyanin mutants

Two poplar plastocyanin mutants adsorbed onto gold electrodes have been characterized at single molecule level by scanning probe microscopy. Immobilization of the two redox metalloprotein mutants on Au(1 1 1) surface was achieved by either a disulphide bridge (PCSS) or a single thiol (PCSH), both the anchoring groups having been introduced by site-directed mutagenesis. Scanning tunneling microscopy (STM) and atomic force microscopy (AFM) analysis gives evidence of a stable and robust binding of both mutants to gold. The lateral dimensions, as estimated by STM, and the height above the gold substrate, as evaluated by AFM, of the two mutants well agree with crystallographic sizes. A narrower height distribution is observed for PCSS compared to PCSH, corresponding to a more homogeneous orientation of the former mutant adsorbed onto gold. Major differences between the mutants are observed by electrochemical STM. In particular, the image contrast of adsorbed PCSS is affected by tuning the external electrochemical potential to the redox levels of the mutant, consistent with some involvement of copper active site in the tunneling process. On the contrary, no contrast variation is observed in electrochemical STM of adsorbed PCSH. Moreover, scanning tunneling spectroscopy experiments reveal asymmetric I–V characteristics for single PCSS proteins, reminiscent of a rectifying-like behaviour, whereas an almost symmetric I–V relation is observed for PCSH.