Microfabricated bioreactor chips for immobilised enzyme assays

A microfabricated device is reported that has been designed to permit the in situ packing of a section of channel with enzyme immobilised onto controlled pore glass (CPG). It is fabricated from glass and polydimethylsiloxane and to prevent dead volumes, has dedicated channels for packing the reactor. The device has the advantage of being simple in design, the flow through enzyme reactor channel being simply a widened section of the analyte channel. The system is suitable for both hydrodynamic and electro-osmotic pumping, and is designed such that when the packing is exhausted it can be repacked. Controlled pore glass provides a reproducible none swelling, high porosity medium onto which the enzyme could be immobilised. The large particle size meant that it was vital to optimise the immobilisation procedure in order to achieve acceptable enzyme activity. The microfabricated device was developed with two enzymes of different molecular masses; alkaline phosphatase and xanthine oxidase. The pore size of the CPG was found to be very important for xanthine oxidase, where the 697 Å pore size (120-200 mesh) CPG was found to give the highest activity (18-20% activity retained after immobilisation). The microfabricated device was used for the assay of p-nitrophenyl phosphate and hypoxanthine with spectrophotometric detection at 405 and 470 nm, respectively. The limits of detection were 5 and 8 μM, respectively.     

Protection of immobilized sulfhydryl groups against autooxidation by alterations in their microenvironment

Immobilized sulfhydryl groups were prepared by partial thiolation of NH₂-glass beads. The microenvironment of the immobilized SH groups was varied by different chemical modifications of neighboring NH₂ groups. Introduction of a strong charge in the surroundings of immobilized sulfhydryls results in their dramatic stabilization against autooxidation. This effect is due to the salting of O₂ from the surface microlayer of the thiolated beads.     

Advances in two-dimensional GC with glass capillary columns

A versatile two-dimensional gas chromatograph is described, consisting of 2 separate ovens, one intermediate trap, an auxiliary inlet, and the necessary hardware to effect off-line switching according to the principle of Deans. The unit has been designed for use with high resolution glass capillary columns. The performance of individual instrumental components was critically evaluated. Results showed that low dead volume glass to metal connections were required in the manifold and detector lines to minimize extra-column effects. The mass of the intermediate trap must be low to allow rapid heating. Operational parameters are discussed and examples of some applications are shown.     

Physicochemical characterization of biological glass coatings

Metallic implants are widely used in orthopaedic surgery but metal release has been reported by several authors. High metallic ion concentration in surrounding tissues may play a major role in therapeutic failure. We have investigated in vivo and in vitro two biological glasses (BVA and BVH) used as coatings of metal implants. Physicochemical characterization was made by several complementary methods, particularly particle induced x‐ray emission (PIXE) and energy‐dispersive x‐ray spectroscopy (EDXS) associated with electronic microscopy. Analyses clearly show the differences of behaviour between both glasses. The BVA glass is bioactive, i.e. it develops a direct chemical bond between prosthesis and bone by the formation of a calcium phosphate layer at its surface. These structural and compositional modifications are caused by hydrolysis of the glass. After its dissolution BVA glass is replaced by bone, which ensures better integration of the implant in the bone site. The BVH glass is not bioactive and is used as a cement to isolate the metal implant from the biological environment, but the coating disaggregates with implantation time and glass grains migrate through the bony lacuna network. Copyright © 2003 John Wiley & Sons, Ltd.     

Prospects of Sol-Gel Process for Spectral Hole-Burning Glasses

Persistent spectral hole burning was studied in Eu³⁺ ions-doped Al₂O₃-SiO₂ glass prepared by a sol-gel method. The gel synthesized by the hydrolysis of Si- and Al-alkoxides and EuCl₃·6H₂O was heated in air and hydrogen gas atmospheres. For the glass heated in air to contain OH bonds, the hole was formed by the photoinduced rearrangement of the OH bonds surrounding the Eu³⁺ ions, and was thermally refilled and erased above 200 K. On the other hand, the glass heated in hydrogen gas showed the hole spectrum above 200 K. It was found that the hole depth was independent of the temperature and was 7% of the total intensity at room temperature. The proposed mechanism was the electron transfer between the Eu³⁺ ions and the defect centers formed in glass matrix.     

Mechanical properties and transition temperatures of crosslinked-oriented gelatin

 This second part of a systematic study of the properties of crosslinked-oriented gelatin involves the effects of orientation and water content on the glass transition temperature T _g and on the melting behavior. The samples were the same as those in the preceding study, and their transition temperatures were determined by both differential scanning calorimetry and dynamic mechanical thermal analysis. The crosslinked gelatin which had been room-conditioned showed two transition temperatures: the lower one was attributed to T _g of the water-plasticized gelatin, and the higher one was interpreted as T _g of dried gelatin superimposed by melting. A rather unusual situation arose because of the fact that the T _g and melting temperatures T _m (217 and 230 ^°C, respectively) are so similar. Using water as plasticizer not only decreases T _g but produces imperfect crystallites which melt below the T _g of the system. The presence of the amorphous phase in the glassy state would presumably make it essentially impossible to define a melting point or crystallization temperature in the normal manner, as an equilibrium between crystalline and amorphous phases. Received: 8 October 1996 Accepted: 2 November 1995     

Analysis of Early Medieval Glass Beads – The Raw Materials to Produce Green, Orange and Brown Colours

 Monochrome coloured glass beads of the Merovingians (5^th–7^th cent. AD) have been examined by different analytical methods. The elemental composition of a large number of mostly unprepared beads have been measured non-destructively by X-ray fluorescence analysis. After subtracting the content of the colouring oxides of the glass beads and normalising the residual values to 100% an identical soda-lime-glass matrix was obtained. X-ray diffraction was used for the identification of the crystalline colouring and opacifying pigments (SnO₂, Cu, Cu₂O, PbSnO₃), and scanning electron microscopy as well as electron probe microanalysis were applied to study the microstructure and the composition of white, brown, green, orange and yellow coloured glass beads. Oxidised metals, alloys (lead, copper, bronze, brass and mixtures of them) and iron smelting slag have been identified as raw materials to colour the soda-lime-glass.     

玻璃载体表面脱氧核糖核酸的固定及其化学发光检测

用硅烷化偶联剂把ＤＮＡ直接共价固定在载玻片表面，将辣根过氧化物酶标记的探针与之进行核酸杂交，杂交后用增强的化学发光检测。方法的检出限为７５ｐｇ。研究了ＤＮＡ分子固定在玻璃载体表面的各种条件，并建立了在玻璃载体表面进行核酸杂交的体系，为研究光纤ＤＮＡ生物传感器打下了基础。     

Determination of the diastereomers of vitamin K1

A method is described for the gas-chromatographic determination of the diastereomers of vitamin K₁ (phylloquinone) in the form of their dihydro dimethyl ethers. The reported method of derivatization and chromatographic analysis in conjunction with optical rotation measurements are useful approaches for characterization of vitamin K₁ samples with respect to their origin.     

Synthesis and Characterization of Fluoro- and Chloro- bimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal alkoxides was retained to a large extent in 4 ： 1 halogenated alcohol-benzene solution. The heteronuclear NMR spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern. SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.