Ion recognition: application of symmetric and asymmetric schiff bases and their complexes for the fabrication of cationic and anionic membrane sensors to determine ions in real samples

Schiff base compounds refer to the branch of supra-molecules and can be used as sensing material in the construction of potentiometric ion selective electrodes (ISEs). This relatively modern field has been subject to extensive research in the period of 1999-2007 when more than 100 ISEs employing Schiff bases were constructed. The quantitative high-throughput detection of 29 cations and 7 anions has been demonstrated in various scientific branches, such as biomedicine, pharmacy, biochemistry, pharmacology, environmental chemistry, food technology, and agriculture. This review discusses Schiff base compounds and their applications in the design and development of ion selective sensors and microsensors.

Determination of sexual hormones in liquid cosmetics by polymer monolith microextraction coupled with high performance liquid chromatography

A method was presented for the determination of testosterone, methyltestosterone and progesterone in liquid cosmetics by coupling polymer monolith microextraction (PMME) to high performance liquid chromatography with UV detection. A poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was selected as the extraction medium, which showed high extraction capacity towards these compounds. To achieve optimum extraction performance, several parameters relating to PMME were investigated, including extraction flow rate and pH value, inorganic salt and organic phase concentration of the sample matrix. By simple dilution with phosphate solution and filtering, the sample solution then could be directly injected into the device for extraction. The limits of detection of testosterone, methyltestosterone and progesterone were calculated to be 2, 3, 2, 8 and 4.6 mu g/L. Good linearity was achieved in the range of 10 to 1000 mu g/L with a linear coefficient. r value above 0. 996. Excellent method reproducibility was found by intra- and inter-day precisions, yielding the relative standard deviations of < 7. 7 % and < 7. 5 %, respectively. Recovery for them in the real samples was between 83% and 119%.

Effect of partial site occupation on the magnetic properties of Nd2Fe17-xSix by supercell calculation

The magnetic properties of the Nd2Fe17-xSix intermetallic compounds are studied by means of spin-polarized supercell calculations in which the selected sites of substitution are close to the situations in real samples. It is shown that the average Fe moment increases with x and saturates near x = 3. This correlates quite well with the experimental dependence of Te on x. The difference between supercell and unit cell calculations are pointed out and the influence of Si atoms on the density of states of the nearby Fe atoms is emphasized. (C) 1997 American Institute of Physics.

Fluorescence Hydrogen Peroxide Probe Based on a Microstructured Polymer Optical Fiber Modified with a Titanium Dioxide Film

A highly sensitive microstructured polymer optical fiber (MPOF) probe for hydrogen peroxide was made by forming a rhodamine 6G-doped titanium dioxide film on the side walls of array holes in an MPOF. It was found that hydrogen peroxide only has a response to the MPOF probe in a certain concentration of potassium iodide in sulfuric acid solution. The calibration graph of fluorescence intensity versus hydrogen peroxide concentration is linear in the range of 1.6 x 10(-7) mol/L to 9.6 x 10(-5) mol/L. The method, with high sensitivity and a wide linear range, has been applied to the determination of trace amounts of hydrogen peroxide in a few real samples, such as rain water and contact lens disinfectant, with satisfactory results.

Cellulose acetate polymer film modified microstructured polymer optical fiber towards a nitrite optical probe

A novel microstructured polymer optical fiber (MPOF) probe for nitrites (NO(2)(-)) detection was made by forming rhodamine 6G (Rh 6G)-doped cellulose acetate (CA) on the side wall of array holes in a MPOF It was found that the MPOF probe only have a response to nitrites in a certain concentration of sulfuric acid solution The calibration graph of fluorescence intensity versus nitrites concentration was linear in the range of 2.0 x 10(-4) g/ml-5.0 x 10(-3) g/ml. The method possesses case of chemical modification, low cost design, and potential for direct integration with existing instrumentation, and has been applied to the determination of nitrites in real samples with satisfactory results. (C) 2010 Elsevier B.V. All rights reserved

Pressurized electrochromatography coupled with electrospray ionization mass spectrometry for analysis of peptides and proteins

Pressurized capillary electrochromatography (pCEC) was coupled with electrospray ionization mass spectrometry (ESI-MS) using a coaxial sheath liquid interface. It was used for separation and analysis of peptides and proteins. The effects of organic modifier and applied voltage on separation were investigated, and the effects of pH value of the mobile phase and the concentration of the electrolyte on ESI-MS signal were investigated. The resolution and detection sensitivity with different separation methods (pCEC, capillary high-performance liquid chromatography) coupled on-line with mass spectrometry were compared for the separation of a peptide mixture. To evaluate the feasibility and reliability of the experimental setup of the system, tryptic digests of cytochrome c and modified protein as real samples were analyzed by using pCEC-ESI-MS.

Determination of 1-phenyl-3-methyl-5-pyrazolone-labeled carbohydrates by liquid chromatography and micellar electrokinetic chromatography

In this paper, the method for the derivatization of carbohydrates with 1-phenyl-3-methyl-5-pyrazolone (PMP) was simplified. One-third of the derivatization time was saved. Five monosaccharide derivatives have been well separated by MEKC and HPLC under optimized conditions. Good reproducibility could be obtained with relative standard deviation (RSD) values of the migration times within 5.0 and 2.3%, respectively. Furthermore, the developed methods have been successfully applied to the analysis of carbohydrates in Aloe powder and food. These methods are quite useful for routine analysis of monosaccharides and oligosaccharides in real samples. (C) 2003 Elsevier B.V. All rights reserved.

Direct electrochemistry of glucose oxidase and biosensing for glucose based on carbon nanotubes@SnO2-Au composite

Multiwalled carbon nanotubes@SnO2-Au (MWCNTs@SnO2-Au) composite was synthesized by a chemical route. The structure and composition of the MWCNTs@SnO2-Au composite were confirmed by means of transmission electron microscopy, X-ray photoelectron and Raman spectroscopy. Due to the good electrocatalytic property of MWCNTs@SnO2-Au composite, a glucose biosensor was constructed by absorbing glucose oxidase (GOD) on the hybrid material. A direct electron transfer process is observed at the MWCNTs@SnO2-Au/GOD-modified glassy carbon electrode. The glucose biosensor has a linear range from 4.0 to 24.0 mM, which is suitable for glucose determination by real samples. It should be worthwhile noting that, from 4.0 to 12.0 mM, the cathodic peak currents of the biosensor decrease linearly with increasing the glucose concentrations in human blood. Meanwhile, the resulting biosensor can also prevent the effects of interfering species.

Multilayer films of carbon nanotubes and redox polymer on screen-printed carbon electrodes for electrocatalysis of ascorbic acid

Multilayer films containing multiwall carbon nanotubes and redox polymer were successfully fabricated on a screen-printed carbon electrode using layer-by-layer (LBL) assembled method. UV-vis spectroscopy, X-ray photoelectron spectroscopy, field-emission scanning electron microscopy and electrochemical method were used to characterize the assembled multilayer films. The multilayer films modified electrodes exhibited good electrocatalytic activity towards the oxidation of ascorbic acid (AA). Compared with the bare electrode, the oxidation peak potential negatively shifted about 350 mV (versus Ag/AgCl). Furthermore, the modified screen-printed carbon electrodes (SPCEs) could be used for the determination of ascorbic acid in real samples.

Amperometric enzyme electrode for the determination of hydrogen peroxide based on sol-gel/hydrogel composite film

A new type of organic-inorganic composite material was prepared by sol-gel method, and a peroxidase biosensor was fabricated by simply dropping sor-gel-peroxidase mixture onto glassy carbon electrode surface. The sol-gel composite film and enzyme membrane were characterized by Fourier-transform infrared (FT-IR) spectroscopy and EQCM, the electrochemical behavior of the biosensor was studied with potassium hexacyanoferrate(II) as a mediator, and the effects of pH and operating potential were explored for optimum analytical performance by using amperometric method. The response time of the biosensor was about 10 s; the linear range was up to 3.4 mM with a detection limit of 5 x 10(-7) M. The sensor also exhibited high sensitivity (15 mu A mM(-1)) and good long-term stability. In addition, the performance of the biosensor was investigated using flow injection analysis (FIA), and the determination of hydrogen peroxide in real samples was discussed. (C)2000 Elsevier Science B.V. All rights reserved.

End-column amperometric detection of 5-fluorouracil by capillary zone electrophoresis with a carbon fiber microelectrode

A rapid and sensitive detection method for the determination of 5-fluorouracil(5-FU) in real samples such as human urine and bovine serum albumin (BSA) was described. A carbon fiber microdisk electrode was used to perform end-column amperometric detection in capillary zone electrophoresis. The detection limit was as low as 2.5x10(-7) M and the wider linear range for the concentration was between 5x10(-6) and 1x10(-4) M with a correlation coefficient of 0.995.

KALMAN FILTERING FOR RESOLUTION OF OVERLAPPING LINES IN INDUCTIVELY COUPLED PLASMA ATOMIC EMISSION-SPECTROMETRY

A Kalman filter was developed for resolving overlapping lines in inductively coupled plasma atomic emission spectrometry (ICP-AES) and evaluated experimentally with the determination of La in the presence of Ho, and Cu in the presence of Pr. The whiteness of the innovation sequence for an optimal filter was explored to be the criterion for the correction of the wavelength positioning errors which may occur in spectral scans. Under the conditions of the medium-resolution spectrometer and 1.5 pm step size in scans, the filter effectively resolved the Cu/Pr line pair having a small peak separation of 4.8 pm. For the La/Ho line pair with a peak distance of 9.8 pm, an unbiased estimate for La concentration was still obtained even when the signal-to-background ratio was down to 0.048. Favourable detection limits for real samples were achieved. Unstructured backgrounds were modeled theoretically and all spectral scans therefore did not require the correction for solvent.

Determination of 30 free fatty acids in two famous Tibetan medicines by HPLC with fluorescence detection and mass spectrometric identification

A simple and sensitive high-performance liquid chromatographic (HPLC) method with fluorescence detection and mass spectrometric identification has been developed for analysis of 30 long-chain and short-chain free Fatty acids (FFAs). The fatty acids were derivatized to their esters with 1-[2-(p-toluenesulfonate)ethyl]-2-phenylimidazole-[4,5-f]-9,10-phenanthrene (TSPP) in N,N-dimethylformamide (DMF) at 90 degrees C with anhydrous K2CO3 as catalyst. A mixture Of C-1-C-30 fatty acids was completely separated within 60 min by gradient elution on a reversed-phase C-8 column. Qualitative identification of the acids was performed by atmospheric-pressure chemical ionization mass spectrometry (APCI-MS) in positive-ion mode. The fluorescence excitation and emission wavelengths were 260 and 380 nm, respectively. Quantitative determination of the 30 acids in two Tibetan medicines Gentiana straminea and G. dahurica was performed. The results indicated that the medicines contained many FFAs. Linear correlation coefficients for the FFA derivatives were > 0.9991. Relative standard deviations (RSDs, n = 6) for the fatty acid derivatives were < 3%. Detection limits (at a signal-to-noise ratio of 3:1) were 3.1-38 fmol. When the fatty acid derivatives were determined in the two real samples results were satisfactory and the sensitivity and reproducibility of the method were good.

Real-Time Measurement on Deformation Fields of Hole-Excavated Samples under Impact Tension

In this paper, the real-time deformation fields are observed in two different kinds of hole-excavated dog-bone samples loaded by an SHTB, including single hole sample and dual holes sample with the aperture size of 0.8mm. The testing system consists of a high-speed camera, a He-Ne laser, a frame grabber and a synchronization device with the controlling accuracy of I microsecond. Both the single hole expanding process and the interaction of the two holes are recorded with the time interval of 10 mu s. The observed images on the sample surface are analyzed by newly developed software based on digital correlation theory and a modified image processing method. The 2-D displacement fields in plane are obtained with a resolution of 50 mu m and an accuracy of 0.5 mu m. Experimental results obtained in this paper are proofed, by compared with FEM numerical simulations.

Real-Time Measurement on Deformation Fields of Notched Samples Under Impact Tension

In this paper, a real-time and in situ optical measuring system is reported to observe high-velocity deformations of samples subjected to impact loading. The system consists of a high-speed camera, a He-Ne laser, a frame grabber, a synchronization device and analysis software based on digital correlation theory. The optical system has been adapted to investigate the dynamic deformation field and its evolution in notched samples loaded by an split Hopkinson tension bar, with a resolution of 50 pin and an accuracy of 0.5 mum. Results obtained in experiments are discussed and compared with numerical simulations. It is shown that the measuring system is effective and valid.