Flow and Sequential Injection Manifolds for the Spectrophotometric Determination of Captopril Based on its Oxidation by Fe(III)

 Two new simple and rapid methods are reported for the accurate and precise spectrophotometric determination of captopril (CPL) using flow (FI) and sequential injection (SI) analysis. The methods are based on the fast oxidation of CPL by Fe(III). The produced Fe(II) reacts with 2,2′-dipyridyl-2-pyridylhydrazone (DPPH) in acidic medium to form a colored complex which is monitored spectrophotometrically at 535 nm. Both methods allow the determination of the analyte up to 1000 mg L⁻¹ at a sampling rate of 120 and 60 injections per hour for FI and SI, respectively. The methods are very precise [s _r=0.8 and 1.2% at 500 mg L⁻¹ CPL (n=12) for FI and SI, respectively] and the 3σ detection limits (c _L=4.0 and 7.0 mg L¹, respectively) are quite satisfactory. Their application to a variety of anti-hypertensive commercial pharmaceutical formulations showed excellent results (relative errors, e _r, < ± 1.6% in all cases compared to an official HPLC method), while common pharmaceutical excipients were found not to interfere. Recovery experiments further verified the accuracy of the developed methods, as the percent recoveries were in the range of 98.1–102.5%. Author for correspondence. E-mail: themelis@chem.auth.gr Received May 9, 2002; accepted January 8, 2003 Published online May 5, 2003     

Kinetics and mechanism of the Co(II)-assisted oxidation of thioureas by dioxygen

Catalytic oxidation of N,N'-dimethylthiourea and thiourea by dioxygen in water using a new cobalt(II) complex of octasulfophenyltetrapyrazinoporphyrazine was performed under mild conditions. The reaction is shown to include the formation of an intermediate anionic five-coordinate complex followed by an unusual two-electron oxidation to produce the corresponding urea and elemental sulfur (S8). Kinetic and thermodynamic parameters for the different reaction steps of the process were determined. Drastic differences in catalytic activity of cobalt and iron octasulfophenyltetrapyrazinoporphyrazines were observed.     

Preparation of a molecularly imprinted polymer for the solid-phase extraction of scopolamine with hyoscyamine as a dummy template molecule

Molecularly imprinted polymers (MIPs) selective for scopolamine were produced using hyoscyamine (a close structural analogue) as template molecule. The produced polymers were used as media for solid-phase extraction, exhibiting selective binding properties for the analyte from biological samples. Human and calf urine and serum were processed on the MIP under various extraction protocols. The best performance was observed after loading the analyte in aqueous environment facilitating retention on the MIP by non-selective hydrophobic interactions. The MIPs were subsequently washed using an optimised solvent system to enable selective desorption of the analyte. Other related and non-related compounds were accessed to evaluate molecular recognition properties. Recoveries of up to 79% were achieved for the analyte of interest from biological samples.     

A study of the behaviour of some new column materials in the chromatographic analysis of Cinchona alkaloids

Summary A major problem in the HPLC analysis of alkaloids is the poor peak shape and consequently low resolution, due to the interactions of the basic alkaloids with the residual acidic silanol groups of most reversed phase materials. The performance of new packing materials specially designed for the separation of basic compounds has been studied using mobile phases without the special additives commonly applied in the analysis of alkaloids. Strongly basic Cinchona alkaloids were used as test compounds. Retention characteristics and selectivities of each material were studied, after mobile phase optimisation for the column. The influence of the major factors (nature and content of the organic modifier, pH value, salt concentration) affecting resolution was studied. The mobile phases were chosen so that they could be used in thermospray LC-MS. The addition of salts to the mobile phase improves separation but in general the modification of the mobile phase gave little change in selectivity. The performance of silicabased C₁₈ material proved superior to the polymer materials tested.     

Immunoaffinity chromatography for the sample pretreatment of Taxus plant and cell extracts prior to analysis of taxanes by high-performance liquid chromatography

The application of immunoaffinity chromatography for the purification of Taxus plant and cell extracts prior to the HPLC analysis is described. Polyclonal antibodies raised against 10-deacetylbaccatin III (10-DAB III), paclitaxel's main precursor in plant, were characterised by enzymed-linked immunosorbent assay. Immunoglobulins from selected antisera were immobilised on CNBr-activated Sepharose 4B. The immunoaffinity column was used for the purification of plant and plant cell culture extracts prior to their analysis by HPLC. Immunoaffinity chromatography enabled the selective concentration of taxoids and enhanced sample clean-up.     

On the development of high-throughput and area-efficient multi-mode cryptographic hash designs in FPGAs

In this paper, area-efficient and high-throughput multi-mode architectures for the SHA-1 and SHA-2 hash families are proposed and implemented in several FPGA technologies. Additionally a systematic flow for designing multi-mode architectures (implementing more than one function) of these families is introduced. Compared to the corresponding architectures that are produced by a commercial synthesis tool, the proposed ones are better in terms of both area (at least 40%) and throughput/area (from 32% up to 175%). Finally, the proposed architectures outperform similar existing ones in terms of throughput and throughput/area, from 4.2× up to 279.4× and from 1.2× up to 5.5×, respectively.     

A Framework for Data Partitioning for C++ Data-Intensive Applications

We present an automated framework that partitions the code and data types for the needs of data management in an object-oriented source code. The goal is to identify the crucial data types from data management perspective and separate these from the rest of the code. In this way, the design complexity is reduced allowing the designer to easily focus on the important parts of the code to perform further refinements and optimizations. To achieve this, static and dynamic analysis is performed on the initial C++ specification code. Based on the analysis results, the data types of the application are characterized as crucial or non-crucial. Continuing, the initial code is rewritten automatically in such a way that the crucial data types and the code portions that manipulate them are separated from the rest of the code. Experiments on well-known multimedia and telecom applications demonstrate the correctness of the performed automated analysis and code rewriting as well as the applicability of the introduced framework in terms of execution time and memory requirements. Comparisons with Rational’s Quantify^TM suite show the failure of Quantify^TM to analyze correctly the initial code for the needs of data management.     

New fast QR decomposition least squares adaptive algorithms

This paper presents two new, closely related adaptive algorithms for LS system identification. The starting point for the derivation of the algorithms is the inverse Cholesky factor of the data correlation matrix, obtained via a QR decomposition (QRD). Both algorithms are of O(p) computational complexity, with p being the order of the system. The first algorithm is a fixed order QRD scheme with enhanced parallelism. The second is an order recursive lattice type algorithm based exclusively on orthogonal Givens rotations, with lower complexity compared to previously derived ones. Both algorithms are derived following a new approach, which exploits efficient the and order updates of a specific state vector quantity     

A Frequency Multiplication Resonant Inverter With Constant Frequency Phase Control

The schematic and analysis of a voltage-fed resonant inverter are presented in this paper. The topology of the inverter allows operation of the resonant tank at higher harmonics and multiples of the switching frequency. The resulting loss in voltage gain is compensated through the use of multiple commutation poles employing low-cost modestly rated MOSFETs. The proposed topology can control power throughput at a fixed frequency through pole phase-shift modulation. Zero voltage switching is maintained down to no load and within the entire input voltage range. Measurements from a multimegahertz 100-W inverter confirm the theoretical predictions, as well as the suggested design and control approach.