Selection of an analytical method for evaluating bovine serum albumin concentrations in pharmaceutical polymeric formulations

Bovine serum albumin (BSA) is a commonly used model protein in the development of pharmaceutical formulations. In order to assay its release from various dosage forms, either the bicinchoninic acid (BCA) assay or a more specific size-exclusion high performance liquid chromatography (SE-HPLC) method are commonly employed. However, these can give erroneous results in the presence of some commonly-used pharmaceutical excipients. We therefore investigated the ability of these methods to accurately determine BSA concentrations in pharmaceutical formulations that also contained various polymers and compared them with a new and compared with a new reverse-phase (RP)–HPLC technique. We found that the RP-HPLC technique was the most suitable method. It gave a linear response in the range of 0.5 -100 µg/ml with a correlation coefficient of 0.9999, a limit of detection of 0.11 µg/ml and quantification of 0.33 µg/ml. The performed ‘t’ test for the estimated and theoretical concentration indicated no significant difference between them providing the accuracy. Low % relative standard deviation values (0.8-1.39%) indicate the precision of the method. Furthermore, the method was used to quantify in vitro BSA release from polymeric freeze-dried formulations.

Strength and ductility of RC jacketed columns: a simplified analytical method

Reinforced concrete (RC) jacketing is a common method for retrofitting existing columns with poor structural performance. It can be applied in two different ways: if the continuity of the jacket is ensured, the axial load of the column can be transferred to the jacket, which will be directly loaded; conversely, if no continuity is provided, the jacket will induce only confinement action. In both cases the strength and ductility evaluation is rather complex, due to the different physical phenomena included, such as confinement, core-jacket composite action, preload and buckling of longitudinal bars.
Although different theoretical studies have been carried out to calculate the confinement effects, a practical approach to evaluate the flexural capacity and ductility is still missing. The calculation of these quantities is often related to the use of commercial software, taking advantage of numerical methods such as fibre method or finite element method.
This paper presents a simplified approach to calculate the flexural strength and ductility of square RC jacketed sections subjected to axial load and bending moment. In particular the proposed approach is based on the calibration of the stress-block parameters including the confinement effect. Equilibrium equations are determined and buckling of longitudinal bars is modelled with a suitable stress-strain law. Moment-curvature curves are derived with simple calculations. Finally, comparisons are made with numerical analyses carried out with the code OpenSees and with experimental data available in the literature, showing good agreement.

Development of a simple analytical method for the simultaneousdetermination of paracetamol, paracetamol-glucuronide andp-aminophenol in river water

Paracetamol is among the most worldwide consumed pharmaceuticals. Although its occurrence in the environment is well documented, data about the presence of its metabolites and transformation products is very scarce. The present work describes the development of an analytical method for the simultaneous determination of paracetamol, its principal metabolite (paracetamol-glucuronide) and its main transformation product (p-aminophenol) based on solid phase extraction (SPE) and high performance liquid chromatography coupled to diode array detection (HPLC-DAD). The method was applied to analysis of river waters, showing to be suitable to be used in routine analysis. Different SPE sorbents were compared and the use of two Oasis WAX cartridges in tandem proved to be the most adequate approach for sample clean up and pre-concentration. Under optimized conditions, limits of detection in the range 40–67 ng/L were obtained, as well as mean recoveries between 60 and 110% with relative standard deviations (RSD) below 6%. Finally, the developed SPE-HPLC/DAD method was successfully applied to the analysis of the selected compounds in samples from seven rivers located in the north of Portugal. Nevertheless all the compounds were detected, it was the first time that paracetamol-glucuronide was found in river water at concentrations up to 3.57 μg/L.

Validation of an analytical method for nitrous oxide (N2O) laughing gas by headspace gas chromatography coupled to mass spectrometry (HS-GC-MS): Forensic application to a lethal intoxication.

Drug abuse is a widespread problem affecting both teenagers and adults. Nitrous oxide is becoming increasingly popular as an inhalation drug, causing harmful neurological and hematological effects. Some gas chromatography-mass spectrometry (GC-MS) methods for nitrous oxide measurement have been previously described. The main drawbacks of these methods include a lack of sensitivity for forensic applications; including an inability to quantitatively determine the concentration of gas present. The following study provides a validated method using HS-GC-MS which incorporates hydrogen sulfide as a suitable internal standard allowing the quantification of nitrous oxide. Upon analysis, sample and internal standard have similar retention times and are eluted quickly from the molecular sieve 5Å PLOT capillary column and the Porabond Q column therefore providing rapid data collection whilst preserving well defined peaks. After validation, the method has been applied to a real case of N2O intoxication indicating concentrations in a mono-intoxication.

Studies on oxamyl : analytical method development and investigation of fate in peach seedlings and corn seeds

A high performance liquid chromatographic method employing two columns connected in series and separated~y·a.switching valve has been developed for the analysis of the insecticide/ nematicide oxamyl (methyl-N' ,N'-dimethyl-N-[(methylcarbamoyl) oxy]-l-thiooxarnimidate) and two of its metabolites. A variation of this method involving two reverse phase columns was employed to monitor the persistence and translocation of oxamyl in treated peach seedlings. It was possible to simultaneously analyse for oxamyl and its corresponding oxime (methyl-N',N'-dimethyl-N-hydroxy-l-thiooxamimidate}, a major metabolite of oxamyl in plants, without prior cleanup of the samples. The method allowed detection of 0.058 pg oxamyl and 0.035 p.g oxime. On treated peach leaves oxamyl was found to dissipate rapidly during the first two-week period, followed by a period of slow decomposition. Movement of oxamyl or its oxime did not occur in detectable quantities to untreated leaves or to the root or soil. A second variation of the method which employed a size exclusion column as·the first column and a reverse phase column as the second was used to monitor the degradation of oxamyl in treated, planted corn seeds and was suitable for simultaneous analysis of oxamyl, its oxime and dimethylcyanoformamide (DMCF), a metabolite of oxamyl. The method allowed detection of 0.02 pg oxamyl, 0.02 p.g oxime and 0.005 pg DMCF. Oxamyl was found to persist for a period of 5 - 6 weeks, which is long enough to permit oxamyl seedtreatment to be considered as a potential means of protecting young corn plants from nematode attack. Decomposition was found to be more rapid in unsterilized soil than in sterililized soil. DMCF was found to have a nematostatic effect at high concentrations ( 2,OOOpprn), but at lower concentrations no effect on nematode mobility was observed. Oxamyl, on the other hand, was found to reduce the mobility of nematodes at concentrations down to 4 ppm.

An analytical method for capacity dimensioning of WCDMA with high speed wireless link

Capacity dimensioning is one of the key problems in wireless network planning. Analytical and simulation methods are usually used to pursue the accurate capacity dimensioning of wireless network. In this paper, an analytical capacity dimensioning method for WCDMA with high speed wireless link is proposed based on the analysis on relations among system performance and high speed wireless transmission technologies, such as H-ARQ, AMC and fast scheduling. It evaluates system capacity in closed-form expressions from link level and system level. Numerical results show that the proposed method can calculate link level and system level capacity for WCDMA system with HSDPA and HSUPA.

Investigation of Iron (III) desferrioxamine B oxalate ligand exchange by UV-vis spectroscopy: the next step in developing a quantitative analytical method for measuring bioavailable iron in marine ecosystems

To date there are no analytical techniques designed to exclusively measure bioavailable iron in marine environments. The goal of this research is to develop such a technique by isolating the bioavailable iron using the terrestrial siderophore desferrioxamine B (DFB). This project contained many challenging aspects, but the specific goal of this study was to develop a robust analytical technique for quantification of Fe(III)-DFB complexes at nanomolar concentrations. Past work showed that oxalate (Ox) promotes photodissociation of Fe(III)-DFB to Fe(Il), and we are specifically interested in the mechanism of this process. A model was developed using known thermodynamic constants for Fe(III)-DFB and Fe(III) oxalato complexes and adjusting for ionic strength. The model was confirmed by monitoring the UV-VIS absorbance of the system at a variety of oxalate concentrations and pH. The model did not include ternary complexes. Next., the rate of Fe(1I) production during UV irradiation was examined. The results showed that the rate of Fe(II) production was based entirely on the [Fe(Ox)?]3- speciation, and that reoxidation of Fe(II) occurred via reactive oxygen intermediates. This reoxidation could be avoided by either decreasing the oxygen concentration or by adding a Fe(II) stabilizing reagent, such as ferrozine. Further studies need to be done to confirm that these results apply at sub nanomolar concentrations, and the issue of Fe(II) reoxidation at lower Fe concentrations needs to be addressed.

A factor analytical method to interactive effects dynamic panel models with or without unit root

In a recent study, Bai (Fixed-Effects Dynamic Panel Models, A Factor Analytical Method. Econometrica 81, 285-314, 2013a) proposes a new factor analytic (FA) method to the estimation of dynamic panel data models, which has the unique and very useful property that it is completely bias-free. However, while certainly appealing, it is restricted to fixed effects models without a unit root. In many situations of practical relevance this is a rather restrictive consideration. The purpose of the current study is therefore to extend the FA approach to cover models with multiple interactive effects and a possible unit root.

Development and validation of an analytical method by RP-HPLC for quantification of sibutramine hydrochloride in pharmaceutical capsules

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A simple and green analytical method for determination of glyphosate in commercial formulations and water by diffuse reflectance spectroscopy

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

A Simple and Green Analytical Method for the Determination of Formaldehyde

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Analytical method for the design of a machine with aligned and skewed permanent magnets

This work aims to present the design and the evaluation of a standard multi-pole machine with permanent magnets inserted in the rotor by two different geometrical forms: aligned and skewed magnets. The design (new analytical method) was based on a standard 250 W three phase 12-pole induction motor (squirrel cage rotor type), beginning with the original stator constructive data to calculate the magnetic flux density to determine the permanent magnets. In the development of the work, a simple and modular rotor was built reusing the original 12-pole stator (concentrated windings). The machine was evaluated in a laboratory for the purpose of checking the quantity and quality of energy produced with the machine operating as a generator and its start, torque, and performance working as a motor. In conclusion, the modular skewed magnet is an option for electrical machines, for the generation of a reasonable quality, in the context of decentralized generation and a motor with high torque and low energetic consumption.

Chemical properties of different peats depending on origin and analytical method

The chemical properties of 12 different peats have been analyzed by methods from VDLUFA (German Association of Agricultural Analysis and Research Institutes) and EN (European Committee for Standardization, Technical Committee 223: Soil improvers and growing media). The analyses of pH (CaCl 2), contents of salts (H 2O), nutrients (CAT), and Na and Cl (H 2O) were carried out by VDLUFA methods, while those of pH (H 2O), EC (H 2O), nutrients (CAT), Na (CAT and H 2O) and Cl (H 2O) according to EN. Ten milled or sod white peats and two dredged frozen black peats of different degrees of decomposition were used. All of them contained high amounts of Mg, while black peats were additionally high in N, Fe and Zn. The pH-values were about the same for all peats. N- and Mn-contents depended most on peat origin. Analytical values of both CAT-methods were in the same range. Extraction with H 2O (EN) as compared to CAT (EN) resulted in considerably lower values.