UV-Derivative Spectrophotometric and Stability-Indicating High-Performance Liquid Chromatographic Methods for Determination of Simvastatin in Tablets

A stability-indicating high-performance liquid chromatographic (HPLC) and a second-order derivative spectrophotometric (UVDS) analytical methods were validated and compared for determination of simvastatin in tablets. The HPLC method was performed with isocratic elution using a C18 column and a mobile phase composed of methanol:acetonitrile:water (60:20:20, v/v/v) at a flow rate of 1.0 ml/min. The detection was made at 239 nm. In UVDS method, methanol and water were used in first dilution and distilled water was used in consecutive dilutions and as background. The second-order derivative signal measurement was taken at 255 nm. Analytical curves showed correlation coefficients > 0.999 for both methods. The quantitation limits (QL) were 2.41 mu g/ml for HPLC and 0.45 mu g/ml for UVDS, respectively. Intra and inter-day relative standard deviations were < 2.0 %. Statistical analysis with t- and F-tests are not exceeding their critical values demonstrating that there is no significant difference between the two methods at 95 % confidence level.

Isolation, functional, and partial biochemical characterization of galatrox, an acidic lectin from Bothrops atrox snake venom

Snake venom lectins have been studied in regard to their chemical structure and biological functions. However, little is known about lectins isolated from Bothrops atrox snake venom. We report here the isolation and partial functional and biochemical characterization of an acidic glycan-binding protein called galatrox from this venom. This lectin was purified by affinity chromatography using a lactosyl-sepharose column, and its homogeneity and molecular mass were evaluated by high-performance liquid chromatography, sodium dodecyl sulfate-polyacrylamide gel electrophoresis, and matrix-assisted laser desorption/ionization-time-of-flight mass spectrometry. The purified galatrox was homogeneous and characterized as an acidic protein (pI 5.2) with a monomeric and dimeric molecular mass of 16.2 and 32.5 kDa, respectively. Alignment of N-terminal and internal amino acid sequences of galatrox indicated that this protein exhibits high homology to other C-type snake venom lectins. Galatrox showed optimal hemagglutinating activity at a concentration of 100 mu g/ml and this effect was drastically inhibited by lactose, ethylenediaminetetraacetic acid, and heating, which confirmed galatrox`s lectin activity. While galatrox failed to induce the same level of paw edema or mast cell degranulation as B. atrox crude venom, galatrox did alter cellular viability, which suggested that galatrox might contribute to venom toxicity by directly inducing cell death.

Effect of process variables on fluiddynamics and adhesion efficiency during spouted bed coating of hard gelatine capsules

This article presents an evaluation of the effects of the spouted bed design and operating conditions on system fluiddynamics and process performance during enteric coating of hard gelatine capsules. The design parameters studied were the column diameter (150 mm and 200 mm), the included angle of the conical base, gamma (60 degrees or 40 degrees) and the presence or absence of a Venturi inserted before the inlet air orifice. The process variables studied were the ratio between the feed flow rate of the coating suspension to the spouting gas flow rate (W(s)/W(g)), the mass of capsules loaded to the equipment (M(0)), and the ratio between the Spouting gas flow rate to the gas flow rate at minimum spouting condition (Q/Q(ms)). The response variables were the rate of increase of the capsules mass (K(1)), and the adhesion efficiency (eta). The linear regression equation for the dependent variable K, in terms of the independent variables adequately described the process with an r(2) value of 0.872. Analysis of variance (ANOVA) revealed that increasing of W(s)/W(g), Q/Q(ms) and gamma significantly increased the adhesion efficiency. Adhesion efficiencies higher than 90% were achieved by selecting precise coating conditions, indicating the feasibility of the process for coating of hard gelatine capsules. (C) 2008 Elsevier B.V. All rights reserved.

Pre and post-natal exposure to ambient level of air pollution impairs memory of rats: the role of oxidative stress

The aims of this study were to evaluate whether air pollution during pre-natal and post-natal phases change habituation and short-term discriminative memories and if oxidants are involved in this process. As secondary objectives, it was to evaluate if the change of filtered to nonfiltered environment could protect the cortex of rats against oxidative stress as well as to modify the behavior of these animals. Wistar, male rats were divided into four groups (n = 12/group): pre and post-natal exposure until adulthood to filtered air (FA); pre-natal period to nonfiltered air (NFA-FA); until (21st post-natal day) and post-natal to filtered air until adulthood (PND21); prenatal to filtered air until PND21 and post-natal to nonfiltered air until adulthood (FA-NFA); pre and post-natal to nonfiltered air (NFA). After 150 days of air pollution exposure, animals were tested in the spontaneous object recognition test to evaluate short-term discriminative and habituation memories. Rats were euthanized; blood was collected for metal determination; cortex dissected for oxidative stress evaluation. There was a significant increase in malondialdehyde (MDA) levels in the NFA group when compared to other groups (FA: 1.730 +/- 0.217; NFA-FA: 1.101 +/- 0.217; FA-NFA: 1.014 +/- 0.300; NFA: 5.978 +/- 1.920 nmol MDA/mg total proteins; p = 0.007). NFA group presented a significant decrease in short-term discriminative (FA: 0.603 +/- 0.106; NFA-FA: 0.669 +/- 0.0666; FA-NFA: 0.374 +/- 0.178; NFA: -0.00631 +/- 0.106 sec; p = 0.006) and an improvement in habituation memories when compared to other groups. Therefore, exposure to air pollution during both those periods impairs short-term discriminative memory and cortical oxidative stress may mediate this process.

Development of the student placement evaluation form: A tool for assessing student fieldwork performance

Evaluation of students undertaking fieldwork education placements is a critical process in the health professions. As training programs and practice evolve, systems for assessing students need to be reviewed and updated constantly. In 1995, staff of the occupational therapy training program at the University of Queensland, Australia decided to develop a new tool for assessing student fieldwork performance. Using an action research methodology, a team developed the Student Placement Evaluation Form, a flexible and comprehensive criterion-referenced evaluation tool. The present paper examines action research as an appropriate methodology for considering real-life organisational problems in a systematic and participatory manner. The action research cycles undertaken, including preliminary information gathering, tool development, trial stages and current use of the tool, are detailed in the report. Current and future development of the tool is also described.

Internal staircase, Carpenter Hall house, Wilston, Brisbane

As seen from lower level of house.

Formal performance appraisal interviews: Can they really be objective, and are they useful anyway?

This paper reports on a qualitative field study conducted in Australia which examined what is occurring in formal performance appraisal interviews in relation to their objectivity and resultant outcomes. Supervisors and subordinates who had recently been involved in performance appraisals were interviewed about their experiences of the process. Perceptions of the utility of, and satisfaction with the interview process were examined. Further, the effect of the relationship between the participants on objectivity was investigated. Results indicated that formal appraisal interviews were not perceived to be of great utility, and that the relationship of the participants influenced the interview.

Spectral properties of the tandem Jackson network, seen as a quasi-birth-and-death process

Quasi-birth-and-death (QBD) processes with infinite “phase spaces” can exhibit unusual and interesting behavior. One of the simplest examples of such a process is the two-node tandem Jackson network, with the “phase” giving the state of the first queue and the “level” giving the state of the second queue. In this paper, we undertake an extensive analysis of the properties of this QBD. In particular, we investigate the spectral properties of Neuts’s R-matrix and show that the decay rate of the stationary distribution of the “level” process is not always equal to the convergence norm of R. In fact, we show that we can obtain any decay rate from a certain range by controlling only the transition structure at level zero, which is independent of R. We also consider the sequence of tandem queues that is constructed by restricting the waiting room of the first queue to some finite capacity, and then allowing this capacity to increase to infinity. We show that the decay rates for the finite truncations converge to a value, which is not necessarily the decay rate in the infinite waiting room case. Finally, we show that the probability that the process hits level n before level 0 given that it starts in level 1 decays at a rate which is not necessarily the same as the decay rate for the stationary distribution.

Modeling control objectives for business process compliance

Business process design is primarily driven by process improvement objectives. However, the role of control objectives stemming from regulations and standards is becoming increasingly important for businesses in light of recent events that led to some of the largest scandals in corporate history. As organizations strive to meet compliance agendas, there is an evident need to provide systematic approaches that assist in the understanding of the interplay between (often conflicting) business and control objectives during business process design. In this paper, our objective is twofold. We will firstly present a research agenda in the space of business process compliance, identifying major technical and organizational challenges. We then tackle a part of the overall problem space, which deals with the effective modeling of control objectives and subsequently their propagation onto business process models. Control objective modeling is proposed through a specialized modal logic based on normative systems theory, and the visualization of control objectives on business process models is achieved procedurally. The proposed approach is demonstrated in the context of a purchase-to-pay scenario.

Solid-phase extraction method with high-performance liquid chromatography and electrochemical detection for the quantitative analysis of oxycodone in human plasma

A sensitive and reproducible solid-phase extraction (SPE) method for the quantification of oxycodone in human plasma was developed. Varian Certify SPE cartridges containing both C-8 and benzoic acid functional groups were the most suitable for the extraction of oxycodone and codeine (internal standard), with consistently high (greater than or equal to 80%) and reproducible recoveries. The elution mobile phase consisted of 1.2 ml of butyl chloride-isopropanol (80:20, v/v) containing 2% ammonia. The quantification limit for oxycodone was 5.3 pmol on-column. Within-day and inter-day coefficients of variation were 1.2% and 6.8% respectively for 284 nM oxycodone and 9.5% and 6.2% respectively for 28.4 nM oxycodone using 0.5-ml plasma aliquots. (C) 1998 Elsevier Science BN. All rights reserved.

The relationship between plasma lactate parameters, W-peak and 1-h cycling performance in women

Purpose: The relationship between six descriptors of lactate increase, peak (V) over dot O-2,W-peak, and 1-h cycling performance were compared in 24 trained, female cyclists (peak (V) over dot O-2 = 48.11 +/- 6.32 mL . kg(-1) . min(-1)). Methods: The six descriptors of lactate increase were: 1) lactate threshold (LT; the power output at which plasma lactate concentration begins to increase above the resting level during an incremental exercise test), 2) LT1 (the power output at which plasma lactate increases by 1 mM or more), 3) LTD (the lactate threshold calculated by the D-max method), 4) LTMOD (the lactate threshold calculated by a modified D-max method), 5) L4 (the power output at which plasma lactate reaches a concentration of 4 mmol-L-1), and 6) LTLOG (the power output at which plasma lactate concentration begins to increase when the log([La-]) is plotted against the log (power output)). Subjects first completed a peak (V) over dot O-2 test on a cycle ergometer. Finger-tip capillary blood was sampled within 30 s of the end of each 3-min stage for analysis of plasma lactate. Endurance performance was assessed 7 d later using a 1-h cycle test (OHT) in which subjects were directed to achieve the highest possible average power output. Results: The mean power output (W) for the OHT (+/- SD) was 183.01 +/- 18.88, and for each lactate variable was: LT (138.54 +/- 46.61), LT1 (179.17 +/- 27.25), LTLOG (143.97 +/- 45.74), L4 (198.09 +/- 33.84), LTD (178.79 +/- 24.07), LTMOD (212.28 +/- 31.75). Average power output during the OHT was more strongly correlated with all plasma lactate parameters (0.61 < r < 0.84) and W-peak (r = 0.81) than with peak (V) over dot O-2 (r = 0.55). The six lactate parameters were strongly correlated with each other (0.54 < r < 0.91) and of the six lactate parameters, LTD correlated best with endurance performance (r = 0.84). Conclusions: It was concluded that plasma lactate parameters and W-peak provide better indices of endurance performance than peak (V) over dot O-2 and that, of the six descriptors of lactate increase measured in this study, LTD is most strongly related to 1-h cycling performance in trained, female cyclists.

Multiphoton ac Stark effect in a bichromatically driven two-level atom

We study the interaction of a two-level atom with two lasers of different frequencies and amplitudes: a strong laser of Rabi frequency 2 Ohm(1) on resonance with the atomic transition, and a weaker laser detuned by subharmonics (2 Ohm(1)/n) of the Rabi frequency of the first. We find that under these conditions the second laser couples the dressed states created by the first in an n-photon process, resulting in doubly dressed states and in a ''multiphoton ac Stark'' effect. We calculate the eigenstates of the doubly dressed atom and their energies, and illustrate the role of this multiphoton ac Stark effect in its fluorescence, absorption, and Autler-Townes spectra. [S1050-2947(98)07607-0].

Two-level atom in a squeezed vacuum with finite bandwidth

The resonance fluorescence of a two-level atom driven by a coherent laser field and damped by a finite bandwidth squeezed vacuum is analysed. We extend the Yeoman and Barnett technique to a non-zero detuning of the driving field from the atomic resonance and discuss the role of squeezing bandwidth and the detuning in the level shifts, widths and intensities of the spectral lines. The approach is valid for arbitrary values of the Rabi frequency and detuning but for the squeezing bandwidths larger than the natural linewidth in order to satisfy the Markoff approximation. The narrowing of the spectral lines is interpreted in terms of the quadrature-noise spectrum. We find that, depending on the Rabi frequency, detuning and the squeezing phase, different factors contribute to the line narrowing. For a strong resonant driving field there is no squeezing in the emitted field and the fluorescence spectrum exactly reveals the noise spectrum. In this case the narrowing of the spectral lines arises from the noise reduction in the input squeezed vacuum. For a weak or detuned driving field the fluorescence exhibits a large squeezing and, as a consequence, the spectral lines have narrowed linewidths. Moreover, the fluorescence spectrum can be asymmetric about the central frequency despite the symmetrical distribution of the noise. The asymmetry arises from the absorption of photons by the squeezed vacuum which reduces the spontaneous emission. For an appropriate choice of the detuning some of the spectral lines can vanish despite that there is no population trapping. Again this process can be interpreted as arising from the absorption of photons by the squeezed vacuum. When the absorption is large it may compensate the spontaneous emission resulting in the vanishing of the fluorescence lines.

Determination of pindolol enantiomers in human plasma and urine by simple liquid-liquid extraction and high-performance liquid chromatography

A simple method for the measurement of pindolol enantiomers by HPLC is presented. Alkalinized serum or urine is extracted with ethyl acetate and the residue remaining after evaporation of the organic layer is then derivatised with (S)-(-)-alpha-methylbenzyl isocyanate. The diastereoisomers of derivatised pindolol and metoprolol (internal standard) are separated by high-performance liquid chromatography (HPLC) using a C-18 silica column and detected using fluorescence (excitation lambda: 215 nm, emission lambda: 320 nm). The assay displays reproducible linearity for pindolol enantiomers with a correlation coefficient of r(2) greater than or equal to 0.998 over the concentration range 8-100 ng ml(-1) for plasma and 0.1-2.5 mu g ml(-1) for urine. The coefficient of variation for accuracy and precision of the quality control samples for both plasma and urine are consistently

Coupling of a Jahn-Teller pseudorotation with a hindered internal rotation in an isolated molecule: 9-hydroxytriptycene

The irregular vibronic structure in the S-1<--S-0 resonant two-photon ionization (R2PI) spectrum of supersonically cooled triptycene is a result of a classic Exe Jahn-Teller effect [A. Furlan et al., J. Chem. Phys. 96, 7306 (1992)]. This is well characterized and can be used as an effective probe of intramolecular perturbations. Here we examine the S-1<--S-0 R2PI spectrum of 9-hydroxytriptycene and the fluorescence from various excited state vibronic levels. In this system the pseudorotation of the Jahn-Teller vibration is strongly coupled to the torsional motion of the bridgehead hydroxy group. This torsional motion results in a tunneling splitting in both the ground and excited states. The population of the upper level in the ground electronic state results in additional vibronic transitions becoming symmetry allowed in the R2PI spectrum that are forbidden in the bare triptycene molecule. The assignment of the R2PI and fluorescence spectra allows the potential energy surfaces of these vibrational modes to be accurately quantified. The full C-3v vibronic point group must be used to interpret the spectra. The time scale of the internal rotation of the-OH group and the butterfly flapping of the Jahn-Teller pseudorotation are of similar magnitude. The tunneling between the nine minima on the three dimensional potential energy surface is such that the Jahn-Teller pseudorotation occurs in concert with the-OH internal rotation. The Berry phase that is acquired during this motion is discussed. The simple physical picture emerges of the angle between two of the three benzene moieties opening in three equivalent ways in the S-1 electronic state. This geometry follows the position of the hydroxy group, which preferentially orients itself to point between these two rings. (C) 1998 American Institute of Physics. [S0021-9606(98)02348-4].