HPLC determination of pyroglutamic acid as a degradation product in parenteral amino acid formulations

Summary The aminoacid glutamine in aqueous solution and in conditions of high temperature and long term storage is partly transformed into pyroglutamic acid which exhibits potential neurotoxic effects.Commercially available aminoacid mixtures supplemented with glutamine are heat-sterilized and some losses of glutamine and formation of pyroglutamic acid may occur.The aim of the work was to set up an easy and reliable HPLC method which allows the determination of pyroglutamic acid as a degradation product of glutamine. The column was a 5 m Hypersil ODS (100×4.6 mm) and the mobile phase 100% 0.007 M phosphate buffer pH 3.5.Stability studies in different conditions of temperature and time of storage were performed on aminoacid mixture available in the commerce.     

Determination of platinum and palladium in strongly acid solution by means of flow injection analysis

Microamounts of Pt(II/IV) (0.25–800 μg/ml) and Pd(II) (5–600 μg/ml) in> 0.5 M hydrochloric acid can readily be determined by means of a simple FIA method based on the selective reaction of tin(II)chloride with these metals. The FIA method has a high linear dynamic range, and is relatively free from interferences of many transition metals, with the exception of Au and Rh; small amounts of other PGMs can be tolerated. Determination of Pt on a hydrogenation catalyst by this method compares well with that found by flame atomic absorption spectroscopy. By monitoring at two or more wavelengths, Pt and Pd can be determined in mixtures by this means, to yield a simple, cost-effective FIA method for possible on-line determinations and quality control of, in particular, Pt containing acidic refinery and other process streams.     

Determination and statistical analysis of trace element and active constituent concentrations in the medicinal plant Eucalyptus camaldulensis Dehnh (E. rostratus Schlecht)

In the leaves of the medicinal plant Eucalyptus camaldulensis Dehnh (E. rostratus Schlecht) collected from different sampling areas of Greece the trace elements antimony, cesium, chromium, cobalt, iron, europium, rubidium, scandium, strontium, thorium and zinc were determined by Instrumental Neutron Activation Analysis. In the same samples, the essential oil was determined by steam distillation and the percent relative composition of the essential oil in 1,8-cineole, p-cymene, -pinene by gas liquid chromatography. Also the refractive index of the essential oil was determined by a refractometer. Statistical analysis included the calculation of the correlation coefficient. Multiple correlation and cluster analysis was applied to all analytical data. The results showed that the trace elements iron, chromium, cobalt and zinc are correlated with the variation of the concentration of essential oil in the examined plant. These four elements along with rubidium and essential oil content could be used for the separation of the samples into groups related to the sampling areas. Statistically significant correlation between active constituents and some trace elements and a linear negative correlation between 1,8-cineole and refractive index were found.     

Characterisation of chlorinated hydrocarbons in a third generation candidate fish reference material (Limanda limanda) prepared under cryogenic conditions

Summary This paper describes the cryogenic preparation of 50 individual specimens of dab (Limanda limanda) from the Baltic Sea to produce a homogeneous fish material. 950 subsamples (8 g each) are stored in the gaseous phase over liquid nitrogen. Five series of analyses were randomly selected out of store. The results show that the obtained precision of 8 to 9% could be used as an indication unit for the deviation of the mean values of CHC concentrations from true values. If the analytical variability is 5%, the maximum inhomogeneity in the subsamples is 3–4%. It may be concluded that the subsamples of the candidate fish reference material (RM) are homogeneous enough for analytical purposes. Thus ESB (German Environmental Specimen Bank) material prepared in accordance with the standard operating procedure (SOP) [1] are valuable and appropriate reference materials. The prepared fish RM is suitable for the analysis of chlorinated hydrocarbons in fat containing marine samples.     

Variable step size destabilizes the Störmer/leapfrog/verlet method

For fixed step-sizeh the Störmer method is stable for the standard test equationÿ= ² y,>0, if and only ifh<2. We show that for variable step sizeh _n there does not exist a (positive) limit onh which ensures stability. Nor can we guarantee stability if, in addition, we limit the step size ratioh _n/h _n–1.This work was supported in part by National Science Foundation Grant DMS 90 15533.     

The permutational power of a priority queue

A priority queue transforms an input permutation of some set of sizen into an output permutation. It is shown that the number of such pairs (, ) is (n + 1) ^n–1. Some related enumerative and algorithmic questions are also considered.Supported by the National Science and Engineering Research Council of Canada under Grant A4219.     

On the construction and calculation of optimal nonlifting critical airfoils

Numerical calculations are carried out in the hodograph plane to construct optimal critical airfoil shapes and the flow about them. These optimal airfoil shapes give the highest free-stream Mach numberM for a given thickness ratio and tail angle _t (nonlifting) for which the flow is nowhere supersonic. A relationship betweenM and for various _t is given. Analytical and numerical solutions to the same problem are found on the basis of transonic small-disturbance theory. These results provide a limiting case asM 1, 0 and agree well with the calculations of the full problem. Using a numerical method to calculate the flow about general (subsonic) airfoils, a comparison is made between the critical free-stream Mach numbers for some standard airfoil shapes and the optimal free stream Mach number of the corresponding and _t . A significant increase in the critical free-stream Mach number is found for the optimal airfoils.     

The classical ruin problem on a finite solvable group

For the classical ruin problem (a special case of a cyclic group), we use an explicit expression for the characteristic function of the time of first hitting an arbitrary subset of a finite solvable group by a random walk, from a fixed subset, to obtain a new proof of the well-known formula which allows one to estimate the characteristic function of the ruin probability (hitting the identity of a group) at theth- trial.Translated from Ukrainskii Matematicheskii Zhurnal, Vol. 45, No. 3, pp. 361–366, March, 1993.     

Path integral evaluation of the Eta function

In a three-dimensional model in which the gauge group does not commute with the Lorentz group, we demonstrate how the phase associated with the one-loop effective action (the function) can be computed by considering a quantum mechanical path integral.     

Optimization of reliability and longevity of cylindrical shells subject to corrosive wear

The problem of the optimal (with respect to the minimum average rate of weight loss in a structure) design of a smooth cylindrical shell loaded by an axial compressive force and under corrosive wear, the rate of which depends exponentially on the stresses, is solved. The problem is solved analytically using apparatus of the method of Lagrange multipliers.Translated from Matematicheskie Metody i Fiziko-mekhanicheskie Polya, No. 26, pp. 59–63, 1987.