Comparison of capillary gas chromatographic method and automated spectrophotofluorometric methods for measuring content uniformity of conjugated oestrogens in pharmaceutical preparations

To measure the content uniformity of conjugated cestrogens tablets, the USP XXII monograph specifies a capillary gas chromatographic method. This involves separation of the trimethylsilyl derivatives of the various oestrogens found in a typical conjugated oestrogens tablet using a fused-silica 0V 225 bonded phase column. Hydrogen is used as the carrier gas with FID detection. A more rapid spectrophotofluorometric method of analysis has been developed in which the oestrogens are extracted from the dosage form into water, then transferred into organic solvent as the dicyclohexylamine complex. Fluorescence is developed by heating the solution of the complex in the presence of 70% sulphuric acid. The chemistry and detection are carried out using a segmented-flow analyser.The spectrophotofluorometric method is preferred as a routine control for content uniformity because considerable time is saved during sample preparation and analysis compared to gas chromatography. Coefficients of variation show that both methods produce acceptable results. These results fall well within the USP XXII [1] monograph, limits and also well within the tighter limits imposed by the USP XXII, section 905.     

Toward a theory of robust compensation for systems with unknownparasitics

The problem of designing a robust compensator based on a plant model with order uncertainty is considered. The uncertainty is characterized mathematically as a class of generalized singular perturbations of the plant. The case of static compensation is examined. A necessary and sufficient condition is established under which actual closed-loop behavior is close to that predicted by the plant model under sufficiently small singular perturbations. The condition is shown to be generic     

POEMS: program for outliers elimination in multidimensional space

A Program for Outliers Elimination in Multidimensional Space (POEMS), which allows the user to eliminate outliers from training spaces as a prior step to any statistical study, is presented. Even though the program can be applied to any scientific field, the characteristics of POEMS makes it particularly suitable for 'series design' on Quantitative Structure-Activity Relationships studies.     

The Macintosh Programmer's Workshop

The authors discuss the Macintosh Programmer's Workshop (MPW), a Macintosh development environment that includes a comprehensive set of programming tools and handles several languages. It also combines the graphical interface common to all Macintosh applications, a command language similar to the Unix shell languages, and Smalltalk's immediate execution of commands in any window. They focus on the program-development environment rather than on the tools in that environment. They give the history of MPW, and describe its design goals. The bulk of the article is a discussion of MPW's design     

Liquid–liquid extraction of a recombinant protein with reverse micelles

Recombinant cytochrome b₅ was extracted into the reversed micelle phase of an anionic surfactant (AOT) in octane and back-extracted to a final aqueous phase. The extraction of the protein was controlled by an electrostatic mechanism, since it was dependent on the global charge of the protein. This was directly demonstrated by experiments with native and mutant cytochromes obtained by site directed mutagenesis. The back-extraction of cytochrome b₅ to a fresh aqueous phase was decreased by factors that reduced the size of the water pool of the organic phase, such as high salt concentrations (1–2 mol dm^?3 NaCl) and low temperatures (4°C), probably because of an increase in a favourable interaction of this protein with the surfactant at closer distances.     

A Macintosh Hypercard stack for calculation of thermodynamically-corrected buffer recipes

This paper describes a stack for the Apple Macintosh Hypercard environment that facilitates the calculation of a set of thermodynamically-corrected pH buffers. Presented in the familiar Macintosh mouse-based environment, the program allows comprehensive buffer design and gives the user full control of buffer species, temperature, ionic strength, pH and choice of counter-ion to maintain the ionic strength at a fixed value. Addition of new buffers to the stack is straightforward and the recipes that are generated, including the weights of the various components, can be displayed on the screen or saved to a disk file for subsequent printing.     

FSK heterodyne transmission experiments at 560 Mbit/s and 1 Gbit/s

Optical frequency-shift-keying (FSK) signals are obtained from directly modulated distributed feedback (DFB) semiconductor lasers. Experimental studies of the direct frequency modulation (FM) characteristics of the DFB lasers show a nonuniform FM response due to the competing effects of thermal modulation of the laser active region and carrier density modulation. Equalization of the signal current to the laser is employed to produce a flat FM response from 30 kHz to 1 GHz. Optical FSK transmission and heterodyne detection experiments at 560-Mbit/s and 1-Gbit/s are conducted at a wavelength of 1497 nm. Receiver sensitivities of -39 dBm at 560 Mbit/s and -37 dBm at 1 Gbit/s are obtained. Transmission through 100 km of single-mode fiber at 1 Gbit/s is achieved with no degradation in receiver sensitivity.