Development and validation of a stability indicating method for S-carboxymethyl-L-cysteine and related degradation products in oral syrup formulation.

A stability-indicating method for the determination of S-carboxymethyl-L-cysteine and related degradation impurities in Exputex® 250mg/5mL syrup was developed in anion-exchange liquid chromatography mode. A forced degradation study supported the method development to ensure stability indicating conditions. Aqueous solutions of the active pharmaceutical ingredient and syrup samples at different pH-values were stress-tested in different thermal, light exposure and headspace conditions.

Predictive elution window stretching and shifting as a generic search strategy for automated method development for liquid chromatography.

We report on the possibilities of a new method development (MD) algorithm that searches the chromatographic parameter space by systematically shifting and stretching the elution window over different parts of the time-axis. In this way, the search automatically focuses on the most promising areas of the solution space. Since only the retention properties of the first and last eluting compounds of the sample need to be (approximately) known, the algorithm can be directly applied to samples with unknown composition, and the proposed solutions are not sensitive to any modeling errors.

Monitoring compliance to therapy during addiction treatments by means of hair analysis for drugs and drug metabolites using capillary zone electrophoresis coupled to time-of-flight mass spectrometry.

Capillary electrophoresis coupled to time-of-flight mass spectrometry was used in the present work for the determination of therapeutic and abused drugs and their metabolites in the hair of subjects undergoing addiction treatments, in order to monitor their compliance to therapy. For this purpose a rapid, qualitative drug screening method was adopted based on capillary electrophoresis hyphenated with time-of-flight mass spectrometry, which had earlier been developed and validated for the forensic-toxicological analysis of hair, limitedly to illicit/abused drugs [1]. Sampling of hair was carried out in order to refer to a time window of about two months from the date of sampling (i.

Comparison of performance of high-performance liquid chromatography columns packed with superficially and fully porous 2.5 μm particles using kinetic plots.

A recently introduced 2.5 μm fully porous support (Kromasil Eternity) is compared with three different brands of superficially porous material (Kinetex, Halo and Poroshell 120) by means of the kinetic plot method using pharmaceutical compounds from GlaxoSmithKline as probe molecules. The kinetic plot method immediately shows the range of plate numbers wherein a support performs better than another.

Recent advances in the application of CE to forensic sciences: a update over years 2007-2009.

This article reviews and comments the applications of CE to forensic sciences covering the short period from 2007 until the first months of 2009, being the latest update of two previous review papers covering the years from 2001 to 2004 and from 2005 to 2007. The overview includes the most relevant examples of analytical applications of capillary electrophoretic and electrokinetic techniques in the following fields: (i) illicit and abused drugs, (ii) small ions of forensic interest (iii) proteins and peptides, (iv) forensic deoxyribonucleic acid, (v) dyes and inks. As many as 69 references are quoted.

Broad-spectrum toxicological analysis of hair based on capillary zone electrophoresis-time-of-flight mass spectrometry.

The coupling of capillary electrophoresis-electrospray ionization and time-of-flight mass spectrometry, combining efficiency and speed of separation with high mass accuracy and fast scanning capability, was for the first time applied to the determination of drugs of abuse (amphetamine, methamphetamine, MDA, MDMA, ephedrine, cocaine, morphine, codeine) and their metabolites in hair (6-MAM, benzoylecgonine). Experimental conditions were as follows. Separation: voltage 15 kV, uncoated fused-silica capillary (75 microm ID, 100 cm total length), running electrolyte 25 mM ammonium formate, pH 9.