LCGC Europe-07-01-2007

Modern gas chromatography (GC) capillary columns are rugged and forgiving but some care should be taken when handling and using these high-efficiency columns. In this instalment of "Column Watch", the authors discuss the issues surrounding avoiding column breakage, stationary phase damage and column contamination. Prolonging the life of a column by keeping an oxygen-free system, providing a cleaner sample and not exceeding the upper temperature limit of the stationary phase are highlighted in this practical discussion.

An evaporative light scattering (ELS) detector is a powerful detection tool if the solutes are less volatile than the eluent. Three main processes occur successively: nebulization, evaporation of the liquid chromatographic (LC) effluent and measurement of the light scattering by the residual particles. This leads to a non-linear calibration curve such as, A= a.m b where A is the peak area,m the sample mass and b the response coefficient measured as the slope of Log A = b>Log m + Log a.

Molecularly imprinted polymers (MIPs) are synthetic polymeric materials that mimic immunosorbents. They are widely used as sorbents for solid-phase extraction (SPE). The most common way to synthesize them is bulk polymerization because of its simplicity and versatility. This produces a hard monolith that has to be ground and sieved to obtain particles in the desired size range. However, the partial loss of the materials as fine dusts; the irregular shape of the particles produced and their wide size distribution, have led to a search for different polymerization methods to offset the drawbacks of the bulk polymerization process.

EuroAnalysis has established itself as the central forum for discussion and presentation of activities for analytical chemistry in Europe.

See so much more with these new video glasses; Tune into your stress levels; A gadget that won't let you close your wallet!; Interaction using a new dimension; Personalize your identity tag

Column temperature plays an important role in controlling peak spacing (selectivity) in reversed-phase liquid chromatography (LC) separations. Temperature has long been known to affect retention time, and more recently, its use in adjusting selectivity has gained popularity (see reference 1 for a review of temperature selectivity). In preparation of a paper for the most recent Pittsburgh Conference, I had an opportunity to reexamine some data that compare temperature selectivity with other variables used to control selectivity in LC separation. This month's instalment of "LC Troubleshooting" examines temperature selectivity and its relationship to pH selectivity.

The acid-base constants of the most frequently used antianginals (diltiazem, nadolol, propranolol and verapamil) were determined using capillary zone electrophoresis (CZE). This method is based on measuring the electrophoretic mobility of the solute as a function of pH. The buffer employed was composed of borate-phosphate buffered across the pH range of 3.0–11.2. The acid-base constants were determined by performing linear and non-linear regression on the data obtained. The results were compared with those reported in literature and with those obtained by a spectrophotometric method. After comparison of the values, no significant differences were observed between the three acid-base constants.