This review is in support of the development of selective, reproducible and validated capillary electrophoretis (CE) methods. Focusing on pharmaceutical and biological applications, the successful use of CE is demonstrated by more than 800 references, mainly from 1994 until 1998. Approximately 80 recent reviews have been catalogued. These articles sum up the existing strategies for method development in CE, especially in the search for generally accepted concepts, but also looking for new, promising reagents and ideas. General strategies for method development were derived not only with regard to selectivity and efficiency, but also with regard to precision, short analysis time, limit of detection, sample pretreatment requirements and validation. Standard buffer recipes, surfactants used in micellar electrokinetic capillary chromatography (MEKC), chiral selectors, useful buffer additives, polymeric separation media, electroosmotic flow (EOF) modifiers, dynamic and permanent coatings, actions to deal with complex matrices and aspects of validation are collected in 20 tables. Detailed schemes for the development of MEKC methods and chiral separations, for optimizing separation efficiency, means of troubleshooting, and other important information for key decisions during method development are given in 19 diagrams. Method development for peptide and protein separations, possibilities to influence the EOF and how to stabilize it, as well as indirect detection are considered in special sections.

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Pharmaceuticals in human plasma are determined on underivatized fused-silica capillaries by micellar electrokinetic capillary chromatography (MEKC) without sample pretreatment. Our best method to date uses as running buffer a sodium dodecyl sulfate (SDS) containing borate buffer (60 mM with 200 mM SDS) at pH 10. Between runs, proteins adsorbed to the capillary wall are removed by an acetonitrile and SDS-buffer rinsing regimen (50% v/v each). A day-to-day precision for relative peak areas of about 2% relative standard deviation (RSD; n > 40) has been reached. Different rinsing approaches are discussed (salts, enzyme-containing solutions, organic solvents, hydrofluoric acid). The separation system is tested in a concentration range between approximately 100 mg/L-10 mg/L. Correlations between the limit of quantitation, the limit of detection and the signal/noise are discussed. The applicability of the system is demonstrated for the pharmaceuticals acetaminophen, salicylic acid, sulfamethoxazole, tolbutamide, and trimethoprim.

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Capillary electrophoresis (CE) is often regarded as a separation technique of choice because of its high selectivity and its cost advantages compared to LC. RSD% of 0.5% have become standard for quality control assays. Using CE, sample pretreatment can often be significantly reduced, leading to notable savings of labor and reagent costs. Moreover, errors from sample pretreatment steps are avoided. A number of pharmaceuticals (e.g. acetaminophen, salicylic acid, sulfamethoxazole, theophylline, tolbutamide, and trimethoprim) have been determined in human plasma on underivatized fused silica capillaries by MEKC without sample pretreatment, the total analysis time being only 10 min. An sodium dodecyl sulfate‐containing borate buffer (60 mM with 200 mM SDS) at pH 10 has been used. Between runs, proteins adsorbed to the capillary wall are removed by a rinsing regimen consisting of SDS buffer and either acetonitrile (e.g. 50% v/v) or isopropanol (e.g. 10% v/v). Other rinsing approaches are discussed (salts, enzyme containing solutions, organic solvents, sodium hydroxide, hydrofluoric acid). The separation system is tested in a concentra‐tion range between 10 ng/mL and 100 μg/mL, the detection limit being about 5 ng/mL. The sensitivity has been substantially improved compared to preceding work using field‐amplified injection mechanisms and efficient computer algorithms that take advantage of multiwavelength detection. Correlations between the limit of quantitation (LOQ), the limit of detection (LOD) and the signal/noise ratio are discussed. A day‐to‐day precision for relative peak areas of 1 to 2% relsdv (n > 40) has been reached in the upper concentration range. Thus, not only drug monitoring but also pharmacokinetic investigations from blood plasma have become possible without further sample pretreatment.

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