RESUMO
The use of internal standards (ISs) improves the quantitative performance of CE. However, ISs chosen for use in CZE often cannot be used for micellar EKC (MEKC). Therefore 22 substances were investigated as potential ISs in MEKC. These substances were selected based upon a literature search. The substances were investigated using a method similar to the standard operating conditions for MEKC as recommended by S. Terabe. Furthermore, the migration time and the corrected migration time (k(S)) were determined for each substance to establish the migration position relative to other peaks in the electropherograms. A combination of eight substances, selected according to the obtained results (t(m) = 4 up to 12 min), was tested for practical benefit and applicability. The peak area precision was in the range of 0.8 and 1.2% (n = 60), and the peaks were well shaped for all the investigated substances. The selected substances covered a wide migration time window and therefore they can be regarded as suitable for future analysis at any required migration position.
Assuntos
Cromatografia Capilar Eletrocinética Micelar/normas , Preparações Farmacêuticas/normas , Padrões de Referência , Ácido 4-Aminobenzoico/isolamento & purificação , Acetaminofen/isolamento & purificação , Benzocaína/isolamento & purificação , Efedrina/isolamento & purificação , Naftóis/isolamento & purificação , Niacina/isolamento & purificação , Fenol/isolamento & purificação , Reprodutibilidade dos Testes , Trimetoprima/isolamento & purificaçãoRESUMO
An MEKC method was developed in order to separate a cold medicine formulation containing acetaminophen, ephedrine sulfate, doxylamine succinate, and dextromethorphan hydrobromide as active pharmaceutical ingredients. Because of their similar physical and chemical properties, it was a challenge to separate the basic compounds without sample pretreatment. In addition, the high content of alcohol and sucrose together with the variety of further excipients had to be considered. Thus, the complex matrix required several optimization steps. These included the search for the optimum pH and for a suitable sodium dodecyl sulfate concentration to avoid matrix-capillary wall interaction and to ensure precision. As a second developing step, an internal standard (benzocaine) was chosen to guarantee a high level of quantitative performance. An RSD% value of the peak areas between 1.0 and 2.0 was reached. The employed method development strategy can be generalized to similar separation approaches in the future.