INVESTIGADORES
GOICOECHEA Hector Casimiro
artículos
Título:
Simultaneous multiresponse optimization applied toepinastine determination in human serum by using capillary electrophoresis
Autor/es:
VERA CANDIOTI, LUCIANA; ALEJANDRO OLIVIERI,; GOICOECHEA, HÉCTOR C
Revista:
ANALYTICA CHIMICA ACTA
Editorial:
ELSEVIER
Referencias:
Año: 2007 p. 310 - 318
ISSN:
0003-2670
Resumen:
Experimental design and optimization techniques were implemented for the development
of a rapid and simple capillary zone electrophoresis method (CZE) for the determination of
epinastine hydrochloride in human serum. The effects of five factors were studied on the
resolution between the peaks for the target analyte (epinastine hydrochloride) and lidocaine
hydrochloride, used as internal standard, as well as on the analysis time. The factors were
the concentration and pH of the buffer, the injection time, the injection voltage and the
separation voltage. The separation was carried out by using an uncoated silica capillary
with 50m i.d. and total length 64.5cm (150m of path length) and UV detection (200 nm).
Multiple response simultaneous optimization by using the desirability function was used
to find experimental conditions where the system generates desirable results. The optimum
conditions were: sodium phosphate buffer solution, 16.0mmolL−1; pH 8.50; injection
voltage, 20.0 kV; injection time, 30 s; separation voltage, 26.7 kV.
The method was confirmed to be linear in the range of 2.012 ngmL−1. The injection
repeatability of the method was evaluated by six injections at three concentration levels,
while intra-assay precision was assessed by analysing a single concentration level,
yielding a CVs of ca. 1% for standard and 2% for serum samples. Accuracy was evaluated
by recovery assays and by comparing with an HPLC method, the results being acceptable
according to regulatory agencies. The rudgeness was evaluated by means of an experimental
PlackettBurman design, in which the accuracy was assessed when small changes were
set in the studied parameters. Clean-up of human serum samples was carried out by means
of a liquidliquid extraction procedure, which gave a high extraction yield for epinastine
hydrochloride (93.00%).