Analysis of spiramycin by capillary electrophoresis.
The development and validation of an analytical method for the determination of spiramycin I in the presence of its related substances by capillary electrophoresis is shown. The separation, performed in a phosphate buffer (80 mM, pH 7.5) containing 12 mM cetyltrimethylammonium bromide (CTAB) and 20 mM sodium cholate, with a 50 microm ID and 44 cm long fused-silica capillary (36 cm effective length), applying a voltage of 12 kV (l approximately 80 microA), at 25 degrees C, is achieved in 15 min. Good selectivity among spiramycin I and its related substances was obtained. The influence of the buffer pH, and of the CTAB and sodium cholate concentrations was investigated. The method robustness, examined by means of a full-fraction factorial design, shows that it can be used within the limits set for the three parameters that were investigated. The method is linear (r = 0.9992) and precise (day-to-day corrected peak area repeatability, n = 18, relative standard deviation = 1.3%). The limits of detection and quantitation are 7 pg (0.025%) and 22 pg (0.08%), respectively, relative to a 2 mg/mL solution.
González-Hernández
R
R
Laboratorio de Análisis, Centro de Química Farmacéutica, Playa, La Habana, Cuba.
Li
Y M
YM
Van Schepdael
A
A
Roets
E
E
Hoogmartens
J
J
D000617:Aminoglycosides; D000900:Anti-Bacterial Agents / Q000032:analysis*; D019075:Electrophoresis, Capillary / Q000379:methods*; D015394:Molecular Structure
D000617:Aminoglycosides; D000900:Anti-Bacterial Agents; C017186:demycarosylturimycin H