Use of micellar mobile phases for the chromatographic determination of clorazepate, diazepam, and diltiazem in pharmaceuticals.
An ODS-2 column, a micellar mobile phase of high elution strength containing 0.1M sodium dodecyl sulfate and 3% (v/v) butanol, and ultraviolet detection at 230 nm are used for the determination of either of two benzodiazepines (clorazepate and diazepam) and a benzothiazepine (diltiazem) in pharmaceuticals. The procedure is shown to be competitive against conventional chromatography with methanol-water mobile phases, especially for diltiazem. The composition of the micellar mobile phase is selected using a predictive strategy based on an accurate retention model and assisted by computer simulation. Calibration graphs are linear at least in the 2.5 to 20 microg/mL, 4 to 20 microg/mL, and 5 to 40 microg/mL ranges for clorazepate, diazepam, and diltiazem, respectively. The intra- and interday repeatabilities (%) are clorazepate (1.7, 5.2), diazepam (0.43, 3.7), and diltiazem (0.36, 3.1). Limits of detection are well below the concentrations of the drugs found in the commercial pharmaceutical preparations analyzed. The drug contents evaluated with the proposed procedure are compared with the declared contents given by the manufacturers. The achieved percentages of label claim are usually between 95 and 104%.
Gil-Agustí
M
M
Area de Química Analítica, Universitat Jaume I, Castelló, Spain.
Carda-Broch
S
S
García-Alvarez-Coque
M C
MC
Esteve-Romero
J
J
D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods*; D003009:Clorazepate Dipotassium / Q000032:analysis*; D003975:Diazepam / Q000032:analysis*; D004110:Diltiazem / Q000032:analysis*; D008823:Micelles; D004364:Pharmaceutical Preparations / Q000737:chemistry*; D013056:Spectrophotometry, Ultraviolet
D008823:Micelles; D004364:Pharmaceutical Preparations; D003009:Clorazepate Dipotassium; D004110:Diltiazem; D003975:Diazepam