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Validation of an HPLC method for determination of aripiprazole and its impurities in pharmaceuticals

Djordjević Filijović N., Pavlović A., Nikolić K., Agbaba D.

Acta Chromatographica

2014

Vol. 26, no. 1

13--28

Aripiprazole is a novel atypical antipsychotic drug used in the treatment of schizophrenia. The sensitive and reproducible ion pair RPLC method was developed and validated for determination of aripiprazole and its nine impurities, which are significantly different in polarity. The separation was performed on Phenomenex Luna® C18 column (5.0 μm particle size, 250 × 4.6 mm id) using a gradient mobile phase A (phosphate buffer pH 3.0) and mobile phase B (acetonitrile) at the working temperature of 25°C. The buffer was 1.11 g KH2PO4 with 1.2 g sodium pentanesulfonate/L of the solution, adjusted to pH 3.0 with orthophosphoric acid. The flow rate was 1.0 mL/min. The detection was carried out at 215 nm using a diode array detector. The developed method was validated according to the International Conference on Harmonization (ICH) guidelines for specificity, limit of detection, limit of quantification, linearity, precision and robustness. The proposed method is convenient and reliable for the purity control in both raw materials and dosage forms.

Analysis of α -lipoic acid in drug formulations and dietary supplement preparations

Ravanić N, Filipić S., Nikolić K, Popović G, Vovk I, Simonovska B, Agbaba D

Acta Chromatographica

2009

Vol. 21, no. 3

433--441

A simple and reliable TLC method for analysis of -lipoic acid (LA) with post-chromatographic derivatisation with palladium(II) chloride immersion reagent has been developed and evaluated. Separation of LA was performed on 20 cm × 10 cm RPTLC plates with 2-propanol-methanol-acetone-water-acetic acid 6:4:2:8:0.2 ( v/v ) as mobile phase. Yellow complexes formed in situ were scanned at 375 nm. The migration distance of LA was 43.0 mm. The relationship between peak area and amount of LA applied was evaluated by use of linear (1.0–3.0 µg per band) and second-degree polynomial (0.5–5.0 µg per band) regression functions. The correlation coefficient ( r = 0.999), the limit of quantification (0.39 µg per band), recovery (98.5–105.2%), and precision (1.8–2.9%) obtained by use of the procedure were satisfactory. The method was used for analysis of LA in several drug formulations and selected dietary supplement preparations. The LA content was 99.5–101.0% in the drug formulations, 98.8–99.5% in three of five dietary supplements tested, and 48.0–185.0% in two other dietary supplements.