Przejdź do zawartości
Merck

Simultaneous quantitation of chloroquine and primaquine by UPLC-DAD and comparison with a HPLC-DAD method.

Malaria journal (2015-01-30)
Tiago A Miranda, Pedro H R Silva, Gerson A Pianetti, Isabela C César
ABSTRAKT

Chloroquine and primaquine are the first-line treatment recommended by World Health Organization for malaria caused by Plasmodium vivax. Since the problem of counterfeit or substandard anti-malarials is well established all over the world, the development of rapid and reliable methods for quality control analysis of these drugs is essential. Thus, the aim of this study was to develop and validate a novel UPLC-DAD method for simultaneously quantifying chloroquine and primaquine in tablet formulations. The UPLC separation was carried out using a Hypersil C18 column (50 × 2.1 mm id; 1.9 μm particle size) and a mobile phase composed of acetonitrile (A) and 0.1% aqueous triethylamine, pH 3.0 adjusted with phosphoric acid (B), at a flow rate 0.6 mL/min. Gradient elution was employed. UV detection was performed at 260 nm. UPLC method was fully validated and the results were compared to a conventional HPLC-DAD method for the analysis of chloroquine and primaquine in tablet formulations. UPLC method was shown to be linear (r2 > 0.99), precise (CV < 2.0%), accurate (recovery rates from 98.11 to 99.83%), specific, and robust. No significant differences were observed between the chloroquine and primaquine contents obtained by UPLC and HPLC methods. However, UPLC method promoted faster analyses, better chromatographic performance and lower solvent consumption. The developed UPLC method was shown to be a rapid and suitable technique to quantify chloroquine and primaquine in pharmaceutical preparations and may be successfully employed for quality control analysis.

MATERIAŁY
Numer produktu
Marka
Opis produktu

Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Sigma-Aldrich
Phosphoric acid solution, suitable for NMR (reference standard), 85% in D2O (99.9 atom % D), NMR tube size 3 mm × 8 in.
Supelco
Methanol, analytical standard
Sigma-Aldrich
Methanol, Absolute - Acetone free
Supelco
Acetonitrile(Neat), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, ampule, ≥99.5% (GC)
Supelco
Triethylamine, analytical standard
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, for amino acid analysis, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, ≥99%
Sigma-Aldrich
Triethylamine, puriss. p.a., ≥99.5% (GC)
Supelco
Residual Solvent - Acetonitrile(solution in DMSO), Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Phosphoric acid solution, suitable for NMR (reference standard), 85% in D2O (99.9 atom % D), NMR tube size 5 mm × 8 in.
Sigma-Aldrich
Phosphoric acid solution, suitable for NMR (reference standard), 85% in D2O (99.9 atom % D), NMR tube size 4.2 mm × 8 in. , WGS-5BL Coaxial NMR tube
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Phosphoric acid solution, 85 wt. % in H2O, FCC, FG
Sigma-Aldrich
Methanol, suitable for NMR (reference standard)
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Triethylamine, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Phosphoric acid-16O4 solution, 70 wt. % in D2O, 99.9 atom % 16O
Sigma-Aldrich
Acetonitrile, anhydrous, 99.8%
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%