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

Miranda TA, Silva PH, Pianetti GA, César IC - Malar. J. (2015)

Bottom Line: 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.No significant differences were observed between the chloroquine and primaquine contents obtained by UPLC and HPLC methods.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.

View Article: PubMed Central - PubMed

Affiliation: Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av Pres Antônio Carlos 6627, Belo Horizonte, 31270-901, MG, Brazil. isaccesar@bol.com.br.

ABSTRACT

Background: 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.

Methods: 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.

Results: 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.

Conclusions: 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.

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Calibration curves of (A) chloroquine and (B) primaquine obtained by HPLC and UPLC methods.
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Fig3: Calibration curves of (A) chloroquine and (B) primaquine obtained by HPLC and UPLC methods.

Mentions: Linear correlation was found between the peak areas and the concentrations of chloroquine and primaquine, in the assayed range, for both HPLC and UPLC methods, using the least squares method. A random pattern of the regression residues was found and no significant deviation of linearity was detected in the assayed range. The regression analysis curves are showed in Figure 3. The regression coefficient (r2) values obtained, higher to 0.99 to both compounds, attested the linearity of the methods.Figure 3


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

Miranda TA, Silva PH, Pianetti GA, César IC - Malar. J. (2015)

Calibration curves of (A) chloroquine and (B) primaquine obtained by HPLC and UPLC methods.
© Copyright Policy - open-access
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC4318193&req=5

Fig3: Calibration curves of (A) chloroquine and (B) primaquine obtained by HPLC and UPLC methods.
Mentions: Linear correlation was found between the peak areas and the concentrations of chloroquine and primaquine, in the assayed range, for both HPLC and UPLC methods, using the least squares method. A random pattern of the regression residues was found and no significant deviation of linearity was detected in the assayed range. The regression analysis curves are showed in Figure 3. The regression coefficient (r2) values obtained, higher to 0.99 to both compounds, attested the linearity of the methods.Figure 3

Bottom Line: 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.No significant differences were observed between the chloroquine and primaquine contents obtained by UPLC and HPLC methods.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.

View Article: PubMed Central - PubMed

Affiliation: Departamento de Produtos Farmacêuticos, Faculdade de Farmácia, Universidade Federal de Minas Gerais, Av Pres Antônio Carlos 6627, Belo Horizonte, 31270-901, MG, Brazil. isaccesar@bol.com.br.

ABSTRACT

Background: 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.

Methods: 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.

Results: 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.

Conclusions: 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.

Show MeSH
Related in: MedlinePlus