Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets

We developed and validated a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to quantify the antimalarials artesunate (ARS) and mefloquine (MFQ) in fixed-dose tablets. The detection was performed by a triple-quadrupole mass spectrometer in multiple reaction monitoring (MRM) in positive ion mode via electrospray ionization. Chromatographic separation was achieved with an XBridge C18 column (50 × 2.1 mm, 5 μm), using isocratic elution (350 μL min-1) of water/acetonitrile/methanol (30:35:35, v/v/v) containing 0.1% formic acid. The method was validated according to the International Conference of Harmonization (ICH) guidelines. The calibration curves obtained for ARS (400 to 600 ng mL-1) and MFQ (800 to 1200 ng mL-1) showed good linearity (r2 > 0.99), precision (relative standard deviation (RSD): ARS < 2.0%; MFQ < 1.9%), and accuracy (recoveries: ARS, 102.4-103.4%; MFQ, 97.4-101.6%), and were stable for 24 h at 8 ºC. The method was successfully applied to commercial tablets, and recoveries of 98.7 ± 4.7% (ARS) and 105.6 ± 3.13% (MFQ). The method developed is a reliable alternative for public quality inspection control with the advantage of tandem mass specificity and speed.

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Main Authors: Marson,Breno M., Vilhena,Raquel O., Pontes,Flavia L. D., Piantavini,Mário S., Pontarolo,Roberto
Format: Digital revista
Language:English
Published: Sociedade Brasileira de Química 2017
Online Access:http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000400615
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spelling oai:scielo:S0103-505320170004006152017-03-06Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose TabletsMarson,Breno M.Vilhena,Raquel O.Pontes,Flavia L. D.Piantavini,Mário S.Pontarolo,Roberto antimalarial artesunate LC-MS/MS mefloquine validation We developed and validated a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to quantify the antimalarials artesunate (ARS) and mefloquine (MFQ) in fixed-dose tablets. The detection was performed by a triple-quadrupole mass spectrometer in multiple reaction monitoring (MRM) in positive ion mode via electrospray ionization. Chromatographic separation was achieved with an XBridge C18 column (50 × 2.1 mm, 5 μm), using isocratic elution (350 μL min-1) of water/acetonitrile/methanol (30:35:35, v/v/v) containing 0.1% formic acid. The method was validated according to the International Conference of Harmonization (ICH) guidelines. The calibration curves obtained for ARS (400 to 600 ng mL-1) and MFQ (800 to 1200 ng mL-1) showed good linearity (r2 > 0.99), precision (relative standard deviation (RSD): ARS < 2.0%; MFQ < 1.9%), and accuracy (recoveries: ARS, 102.4-103.4%; MFQ, 97.4-101.6%), and were stable for 24 h at 8 ºC. The method was successfully applied to commercial tablets, and recoveries of 98.7 ± 4.7% (ARS) and 105.6 ± 3.13% (MFQ). The method developed is a reliable alternative for public quality inspection control with the advantage of tandem mass specificity and speed.info:eu-repo/semantics/openAccessSociedade Brasileira de QuímicaJournal of the Brazilian Chemical Society v.28 n.4 20172017-04-01info:eu-repo/semantics/articletext/htmlhttp://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000400615en10.21577/0103-5053.20160206
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libraryname SciELO
language English
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author Marson,Breno M.
Vilhena,Raquel O.
Pontes,Flavia L. D.
Piantavini,Mário S.
Pontarolo,Roberto
spellingShingle Marson,Breno M.
Vilhena,Raquel O.
Pontes,Flavia L. D.
Piantavini,Mário S.
Pontarolo,Roberto
Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
author_facet Marson,Breno M.
Vilhena,Raquel O.
Pontes,Flavia L. D.
Piantavini,Mário S.
Pontarolo,Roberto
author_sort Marson,Breno M.
title Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
title_short Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
title_full Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
title_fullStr Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
title_full_unstemmed Simultaneous Determination of Antimalarial Agents by LC-MS/MS and Its Application to Evaluation of Fixed-Dose Tablets
title_sort simultaneous determination of antimalarial agents by lc-ms/ms and its application to evaluation of fixed-dose tablets
description We developed and validated a liquid chromatography tandem mass spectrometry (LC-MS/MS) method to quantify the antimalarials artesunate (ARS) and mefloquine (MFQ) in fixed-dose tablets. The detection was performed by a triple-quadrupole mass spectrometer in multiple reaction monitoring (MRM) in positive ion mode via electrospray ionization. Chromatographic separation was achieved with an XBridge C18 column (50 × 2.1 mm, 5 μm), using isocratic elution (350 μL min-1) of water/acetonitrile/methanol (30:35:35, v/v/v) containing 0.1% formic acid. The method was validated according to the International Conference of Harmonization (ICH) guidelines. The calibration curves obtained for ARS (400 to 600 ng mL-1) and MFQ (800 to 1200 ng mL-1) showed good linearity (r2 > 0.99), precision (relative standard deviation (RSD): ARS < 2.0%; MFQ < 1.9%), and accuracy (recoveries: ARS, 102.4-103.4%; MFQ, 97.4-101.6%), and were stable for 24 h at 8 ºC. The method was successfully applied to commercial tablets, and recoveries of 98.7 ± 4.7% (ARS) and 105.6 ± 3.13% (MFQ). The method developed is a reliable alternative for public quality inspection control with the advantage of tandem mass specificity and speed.
publisher Sociedade Brasileira de Química
publishDate 2017
url http://old.scielo.br/scielo.php?script=sci_arttext&pid=S0103-50532017000400615
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