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Research Paper |
Title |
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A validated UPLC method for the determination of processrelated
impurities in Antimigraine bulk drug |
Country |
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India |
Authors |
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N. Balaji, V. R. Sivaraman, Dr. P. Neeraja |
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10.9790/5736-0342028 |
Abstract: An UPLC method has been developed and subsequently validated for the determination of
antimigraine drug and its process-related impurities. Separation was achieved with Halo C18, 50x 4.6 mm,
2.7μm column and 1.36 g ofmonobasic potassium phosphate in 1000 mL of water with 2 mL of triethylamine at
pH 6.8 using H3PO4, acetonitrile and methanol in the ratio of 55 : 38 : 7 as eluent in isocratic mode. Flow rate
was set as 1 mL.min-1UV detection was performed at 225 nm. The method was validated with respect to
specificity, accuracy, precision, linearity, robustness, limit of quantification and limit of detection. The accuracy
of the method demonstrated at three levels in the range of 50-150% of the specification limit and the recovery of
impurities were found to be in range of 98 to 102%. The detection limits of the process related impurities
ranged between 0.16 and 0.24 μgmL-1. The described method is simple, rapid, linear, precise, accurate, robust
and stability indicating. The method is useful during process development and quality of bulk manufacturing.
Keywords: Ultra performance liquid chromatography (UPLC), Antimigrainedrugs, Validationand Process
related impurities.
[1] Cooper, J. D. H. ;, Muirhead, D. C. ; Taylor, J. E., Determination of Eletriptan in plasma and saliva using automated sequential trace
enrichment of dialyzate and high performance liquid chromatography, Journal of Pharmaceutical and Biomedical Analysis (1999),
21(4), 787-796.
[2] Zecevic, Mira; Jocic, Biljana; Agatonovic-Kustrin, Snezana; Zivanovic, Ljiljana, Validation of an HPLC method for the simultaneous
determination of eletriptan and UK 120.413, Journal of the Serbian Chemical Society (2006), 71(11), 1195-1205.
[3] Suneetha, D.; Rao, A. Lakshmana, RP-HPLC method for the estimation of eletriptan in pharmaceutical dosage forms, International
Journal of Chemical, Environmental and Pharmaceutical Research (2010), 1(2), 95-99.
[4] Kumar, A. Phani; Ganesh, V. R. L.; Prasad, K. Hari; Hariharakrishnan, V. S.; Dubey, P. K.; Rao, B. Venugopala , HPLC method for
the enantiomeric purity of eletriptan hydrobromide, Asian Journal of Chemistry (2011), 23(4), 1621-1624.
[5] El-Bagary, Ramzia I.; Mohammed, Nashwah G.; Nasr, Heba A, Two chromatographic methods for the determination of some
antimigraine drugs, Analytical Chemistry Insights (2012), 7, 13-21.
[6] KumaraSwamy, G.; Kumar, J. M. R.; Sheshagiri Rao, J. V. L. N., Development and validation of RP - HPLC method for the
estimation of Eletriptan hydrobromide in bulk and tablet dosage form, Journal of Pharmacy Research (2012), 5(1), 538-540.
[7] Sagirli, Olcay; Onal, Armagan; Sensoy, Demet, LC assay of eletriptan in tablets and in vitro dissolution studies, Chromatographia
(2008), 68(3/4), 269-273.
[8] Jocic, Biljana; Zecevic, Mira; Zivanovic, Ljiljana; Protic, Ana; Jadranin, Milka; Vajs, Vlatka, Study of forced degradation behavior
of Eletriptan hydrobromide by LC and LC-MS and development of stabilityindicating method, Journal of Pharmaceutical and
Biomedical Analysis (2009), 50(4), 622-629.
[9] Ponnuru, Venkata Suresh; Challa, B. R.; Nadendla, Ramarao, Quantitative analysis of eletriptan in human plasma by HPLC-MS/MS
and its application to pharmacokinetic study, Analytical and Bioanalytical Chemistry (2011), 401(8), 2539-2548.
[10] Speir, J. Paul; Perkins, George; Berg, Christian; Pullen, Frank, Fast, generic gradient high performance liquid chromatography
coupled to Fourier transform ion cyclotron resonance mass spectrometry for the accurate mass analysis of mixtures, Rapid
Communications in Mass Spectrometry (2000), 14(20), 1937-1942.