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Farmasötik Formülasyonlarda Roflumilast’ın Türev Spektrofotometrik Yöntem ile Tayini

Year 2016, Issue: 1, 27 - 49, 01.01.2016

Abstract

Bu çalışmada, farmasötik formülasyonlardaki roflumilastın tayini için basit, hızlı, güvenilir ve tamamen valide edilmiş birinci derece UV spektrofotometrik yöntem geliştirilmiştir. Analiz koşullarını optimize etmek için çözücü tipi, türev derecesi, dalga boyu aralığı ve N değeri test edilmiştir. İlacın kantitatif tayini 190 -350 nm dalga boyu aralığında 220 nm N = 4 ’de birinci türev değerleri kullanılarak yapılmıştır. Geliştirilen yöntem, kararlılık, doğrusallık, duyarlılık, özgünlük, kesinlik, doğruluk, sağlamlık ve tutarlılık açısından valide edilmiştir. Önerilen yöntemin doğrusal olduğu kalibrasyon aralığı 0.75 - 35.00 μg mL-1 ve alt tayin sınırı 0.08 μg mL−1’dir. Geliştirilen ve valide edilen yöntem, farmasötik formulasyonlarındaki roflumilastın tayini için direkt olarak uygulanmıştır. Analiz koşullarında ve seçilen dalga boyunda tablet yardımcı maddelerinden gelen bir girişim bulunmamıştır. Geliştirilen yöntemden elde edilen veriler, literatürdeki yüksek basınçlı sıvı kromatografisi yönteminden elde edilen veriler ile karşılaştırılmış ve iki yöntem arasında istatistiksel olarak anlamlı fark bulunmamıştır. Geliştirilmiş yöntemin duyarlı, doğru, kesin, seçici, sağlam ve tutarlı olduğu sonucuna varılmıştır.

References

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  • 13. Fang Tan: Development and validation of stability-indicating HPLC method for roflumilast and related substances. Advanced Materials Research (Durnten-Zurich, Switzerland) 2013, 781-784.
  • 14. Zheng Xi-zi, Guangpu S: Assay of roflumilast and the determination of its related substances by HPLC. Guangpu Shiyanshi 2013, 30 (6): 3122-3126.
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  • 16. Shah A.D, Patel C.N: Implementation of QbD approach to the RP-HPLC method development and validation of roflumilast in bulk and tablet dosage form: an application in degradation study. World Journal of Pharmacy and Pharmaceutical Sciences 2014, 3(6): 2281-2307.
  • 17. Satheeshmanikandan R.S Thappali, Kanthikiran V.S Varanasi, Sridhar V, Swaroop Kumar V.S. Vakkalanka, Mukkanti K: Simultaneous quantitation of IC87114, roflumilast and its active metabolite roflumilast N-oxide in plasma by LC-MS/MS: application for a pharmacokinetic study. Journal of Mass Spectrometry 2012, 47 (12): 1612-1619.
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  • 21. Ladani J.J, Bhimani R.D, Vyas K.B, Nimavat K.S: Method development and validation of roflumilast in tablet dosage form by UV spectrophotometry. Journal of Atoms and Molecules 2012, 2 (5): 369-374.
  • 22. Patel K.R, Desai D.G, Zanwar A, Sen A.K, Seth A.K: Development and validation of UV spectroscopy method for estimation of roflumilast in bulk and tablet dosage form. Pharma Science Monitor 2013, 4 (3): 274-280.
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  • 29. Ermer J, Ploss H.J. Validation in pharmaceutical analysis, part II: central importance of precision to establish acceptance criteria and for verifying and improving the quality of analytical data. Journal of Pharmaceutical and Biomedical Analysis, 2005, 37: 859-870.
  • 30. Vander Heyden Y, Nijhuis A, Smeyers-Vebreke J, Vandeginste B.G.M, Massart D.L: Guidance for robustness/ruggedness tests in method validation. Journal of Pharmaceutical and Biomedical Analysis ,2001, 24: 723-753.
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Determination of Roflumilast in Pharmaceutical Formulations by Derivative Spectrophotometric Method

Year 2016, Issue: 1, 27 - 49, 01.01.2016

Abstract

In this study, a simple, rapid, reliable and fully validated first order derivative UV spectrophotometric method was developed for determination of roflumilast in pharmaceutical formulations. The type of solvent, the degree of derivation, range of wavelength and N value were tested in order to optimize the analysis conditions. The quantitative determination of the drug was carried out using the first - derivative values measured at 220 nm N = 4 in the wavelength range of 190 - 350 nm. The developed method was validated with respect to stability, linearity, sensitivity, specificity, precision, accuracy, robustness and ruggedness. The linear calibration range was found to be 0.75 - 35.00 µg mL-1 and limit of quantitation was 0.08 μg mL−1 for the proposed method. The developed and validated method was directly applied for the determination of roflumilast in its pharmaceutical dosage forms. No interference was found from tablet excipients at the selected wavelength and analysis conditions. The results obtained from the developed method were compared with those obtained by the high performance liquid chromatographic method in the literature and no significant difference was found statistically between two methods. It was concluded that the developed method was sensitive, accurate, precise, selective, robust and rugged.

References

  • 1. Antoniu S. A.: New therapeutic options in the management of COPD - focus on roflumilast. International Journal of Chronic Obstructive Pulmonary Disease 2011, 6: 147-155.
  • 2. Schudt AC, Gantner F, Tenor H, Hatzelmann A: Therapeutic potential of selective PDE inhibitors in asthma. Pulmonary Pharmacology and Therapeutics 1999, 12(2): 123-129.
  • 3. Essayan D. M.: Cyclic nucleotide phosphodiesterase (PDE) inhibitors and immunomodulation. Biochemical Pharmacology 1999, 57: 965-973.
  • 4. Hatzelmann A, Schudt C: Anti-inflammatory and immunomodulatory potential of the novel PDE4 inhibitor roflumilast in vitro. Journal of Pharmacology and Experimental Therapeutics 2001, 297: 267-279.
  • 5. Boswell-Smith V, Spina D: PDE4 inhibitors as potential therapeutic agents in the treatment of COPD-focus on roflumilast. International Journal of Chronic Obstructive Pulmonary Disease 2007, 2 (2): 121-129.
  • 6. Field, SK: Roflumilast: an oral, once-daily selective PDE-4 inhibitor for the management of COPD and asthma. Expert Opinion on Investigational Drugs 2008, 17 (5): 811-818.
  • 7. Frankel SK, Cool CD, Lynch DA, et al.: Idiopathic pleuroparenchymal fibroelastosis: Description of a novel clinicopathologic entity. Chest 2004, 126: 2007-2013.
  • 8. Yu T, Fain K, Boyd C.M, Singh S, Weiss C.O, Li TJ, Varadhan R, Puhan M.A: Benefits and harms of roflumilast in moderate to severe COPD. Thorax 2014, 69 (7): 616-622.
  • 9. Barhate, V.D, Deosthalee Priya: Rapid liquid chromatographic method for the determination of roflumilast in the presence of degradation products. From Indian Journal of Pharmaceutical Sciences 2010, 72 (3): 401-404.
  • 10. Barhate V.D, Deosthalee P.C: Validation of rapid liquid chromatographic method for the determination of roflumilast. Journal of Chemical and Pharmaceutical Research 2011, 3 (2): 770-775.
  • 11. Ladani J.J, Bhimani R.D, Vyas K.B, Nimavat K.S: Analytical method development and validation of RP-HPLC for estimation of roflumilast in bulk drug and tablet dosage form. International Journal for Pharmaceutical Research Scholars 2012, 1 (3): 28-32.
  • 12. Lakshmi B, Reddy T: RP-HPLC method for the quantification of roflumilast in formulations. South Pacific Journal of Technology and Science (SPJTS) 2013, 1 (1): 015-023.
  • 13. Fang Tan: Development and validation of stability-indicating HPLC method for roflumilast and related substances. Advanced Materials Research (Durnten-Zurich, Switzerland) 2013, 781-784.
  • 14. Zheng Xi-zi, Guangpu S: Assay of roflumilast and the determination of its related substances by HPLC. Guangpu Shiyanshi 2013, 30 (6): 3122-3126.
  • 15. Yan W, Chen Y.M, Ni C.L, Zheng X: Identification and quantitative analysis of related substances in roflumilast. Chinese Journal of Pharmaceutical Analysis 2013, 33 (10): 1726-1730.
  • 16. Shah A.D, Patel C.N: Implementation of QbD approach to the RP-HPLC method development and validation of roflumilast in bulk and tablet dosage form: an application in degradation study. World Journal of Pharmacy and Pharmaceutical Sciences 2014, 3(6): 2281-2307.
  • 17. Satheeshmanikandan R.S Thappali, Kanthikiran V.S Varanasi, Sridhar V, Swaroop Kumar V.S. Vakkalanka, Mukkanti K: Simultaneous quantitation of IC87114, roflumilast and its active metabolite roflumilast N-oxide in plasma by LC-MS/MS: application for a pharmacokinetic study. Journal of Mass Spectrometry 2012, 47 (12): 1612-1619.
  • 18. Knebel N. G, Herzog R, Reutter Felix, Zech Karl: Sensitive quantification of roflumilast and roflumilast N-oxide in human plasma by LC-MS/MS employing parallel chromatography and electrospray ionisation. Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences 2012, 893-894: 82-91.
  • 19. Thevis M, Krug O, Schaenzer Wilhelm: Monitoring phosphodiesterase-4 inhibitors using liquid chromatography/(tandem) mass spectrometry in sports drug testing. Rapid Communications in Mass Spectrometry 2013, 27 (9): 993-1004.
  • 20. Qiu X, Wang Ai-di: Determination of residual solvents in roflumilast by headspace gas chromatography. Yingyong Huagong 2013, 42 (8): 1541-1543.
  • 21. Ladani J.J, Bhimani R.D, Vyas K.B, Nimavat K.S: Method development and validation of roflumilast in tablet dosage form by UV spectrophotometry. Journal of Atoms and Molecules 2012, 2 (5): 369-374.
  • 22. Patel K.R, Desai D.G, Zanwar A, Sen A.K, Seth A.K: Development and validation of UV spectroscopy method for estimation of roflumilast in bulk and tablet dosage form. Pharma Science Monitor 2013, 4 (3): 274-280.
  • 23. Popovic G.V, Pfendt L.B, Stefanovic V.M: Analytical application of derivative spectrophotometry. Journal of Serbian Chemical Society, 2000, 65 (7): 457-472.
  • 24. ICH Harmonized Tripartite Guideline Q2 (R1) International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use, Validation of Analytical Procedures: Text and Methodology, International Conference on Harmonization, Geneva, Switzerland 2005.
  • 25. International Conference on Harmonization (ICH) Topic Q2A, Validation of Analytical Procedures; Methodology, CPMP / ICH /281, 1995.
  • 26. The United States Pharmacopoeia 29, The National Formulary 24, U.S. Pharmacopeial Convention, Rockville MD, 2006, 3050-3053.
  • 27. Ermer J: Validation in pharmaceutical analysis. Part I: An integrated approach. Journal of Pharmaceutical Biomedical. Analysis, 2001, 24: 755-767.
  • 28. Taverniers I, Loose D.M, Bockstaele E.V: Trends in quality in the analytical laboratory. II. Analytical method validation and quality assurance. Trends in Analytical Chemistry, 2004, 23 (8): 535-552.
  • 29. Ermer J, Ploss H.J. Validation in pharmaceutical analysis, part II: central importance of precision to establish acceptance criteria and for verifying and improving the quality of analytical data. Journal of Pharmaceutical and Biomedical Analysis, 2005, 37: 859-870.
  • 30. Vander Heyden Y, Nijhuis A, Smeyers-Vebreke J, Vandeginste B.G.M, Massart D.L: Guidance for robustness/ruggedness tests in method validation. Journal of Pharmaceutical and Biomedical Analysis ,2001, 24: 723-753.
  • 31. Green J.M: A practical guide to analytical method validation. Journal of Analytical Chemistry, 1996, 68: 305A-309A.
There are 31 citations in total.

Details

Primary Language Turkish
Journal Section Research Article
Authors

Mehmet Atmaca This is me

İncilay Süslü

Publication Date January 1, 2016
Published in Issue Year 2016 Issue: 1

Cite

Vancouver Atmaca M, Süslü İ. Farmasötik Formülasyonlarda Roflumilast’ın Türev Spektrofotometrik Yöntem ile Tayini. HUJPHARM. 2016(1):27-49.