Palavras-chave
teste de estresse
cromatografia líquida de alta eficiência
validação analítica
Como Citar
Resumo
Bromidrato de fenoterol é um agente agonista adrenérgico β2-seletivo utilizado para tratamento de asma e doenças pulmonares crônicas obstrutivas. A metodologia analítica por cromatografia líquida de alta eficiência (CLAE) foi desenvolvida e validada para a determinação quantitativa de bromidrato de fenoterol. A condição analítica empregada incluiu coluna em fase reversa C18 (150 mm × 3,9 mm d.i., 5 μm) Thermo®, fase móvel composta de mistura de acetonitrila e água (30:70, v/v) com 0,1% de trietilamina e pH ajustado para 5,0 com ácido fórmico, vazão de 1,0 mL.min-1 e detecção em UV a 276 nm. A faixa de linearidade foi de 0,025 a 0,15 mg.mL-1; a curva analítica mostrou coeficiente de correlação > 0,999. O limite de detecção (LD) foi de 0,003 mg.mL-1 e o limite de quantificação de 0,012 mg.mL-1. A repetitibilidade da técnica (desvio padrão relativo) foi ≤ 2,0% e a exatidão revelou média percentual de recuperação de 99,53%. A metodologia proposta é de simples execução, rápida, precisa, exata e sensível. As vantagens sobre as demais técnicas são baixo custo e poucas condições poluentes. Demonstrou, ainda, simplicidade e resultados confiáveis para ser aplicada no controle de qualidade de produtos farmacêuticos contendo bromidrato de fenoterol como ingrediente ativo.Referências
1. Gleiter CH. Fenoterol: Pharmacology and Clinical Use. Cardiovasc Drug Rev. 1999;17:87-106.
2. Jacobson GA, Peterson GM. High-performance liquid chromatographic assay for the simultaneous determination of ipratropium bromide, fenoterol, salbutamol and terbutaline in nebulizer solution. J Pharm Biomed Anal. 1994;12:825-32.
3. Polettini A, Montagna M, Hogendoorn EA, Dijkman E, van Zoonen P, van Ginkel LA. Applicability of coupled-column liquid chromatography to the analysis of β-agonists in urine by direct sample injection I. Development of a single-residue reversed-phase liquid chromatography-UV method for clenbuterol and selection of chromatographic conditions suitable for multi-residue analysis. J Chromatogr A. 1995;695:19-31.
4. Kramer S, Blaschke G. High-performance liquid chromatographic determination of the β2-selective adrenergic agonist fenoterol in human plasma after fluorescence derivatization. J Chromatogr B. 2001;751:169-75.
5. Meineke I, Steinmetz H, Kramer S, Gleiter CH. Determination of fenoterol in human plasma by HPLC with fluorescence detection after derivatization. J Pharm Biomed Anal. 2002;29:147-52.
6. Shen S, Ouyang J, Baeyens WRG, Delanghe JR, Yang Y. Determination of β2-agonists by ion chromatography with direct conductivity detection. J Pharm Biomed Anal. 2005;38:166-72.
7. Siluk D, Kim HS, Cole T, Wainer IW. HPLC-electrospray mass spectrometric assay for the determination of (R,R)-fenoterol in rat plasma. J Pharm Biomed Anal. 2008;48:960-4.
8. Henze MK, Opfermann G, Spahn-Langguth H, Schänzer W. Screening of β-2 agonists and confirmation of fenoterol, orciprenaline, reproterol and terbutaline with gas chromatography–mass spectrometry as tetrahydroisoquinoline derivatives. J Chromatogr B. 2001;751:93-105.
9. Boyd D, Barreira-Rodriguez JR, Miranda-Ordieres AJ, Tunon-Blanco P, Smyth MR. Voltammetric study of salbutamol, fenoterol and metaproterenol at unmodified and Nafion-modified carbon paste electrodes. Analyst. 1994;119:1979-84.
10. Belal F,AL-Malaq HA,AL-Majed AA. Voltammetric determination of isoxsuprine and fenoterol in dosage forms and biological fluids through nitrosation. J Pharm Biomed Anal. 2000;23:1005-15.
11. Haasnoot W, Stouten P, Lommen A, Cazemier G, Hooijerink D, Schilt R. Determination of fenoterol and ractopamine in urine by enzyme immunoassay. Analyst. 1994;119:2675-80.
12. Nikolic K, Arsenijevec L, Bogavac M. Coulometric determination of some antiasthmatics. J Pharm Biomed Anal. 1993;11:207-10.
13. Tanabe S, Togawa T, Kawanabe K. Colorimetric flow injection determination of resorcinol-type β2-adrenergic drugs with phenanthro [9,10-d]imidazole-2-N-chloroimide. Anal Sci. 1989;5:513-6.
14. Wachs T, Sheppard RL, Henion J. Design and applications of a self-aligning liquid junction-electrospray interface for capillary electrophoresis-mass spectrometry. J Chromatogr B. 1996;685:335-42.
15. Sirichaia S, Khanatharana P. Rapid analysis of clenbuterol, salbutamol, procaterol, and fenoterol in pharmaceuticals and human urine by capillary electrophoresis. Talanta. 2008;76:1194-8.
16. Ullrich T, Wesenberg D, Bleuel C, Krauss G, Schmid MG, Weiss M et al. Chiral separation of the β2-sympathomimetic fenoterol by HPLC and capillary zone electrophoresis for pharmacokinetic studies. Biomed Chromatogr. 2010;24:1125-9.
17. El-Shabrawy Y, Belal F, Sharaf El-Din M, Shalan S. Spectrophotometric determination of fenoterol hydrobromide in pure form and dosage forms. Il Fármaco. 2003; 58: 1033-8.
18. ICH Steering Committee, International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use, Validation of Analytical Procedures: Text and Methodology, Q2(R1), novembro, Genebra, Suíça, 2005.
19. Association of Official Analytical Chemists International. Official Methods of Analytical Chemists of AOAC International, 17. ed., XX, 2003.
Este trabalho está licenciado sob uma licença Creative Commons Attribution 4.0 International License.
Copyright (c) 2012 Helena Miyoco Yano, Fernanda Fernandes Farias, Marcelo Beiriz Del Bianco, Pedro Lopez Garcia