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1.
J AOAC Int ; 96(2): 324-30, 2013.
Artigo em Inglês | MEDLINE | ID: mdl-23767357

RESUMO

A size-exclusion LC method was validated for the determination of interferon-a2a (rhlFN-alpha2a) in pharmaceutical formulations without interference from human serum albumin. Chromatographic separation was performed on a BioSep-SEC-S 2000 column (300 x 7.8 mm id). The mobile phase consisted of 0.001 M monobasic potassium phosphate, 0.008 M sodium phosphate dibasic; 0.2 M sodium chloride buffer, pH 7.4, run at a gradient flow rate and using photodiode array detection at 214 nm, was used. Chromatographic separation was achieved with a retention time of 17.2 min, and the analysis was linear over the concentration range of 1.98 to 198 microg/mL (r2 = 0.9996). The accuracy was 101.39%, with bias lower than 1.67%. The LOD and LOQ were 0.87 and 1.98 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for precision and robustness. The method was applied to the assessment of rhlFN-alpha2a and related proteins in biopharmaceutical dosage forms, and the content/potencies were correlated to those given by a validated RP-LC method and an in vitro bioassay. It was concluded that use of the methods in conjunction allows a great improvement in monitoring stability and QC, thereby ensuring the therapeutic efficacy of the biotechnology-derived medicine.


Assuntos
Cromatografia Líquida/métodos , Interferon-alfa/química , Linhagem Celular Tumoral , Estabilidade de Medicamentos , Humanos , Reprodutibilidade dos Testes , Sensibilidade e Especificidade
2.
J Chromatogr Sci ; 51(2): 192-9, 2013 Feb.
Artigo em Inglês | MEDLINE | ID: mdl-22832547

RESUMO

A reversed-phase liquid chromatography (RP-LC) method was validated for the determination of tigecycline in lyophilized powder. The LC method was conducted on a Luna C18 column (250 × 4.6 mm i.d.), maintained at room temperature. The mobile phase consisted of buffer containing sodium phosphate monobasic (0.015M) and oxalic acid (0.015M) (pH 7.0)-acetonitrile (75:25, v/v), run at a flow rate of 1.0 mL/min and using ultraviolet detection at 280 nm. The chromatographic separation was obtained with a retention time of 8.6 min, and was linear in the range of 40-100 µg/mL (r(2) = 0.9997). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed no interference of the excipients. The accuracy was 99.01% with a bias lower than 1.81%. The limits of detection and quantitation were 1.67 and 5.05 µg/mL, respectively. Moreover, method validation demonstrated satisfactory results for precision and robustness. The proposed method was applied for the analysis of the lyophilized powder formulation, contributing to improve the quality control and to assure the therapeutic efficacy.


Assuntos
Cromatografia de Fase Reversa/métodos , Minociclina/análogos & derivados , Estabilidade de Medicamentos , Limite de Detecção , Modelos Lineares , Minociclina/análise , Minociclina/química , Minociclina/normas , Pós/química , Pós/normas , Reprodutibilidade dos Testes , Tigeciclina
3.
J Chromatogr Sci ; 48(8): 641-6, 2010 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-20819293

RESUMO

A micellar electrokinetic chromatography method (MEKC) is developed and validated for the analysis of fluticasone propionate (FP) in nasal sprays. The MEKC method is performed on a fused-silica capillary (50 mum i.d.; effective length, 40 cm). The background electrolyte consists of 25 mM borate and 25 mM anionic detergent SDS solution at pH 9. The capillary temperature is maintained at 35 degrees C, and the applied voltage is 20 kV. The injection is performed using the hydrodynamic mode at 50 mbar for 6 s with detection at 238 nm. The method is linear in the range of 2-80 mug/mL (r(2) = 0.9956). The specificity and stability-indicating capability are proven through forced degradation studies inclusive by mass spectrometry, which also shows that there is no interference of the excipients. The limit of detection and limit of quantitation are 0.56 and 2 mug/mL, respectively. Moreover, method validation demonstrates acceptable results for accuracy, precision, and robustness. The proposed method was successfully applied for the quantitative analysis of FP nasal sprays, and the results were compared to a validated reversed-phase liquid chromatographic method, showing non-significant difference (P > 0.05).


Assuntos
Androstadienos/análise , Cromatografia Capilar Eletrocinética Micelar/métodos , Sprays Nasais , Androstadienos/química , Boratos , Estabilidade de Medicamentos , Fluticasona , Concentração de Íons de Hidrogênio , Análise dos Mínimos Quadrados , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Dodecilsulfato de Sódio , Temperatura
4.
J AOAC Int ; 93(2): 523-30, 2010.
Artigo em Inglês | MEDLINE | ID: mdl-20480899

RESUMO

An RP-HPLC method was validated for the determination of entecavir in tablet dosage form. The HPLC method was carried out on a Gemini C18 column (150 x 4.6 mm id) maintained at 30 degrees C. The mobile phase consisted of acetonitrile-water (95 + 5, v/v)/potassium phosphate buffer (0.01 M, pH 4; 9 + 91, v/v) pumped at a flow rate of 1.0 mL/min. Photodiode array detection was at 253 nm. The chromatographic separation was obtained with a retention time of 4.18 min, and the method was linear in the range of 0.5-200 microg/mL (r2 = 0.9998). The specificity and stability-indicating capability of the method was proven through forced degradation studies, which also showed that there was no interference of the excipients and an increase of the cytotoxicity only by the basic condition. The accuracy was 101.19%, with bias lower than 1.81%. The LOD and LOQ were 0.39 and 0.5 microg/mL, respectively. Method validation demonstrated acceptable results for precision and robustness. The proposed method was applied for the analysis of tablet formulations, to improve QC and assure therapeutic efficacy.


Assuntos
Antivirais/análise , Antivirais/química , Cromatografia Líquida de Alta Pressão/métodos , Guanina/análogos & derivados , Comprimidos/análise , Tecnologia Farmacêutica/métodos , Soluções Tampão , Química Farmacêutica/métodos , Cromatografia/métodos , Guanina/análise , Guanina/química , Hidrólise , Espectrometria de Massas/métodos , Modelos Químicos , Fosfatos/química , Compostos de Potássio/química , Valores de Referência , Reprodutibilidade dos Testes , Água/química
5.
Ther Drug Monit ; 32(3): 282-8, 2010 Jun.
Artigo em Inglês | MEDLINE | ID: mdl-20431506

RESUMO

Tigecycline is a new glycylcycline with an expanded broad-spectrum antibiotic, including inhibition of Gram-positive, Gram-negative, atypical, anaerobic, and antibiotic-resistant organisms. Trials have demonstrated that tigecycline is noninferior to the comparators for the treatment of complicated skin and skin structure infections as well as complicated intra-abdominal infections. Tigecycline is only available as an intravenous preparation and analytical methods to its quantitation in pharmaceutical products has not been published to date. This review examined tigecycline characteristics, the spectrum and mechanism of action, pharmacokinetics, applications, and, mainly, the instrumental conditions of published chromatographic methods used to measure tigecycline, its metabolites, and some analogs in clinical and biologic research.


Assuntos
Antibacterianos/farmacologia , Bactérias/efeitos dos fármacos , Farmacorresistência Bacteriana Múltipla/efeitos dos fármacos , Minociclina/análogos & derivados , Tetraciclinas/farmacologia , Testes de Sensibilidade Microbiana , Minociclina/farmacologia , Tigeciclina
6.
J Chromatogr B Analyt Technol Biomed Life Sci ; 877(24): 2471-6, 2009 Aug 15.
Artigo em Inglês | MEDLINE | ID: mdl-19560410

RESUMO

A capillary zone electrophoresis (CZE) method was validated for the analysis of recombinant human granulocyte colony-stimulating factor (rhG-CSF) and performed on a fused-silica capillary, with detection at 195 nm. The background electrolyte solution consisted of 50 mM sodium tetraborate solution at pH 9. The method was linear in the concentration range of 1-200 microg/mL and the limit of quantitation (LOQ) was 1 microg/mL, with acceptable validation parameters. The method was applied for the analysis of pharmaceutical formulations, and the results were correlated to the reversed-phase HPLC method (RP-HPLC), size-exclusion HPLC method (SE-HPLC) and in vitro bioassay method.


Assuntos
Eletroforese Capilar/métodos , Fator Estimulador de Colônias de Granulócitos/análise , Bioensaio/métodos , Linhagem Celular , Química Farmacêutica , Cromatografia Líquida de Alta Pressão/métodos , Fator Estimulador de Colônias de Granulócitos/farmacologia , Humanos , Proteínas Recombinantes/análise , Proteínas Recombinantes/farmacologia
7.
J Sep Sci ; 31(16-17): 3098-105, 2008 Sep.
Artigo em Inglês | MEDLINE | ID: mdl-18693320

RESUMO

A stability-indicating MEKC was developed and validated for the analysis of rupatadine in tablet dosage forms, using nimesulide as internal standard. The MEKC method was performed on a fused-silica capillary (50 microm id; effective length, 40 cm). The BGE consisted of 15 mM borate buffer and 25 mM anionic detergent SDS solution at pH 10. The capillary temperature was maintained at 35 degrees C and the applied voltage was 25 kV. The injection was performed using the hydrodynamic mode at 50 mbar for 5 s, with detection by photodiode array detector set at 205 nm. The method was linear in the range of 0.5-150 microg/mL (r2=0.9996). The specificity and stability-indicating capability of the method were proven through degradation studies inclusive by MS, and showing also that there was no interference of the excipients and no increase of the cytotoxicity. The accuracy was 99.98% with bias lower than 1.06%. The LOD and LOQ were 0.1 and 0.5 microg/mL, respectively. The proposed method was successfully applied for the quantitative analysis of rupatadine in pharmaceutical formulations, and the results were compared to a validated RP-LC method, showing non-significant difference (p>0.05).


Assuntos
Cromatografia Capilar Eletrocinética Micelar/métodos , Ciproeptadina/análogos & derivados , Preparações Farmacêuticas/química , Animais , Cromatografia Capilar Eletrocinética Micelar/instrumentação , Ciproeptadina/análise , Ciproeptadina/farmacologia , Estabilidade de Medicamentos , Células L/efeitos dos fármacos , Camundongos , Estrutura Molecular , Reprodutibilidade dos Testes , Sensibilidade e Especificidade , Comprimidos , Fatores de Tempo
8.
J Sep Sci ; 31(1): 169-76, 2008 Jan.
Artigo em Inglês | MEDLINE | ID: mdl-18069701

RESUMO

A CZE method was developed and validated for the analysis of etoricoxib in pharmaceutical dosage forms, using prilocaine as an internal standard. The CZE method was carried out on a fused-silica capillary (50 microm id, effective length 40 cm). The BGE consisted of 25 mM tris-phosphate solution at pH 2.5. The capillary temperature was maintained at 35 degrees C, the applied voltage was 25 kV, the injection was performed using the pressure mode at 50 mbar for 5 s, with detection at 234 nm using a photodiode array detector. The method was linear in the range of 2-150 microg/mL (r(2) = 0.9999). The specificity and stability-indicating capability were proven through the degradation studies and showing also that there was no interference of the excipients of the formulation. The accuracy was 99.49% with RSD of 0.66%. The limits of quantitation and detection were 2 and 0.58 microg/mL, respectively. Moreover, method validation demonstrated acceptable results for the precision, sensitivity, and robustness. The proposed method was successfully applied for the quantitative analysis of etoricoxib pharmaceutical formulations, and the results compared to the HPLC and LC-MS/MS methods, showing nonsignificant difference (p >0.05).


Assuntos
Formas de Dosagem , Eletroforese Capilar/métodos , Piridinas/análise , Piridinas/química , Sulfonas/análise , Sulfonas/química , Química Farmacêutica , Etoricoxib , Estrutura Molecular
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