RESUMO
Two simple validated and highly selective methods for analysis of paracetamol, codeine, guaifenesin and pseudoephedrine or phenylephrine quaternary mixtures were developed. The first method is a high performance liquid chromatography with diode array detection method where separation was successful using Agilent C18 (150 × 4.6 mm) column, gradient elution of phosphate buffer pH 3, methanol and acetonitrile and diode-array detection at 210 nm. The second method is a HPTLC method followed by densitometric measurement of the spots at 257 nm. Separation was carried out on Merck HPTLC aluminum sheets of silica gel using methylene chloride: methanol: glacial acetic acid: ammonia (17.8: 1.68: 0.4: 0.12, v/v) mobile phase. The methods were applied successfully for analysis of both quaternary mixtures in laboratory-prepared tablets and also validated in regards to linearity, precision, accuracy, sensitivity and stability.
Assuntos
Acetaminofen/análise , Cromatografia Líquida de Alta Pressão/métodos , Codeína/análise , Guaifenesina/análise , Fenilefrina/análise , Pseudoefedrina/análise , Cromatografia em Camada Fina/métodos , Limite de Detecção , Modelos Lineares , Medicamentos Compostos contra Resfriado, Influenza e Alergia/análise , Medicamentos Compostos contra Resfriado, Influenza e Alergia/química , Reprodutibilidade dos Testes , ComprimidosRESUMO
A novel generic reverse phase high performance liquid chromatography (RP-HPLC) method is developed and validated for simultaneous determination of seven pharmaceutically active ingredients, namely, acetaminophen, dextromethorphan, doxylamine, phenylephrine, guaifenesin, caffeine and aspirin. All seven ingredients were quantified in soft gel, syrup and tablet formulations of the over-the-counter US-marketed products, as per the guidelines of the International Conference on Harmonization. The separation was achieved in a 16 min run time on an Agilent Zorbax Phenyl column using a gradient method with two mobile phases. Mobile phase A was 0.15% trifluoro acetic acid in purified water and while mobile phase B was a mixture of acetonitrile and methanol (750:250 v/v) with 0.02% trifluoro acetic acid. The flow rate was 1.0 mL min-1 and injection volume was 10 µL. Detection was performed at 280 nm using a photodiode array detector. As part of the method validation, specificity, linearity, precision and recovery parameters were verified. The concentration and area relationships were linear (R2 > 0.999), over the concentration ranges 20-120 µg mL-1 for acetaminophen, 75-450 µg mL-1 for dextromethorphan, 31.25-187.5 µg mL-1 for doxylamine, 25-150 µg mL-1 for phenylephrine, 25-150 µg mL-1 for aspirin, 6.5-39 µg mL-1 for caffeine and 12-72 µg mL-1 for guaifenesin. The relative standard deviations for precision and intermediate precision were <1.5%. The proposed RP-HPLC generic method is applicable for routine analysis of cold and cough over-the-counter products.
Assuntos
Cromatografia Líquida de Alta Pressão/métodos , Cromatografia de Fase Reversa/métodos , Medicamentos para o Sistema Respiratório/análise , Medicamentos para o Sistema Respiratório/química , Estabilidade de Medicamentos , Limite de Detecção , Modelos Lineares , Medicamentos Compostos contra Resfriado, Influenza e Alergia/análise , Medicamentos Compostos contra Resfriado, Influenza e Alergia/química , Reprodutibilidade dos TestesRESUMO
Orthogonal design (OD) was employed to optimize the separation condition of flow injection-capillary electrophoresis (FI-CE). In order to compare the optimum condition, uniform design and univariate approach were also adopted. The influences of variables such as buffer pH, buffer concentration, acetonitrile (ACN) percentage, and separation voltage were discussed. The optimum separation condition was established. The limits of detection were 1.94 × 10(-2), 6.40 × 10(-3), 1.16 × 10(-2) and 1.94 × 10(-2) µg/mL for dextromethorphan hydrobromide (Dex), chlorphenamine hydrogen maleate (Chl), pseudoephedrine hydrochloride (Pse), and paracetamol (Par), respectively. The RSDs of peaks areas were less than 2.0%. The results showed the OD was an effective method among experimental designs for optimizing the separation conditions of CE. The optimum condition was used for separation and determination of Dex, Chl, Pse, and Par in cold medicines. The average recovery was between 96.68-101.25%.