Advanced chemometric methods for simultaneous quantitation of caffeine, codeine, paracetamol, and p-aminophenol in their quaternary mixture (original) (raw)
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Journal of AOAC INTERNATIONAL, 2005
A ratio-spectra zero-crossing first-derivative spectrophotometric method and 2 chemometric methods have been used for the simultaneous determination of ternary mixtures of caffeine (A), 8-chlorotheophylline (B), and chlorphenoxamine hydrochloride (C) in bulk powder and dosage forms. In the ratio-spectra zero-crossing first-derivative spectrophotometric technique (1DD), calibration curves were linear in the range of 4–20 μg/mL for A, B, and C (r = 0.9992, 0.9994, and 0.9976, respectively). The measurements were carried out at 212, 209.2, and 231.4 nm for A, B, and C, respectively. The detection limits for A, B, and C were calculated to be 0.24, 0.34, and 0.13 μg/mL, and the percentage recoveries were 99.1 ± 0.89, 100.1 ± 0.95, and 100.1 ± 1.0, respectively. Two chemometric methods, namely, the partial least-squares (PLS) model and the principal component regression (PCR) model, were also used for the simultaneous determination of the 3 drugs in the ternary mixture. A training set con...
A simple stability-indicating HPLC method for simultaneous analysis of paracetamol and caffeine
A simple, economic, rapid, reliable, and stability-indicating high-performance liquid chromatography (HPLC) method has been developed and validated for the simultaneous determination of paracetamol (PCM) and caffeine (CF) in solid dosage form. The chromatographic separations were achieved with a Waters Symmetry W C18 column (5 μm, 4.6 × 150 mm), using a mixture of methanol and water (40:60, v/v) as a mobile phase, under isocratic elution mode with a flow rate of 0.8 mL/min, and ultraviolet (UV) detection was set at 264 nm. The oven temperature for the column was set and maintained at 35°C. The method was validated according to International Conference on Harmonization (ICH) guidelines, and it demonstrated excellent linearity, with a correlation coefficient of 1 and 0.9999 for PCM and CF, respectively, over the concentration ranges of 15-300 μg/mL (PCM) and 2.5-50 μg/mL (CF). The retention time (t R ) was found to be 2.6 ± 0.001 and 3.5 ± 0.002 min for PCM and CF, respectively. Extensive stress degradation studies were conducted by subjecting the analytes to various stress conditions of acidic and alkaline hydrolysis as well as oxidative, photolytic, and heat degradations. The method was found to efficiently separate the analytes' peaks from that of the degradation products, without any variation in their retention times. The relative standard deviation (RSD) values of all recoveries for PCM and CF were less than 1.3%. The method was found to be suitable for routine analysis of PCM and CF in pharmaceutical dosage form.
Objective: This study was to develop a spectrophotometric method with derivative zero-crossing for determines the levels of paracetamol (PCT), propyphenazone (PRO), and caffeine (CAF) in tablet dosage form without prior separation. Method: The study begins with optimizing the type of solvent, phosphate buffer (pH 7.2) and a mixture of phosphate buffer (pH 7.2) with methanol at ratio 90:10; 70:30; 50:50; 30:70; and 10:90. Spectrophotometric method with zero-crossing, tested validity based on linearity, accuracy, precision, limit of detection, and limit of quantification. Then, the method applied to determine the levels of PCT, PRO, and CAF in tablet. Result: The mixture of phosphate buffer (pH 7.2) with methanol at ratio 70:30 can be used for analysis. Applications zero-crossing technique on assay of PCT and CAF performed on the first derivative and Δλ 2 with λ 239.4 nm for PCT and Δλ 8 with λ 245.6 nm for CAF while PRO in the third derivative and Δλ 8 with λ 249.6 nm, resulting 100.91%, 104.75%, and 103.33% for levels of PCT, PRO, and CAF, respectively. Conclusion: Spectrophotometric derivative method with zero-crossing qualified in validation parameters.
Journal of pharmaceutical and biomedical analysis, 2001
An accurate, simple, reproducible and sensitive method for the determination of paracetamol, caffeine and codeine phosphate has been developed and validated. Paracetamol, caffeine and codeine phosphate were separated using a mBondapack C 8 column by isocratic elution with flow rate 1.0 ml/min. The mobile phase composition was 420/20/30/30 (v/v/v/v) 0.01 M KH 2 PO 4 , methanol, acetonitrile, isopropyl alcohol and spectrophotometric detection was carried out at 215 nm. The linear range of detection for paracetamol, caffeine and codeine phosphate were between 0.400 and 1500 mg/ml; 0.075 and 90 mg/ml; 0.300 and 30 mg/ml, respectively. The method has been shown to be linear, reproducible, specific, sensitive and rugged.
Acta Chromatographica, 2019
A simple, economic, rapid, reliable, and stability-indicating high-performance liquid chromatography (HPLC) method has been developed and validated for the simultaneous determination of paracetamol (PCM) and caffeine (CF) in solid dosage form. The chromatographic separations were achieved with a Waters Symmetry W C18 column (5 μm, 4.6 × 150 mm), using a mixture of methanol and water (40:60, v/v) as a mobile phase, under isocratic elution mode with a flow rate of 0.8 mL/min, and ultraviolet (UV) detection was set at 264 nm. The oven temperature for the column was set and maintained at 35°C. The method was validated according to International Conference on Harmonization (ICH) guidelines, and it demonstrated excellent linearity, with a correlation coefficient of 1 and 0.9999 for PCM and CF, respectively, over the concentration ranges of 15-300 μg/mL (PCM) and 2.5-50 μg/mL (CF). The retention time (t R) was found to be 2.6 ± 0.001 and 3.5 ± 0.002 min for PCM and CF, respectively. Extensive stress degradation studies were conducted by subjecting the analytes to various stress conditions of acidic and alkaline hydrolysis as well as oxidative, photolytic, and heat degradations. The method was found to efficiently separate the analytes' peaks from that of the degradation products, without any variation in their retention times. The relative standard deviation (RSD) values of all recoveries for PCM and CF were less than 1.3%. The method was found to be suitable for routine analysis of PCM and CF in pharmaceutical dosage form.
Simultaneous determination of paracetamol and caffeine in plasma by RP-HPLC
2003
O presente trabalho apresenta uma metodologia simples, rápida e de baixo custo para determinação simultânea de paracetamol (PC) e ibuprofeno (IB) em formulações farmacêuticas por voltametria de pulso diferencial usando eletrodo de diamante dopado com boro (BDD). Os analitos apresentaram picos de oxidação definidos em 0,85 V para o PC e 1,72 V para o IB (vs. Ag/AgCl) sobre o eletrodo de trabalho de BDD em meio de uma solução de H 2 SO 4 0,1 mol L -1 com 10% (v/v) de etanol. As curvas de calibração mostraram uma resposta linear para determinação simultânea dos analitos entre 20 a 400 μmol L -1 (r 2 = 0,999) e os limites de detecção obtidos pelas regressões foram de 7,1 μmol L -1 e 3,8 μmol L -1 para PC e IB, respectivamente. Os estudos de adição e recuperação nas amostras ficaram próximos de 100% e os resultados foram validados por métodos cromatográficos.