Determination of Propranolol Hydrochloride in Pharmaceutical Preparations Using Near Infrared Spectrometry with Fiber Optic Probe and Multivariate Calibration Methods (original) (raw)
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2015
Objective: to develop and validate a new very rapid, sensitive, reverse phase Ultra Performance Liquid Chromatography (RP-UPLC) technique for the estimation of Propranolol Hydrochloride in dosage form, as there is no official monograph & no analytical method by UPLC. Methodology: Chromatographic separation was achieved on a Waters Acquity BEH C 18 column (30 x 2.1 mm, 1.7μm) using a gradient method with mobile phase composed of trifluoroacetic acid (0.1%) and acetonitrile in the ratio 80:20 v/v. The flow rate was 0.3 ml/min, temperature of the column was maintained at ambient and detection was made at 230 nm. The run time was as short as 2.5 min. The developed method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to linearity, accuracy, precision, specificity and robustness. Results: The developed method was linear for Propranolol Hydrochloride from 10-50 μg/ml and the linear regression obtained was > 0.999. Precision, evaluated by intra-and inter-day assays had relative standard deviation (R.S.D) values within 0.72 %. Recovery data were in the range 96.70 to 98.72%. Conclusion: The method is precise, accurate, linear, robust and fast. The short retention time of 0.98 min allows the analysis of a large number of samples in a short period of time and, therefore, should be cost-effective for routine analysis in the pharmaceutical industry.
Analytical and Bioanalytical Chemistry, 2006
Two new analytical methods have been developed as convenient and useful alternatives for simultaneous determination of hydrochlorothiazide (HCT) and propranolol hydrochloride (PRO) in pharmaceutical formulations. The methods are based on the first derivative of ratio spectra (DRS) and on partial least squares (PLS) analysis of the ultraviolet absorption spectra of the samples in the 250-350-nm region. The methods were calibrated between 8.7 and 16.0 mg L −1 for HCT and between 14.0 and 51.5 mg L −1 for PRO. An asymmetric full-factorial design and wavelength selection (277-294 nm for HCT and 297-319 for PRO) were used for the PLS method and signal intensities at 276 and 322 nm were used in the DRS method for HCT and PRO, respectively. Performance characteristics of the analytical methods were evaluated by use of validation samples and both methods showed to be accurate and precise, furnishing near quantitative analyte recoveries (100.4 and 99.3% for HCT and PRO by use of PLS) and relative standard deviations below 2%. For PLS the lower limits of quantification were 0.37 and 0.66 mg L −1 for HCT and PRO, respectively, whereas for DRS they were 1.15 and 3.05 mg L −1 for HCT and PRO, respectively. The methods were used for quantification of HCT and PRO in synthetic mixtures and in two commercial tablet preparations containing different proportions of the analytes. The results of the drug content assay and the tablet dissolution test were in statistical agreement (p<0.05) with those furnished by the official procedures of the USP 29. Preparation of dissolution profiles of the combined tablet formulations was also performed with the aid of the proposed methods. The methods are easy to apply, use relatively simple equipment, require minimum sample pre-treatment, enable high sample throughput, and generate less solvent waste than other procedures.
INTERNATIONAL RESEARCH JOURNAL OF PHARMACY, 2013
The first order derivative of UV spectrometry method for simultaneous determination of Propranolol hydrochloride (PRO) and Flunarizine dihydrochloride (FLU) in pure bulk drug and combined dosage form was found to be simple, accurate, fast, precise and reproducible. The first derivative values measured at 289nm for PRO and 253nm for FLU. The linearity for zero order derivative method was carried out by using the concentration range 4-28µg/ml for PRO and 3-7µg/ml for FLU. The coefficient correlation of PRO and FLU for zero order was found to be 0.9995 and 0.9991 respectively. At zero crossing point of PRO (289nm) FLU showed a measurable derivative absorbance where as at the zero crossing point of FLU (253nm), PRO showed appreciable derivative absorbance value. The coefficient correlation of PRO and FLU for first order derivative was found to be 0.9991 and 0.9995 respectively. Precision study showed that % RSD was within the range of acceptable limits (<2). The % recovery for PRO and FLU was found to be in the range of 98-102% and 100-101% respectively. The percentage assay was found to be as 99.5 and 100.12% for PRO and FLU. The results of analysis have been validated as per ICH Q2 (R1) guidelines. This method has applied successfully for the determination of PRO and FLU in its combination with a high percentage of recovery good accuracy and precision.
European Journal of Pharmaceutical Sciences, 2006
Near infrared spectroscopy Simultaneous determination Method validation a b s t r a c t A near infrared spectroscopic method for the simultaneous determination of the active principles paracetamol, ascorbic acid, dextrometorphan hydrobromide, caffeine and chlorpheniramine maleate in a pharmaceutical preparation was developed. The five active principles are quantified using a partial least-squares regression method (PLS1). The proposed method is applicable over a wide analyte concentration range (0.04-6.50 wt.%), so it requires careful selection of the calibration set. Also, there is the difficulty of ensuring thorough homogenization of the product. The method was validated in accordance with the ICH standard and the EMEA validation guidelines for NIR spectroscopy by determining its selectivity, linearity, accuracy, precision and robustness. Based on the results, it is an effective alternative to existing choices (HPLC and redox titrimetry) for the same purpose.
The present study narrates the developed and validated simple, reliable, sensitive, precise and accurate Spectrophotometric and RP-HPLC methods for the simultaneous estimation of Fenbendazole and Niclosamide in pharmaceutical dosage form. In the first order derivative method 0.1 N methanolic HCl was used as diluent. The zero crossing point wavelengths selected for the analysis were 226 nm and 317 nm for Fenbendazole and Niclosamide, respectively and RP – HPLC method has been developed using 1% methanolic HCl as diluent. Separations of drugs were achieved on L1 C18 100 A⁰ column (250 x 4.6 mm, 5 μ) using 2 gm potassium dihydrogen phosphate and acetonitrile (70:30, v/v) as mobile phase with flow rate 1.0 mL/min. The detection wavelength was 290 nm. Validation of developed methods was done according to ICH Q2 (R1) guideline. Calibration curve was linear over the concentration range of 3-9μg/mL (Fenbendazole) and 10-30 μg/mL (Niclosamide) for spectrophotometric method and 24 - 39 μg/mL (Fenbendazole) and 80 – 130 μg/mL (Niclosamide) for RP – HPLC method. The developed RP-HPLC and derivative spectrophotometric method were successfully applied for the quantitative determination of cited drugs in pharmaceutical dosage form. The correlation coefficients (r2) value greater than 0.995. Accuracy of methods were determined by recovery studies and it was found to be 98 to 102 %. The % RSD values for all the validation parameters were less than 2.0 % for both the methods. The developed UV and RP-HPLC methods were compared by t - test and it was found that tstat value was less than tcritical value for all. Hence there was no significant difference between the developed methods.
Rasayan Journal of Chemistry, 2021
Chloramphenicol is an antibiotic compound that inhibits bacterial protein synthesis. All pharmaceutics in the form of finished goods and raw materials must meet the requirements of Indonesian Pharmacopoeia or other standard books. The objectives of this study were to develop and validate a simple and fast analytic method by Fourier Transform Infrared (FTIR) spectrophotometry that allows for qualitative and quantitative analysis of chloramphenicol levels in capsule preparations. Chloramphenicol levels were determined by FTIR analysis using methanol solvents with 0.1 mm slit in the wavenumber range 4000 cm-1 to 650 cm-1. The specific wavenumbers of chloramphenicol solution in methanol were 1695.9 cm–1, 1526.3 cm–1, and 1351.2 cm–1. Peak height analysis was not significantly different from peak area analysis, and all samples analyzed fulfilled the requirements of the Indonesian Pharmacopoeia, 6th Edition (2020). Analytical validation met requirements for accuracy, precision, linearity,...
Analytica Chimica Acta, 2007
This work presented an application of the second-order advantage provided by parallel factor analysis (PARAFAC) aiming at direct determination of propranolol, a -blocker also used as doping agent, in human urine by spectrofluorimetry. The adopted strategy combined the use of PARAFAC, for extraction of the pure analyte signal, with the standard addition method, for a determination in the presence of an individual matrix effect caused by the quenching action of the proteins present in the urine. The urine samples were previously 100 times diluted. For each sample, four standard additions were performed, in triplicates. A specific PARAFAC model was built for each triplicate of each sample, from three-way arrays formed by 231 emission wavelengths, 8 excitation wavelengths and 5 measurements (sample plus 4 additions). The models were built with three factors and always explained more than 99.87% of the total variance. The obtained loadings were related to PRO and two background interferences. The scores related to PRO were used for a linear regression in the standard addition method. The obtained determinations in the PRO concentration range from 5.0 to 20.0 g ml −1 provided recoveries between 91.1 and 108.4%.
International Journal of Pharmacy and Pharmaceutical Sciences, 2018
Objective: A new spectrophotometric method for the determination of propranolol hydrochloride (PRO) and metoprolol tartrate (MTP), beta blocker drugs, has been developed for their analysis in pharmaceutical dosage forms for the purpose of quality control and water samples for monitoring impact on environmental water quality of natural sources and in biological fluids for ascertaining their physiological performance. Methods: The method is based on the derivatization of the amino function present in these drugs to the corresponding yellow copper (I) drug dithiocarbamate derivative through reaction with carbon disulphide, pyridine and copper (I) perchlorate in aqueous acetonitrile and measuring absorbance at 406 nm for propranolol and 400 nm for metoprolol. The different experimental parameters affecting the development and stability of the colour were carefully studied and optimized. Results: The Beer's law is obeyed in the range of 1.0-40.0 μg/ml of each drug solution with a correlation coefficient 0.999. The maximum relative standard deviations (RSDs) in the analysis of pure PRO and MTP were 1.01 and 1.52 % respectively. The recoveries of the drugs from pharmaceutical formulations, spiked water samples and biological fluids were in the range 98.0-100.5 % with RSDs in the range 0.23-1.94% indicating good accuracy and precision of the method. Conclusion: The instantaneous development of colour and its stability, well-established stoichiometry of the reaction and above simplicity and rapidity of procedures are some special attributes of the proposed method.
Resolution of binary mixtures of metoprolol and propranolol without sample pretreatment has been successfully achieved, using three different methods. The first method was based on application of Vierodt’s method that involves measurements of the absorbances at 222.6 and 213.4 nm for metoprolol and propranolol. Calibration graphs were established in the range of 1-70 μg/mL and 0.5-30 μg/mLfor metoprolol and propranolol, respectively. The second method describes the use of multivariate spectophotometric calibration by using partial least squares (PLS) analysis of UV spectral data. In the third method, high performance liquid chromatography (HPLC) was performed by using reversed phase column and a mobile phase composed of 0.01 mol/LNaH2PO4 (adjusted to pH 3.0 with phosphoric acid) - methanol - acetonitril (45:45:10, v:v:v). The proposed methods were validated and results obtained by adopting the three methods were statistically analyzed.