Authors:Hanadi A. Al Shaker, Nidal A. Qinna, Hamza Al Hroub, Mahmoud M. H. Al Omari, and Adnan A. Badwan
Propranolol is chemically described as 2-propanol, 1-[(1-methylethyl) amino]-3-(1-naphthalenyloxy) (Figure 1 ). Propranolol is a highly lipophilic drug that is almost completely absorbed from the gastrointestinal
Authors:Sigrid Mennickent, M. Vega, H. Vega, Marta Diego, and Ricardo Fierro
A high-performance thin-layer chromatography (HPTLC) method for the quantification of propranolol in human serum is developed and validated. The method includes a liquid-liquid extraction of the analyte from the matrix using n-heptane-isoamyl alcohol (98.5:1.5, v/v) as the extraction solvent and verapamil as the internal standard.The HPTLC method employed precoated silica gel F254 HPTLC plates (10 cm × 10 cm and 10 cm × 20 cm; layer thickness 0.2 mm) prewashed with methanol, and a mobile phase comprising chloroform-methanol-ammonia (9:1:0.04, v/v/v). The developing solvent was run up to 80 mm in a vertical CAMAG chamber previously saturated with the solvent mixture for 20 min. Densitometric detection was done at λ = 290 nm. The method was linear between 5 and 100 ng/band, corresponding to 0.01 and 0.20 ng μL−1 of propranolol in human serum after the extraction process and applying 50 μL to the chromatographic plates (correlation coefficient = 0.998). The %RSD (absolute value of the coefficient of variation) of intra-assay and inter-assay precision was in the range 1.84–2.85% (n = 3) and 3.52–3.95% (n = 9), respectively. The limit of detection and limit of quantitation were found to be 3.15 and 4.02 ng/band, respectively. The method proved to be accurate, with a recovery between 96.35% and 98.82%, with an RSD not higher than 4.17%, and was selective for the active substance tested, its major metabolite, and the internal standard. This method was successfully applied to quantify propranolol in patient serum samples. Therefore, the method is useful for the quantitative determination of propranolol in human serum.
Authors:Ghodratollah Absalan, Morteza Akhond, Elmira Rafatmah, and Yousef Alipour
Gold nanoparticles (AuNPs) and l-cysteine (l-cys), in order, as first and second layer were coated on the surface of a commercial thin-layer chromatography (TLC) plate. This assemble has been used as a new substrate for direct resolution of propranolol enantiomers based on the ordinary TLC technique. The effect of concentrations of the involved chemicals, time periods of the required processes, pH of the sample solutions, as well as the effects of different coating protocols on the resolution of the enantiomers, were investigated in order to find the optimized separation conditions. The results showed that 10.0 mM copper(II) acetate, in 70% ethanol-water adjusted at pH = 6.3, was suitable for being used as the mobile phase. The AuNPs with the average size of 15 nm and l-cys solution with a concentration of 10.0 mM and pH = 8.1 had been chosen for impregnating TLC plates.
Authors:G. Berger, M. Maziere, C. Prenant, J. Sastre, A. Syrota, and D. Comar
A method is described by which 60 mCi11C propranolol may be obtained from about 1 Ci11CO2 in 30 min without irradiation risk for personnel. The product is chromatographically pure, sterile and apyrogenic with a
specific activity between 500 mCi and 2 Ci/μmole at the time of use. The synthesis involves the preparation of11C acetone followed by fixation of the isopropyl group on the precursor [1-amino-3-(1-naphtyloxy)-2-propanol] by formation
of an imine, then reduction of the latter by sodium cyanoboro hydride. The influence of certain parameters (reagents, precursor,
impurities) on the final product is discussed.
Authors:R. Macêdo, T. Gomes do Nascimento, and J. Veras
This study demonstrates the thermalanalysis applications in compatibility and stability studies of the propranolol binary
mixture sand tablets A and B. The propranolol binary mixtures were prepared in the laboratory and compared to the fully formulated
tablets using the thermogravimetric (TG) and calorimetric(DSC) methods. DSC of binary mixtures showed similar phase transition
to propranolol drug. The tablets phase transition decreased and there was no detectable significant interaction in propranolol–lactose
mixture and tablets. The DSC-photovisual test revealed an interaction similar to the Maillard reaction. The TG isothermal
study showed a difference in the profile between the drug and tablets due excipients quality and problems in manufacture process.
The kinetic parameters indicated a lower stability for the tablets than propranolol drug. The thermal techniques thermally
differentiated the propranolol preparations demonstrating the importance in the design development of pharmaceuticals solid-dosage
Enantiomeric resolution of two commonly used β-blockers, namely, (±)-propranolol and (±)-atenolol, has been achieved on silica gel layers which were bulkimpregnated with β-cyclodextrin. Solvent systems DMF-ethyl acetate-butanol (3:2:5, υ/υ) and butanol-acetic acid-ethyl acetate-ammonia (5:2:2:0.5, υ/υ) successfully resolved the enantiomers of (±)-propranolol and (±)-atenolol, respectively. The spots were located with iodine vapor. The effects of concentration of the chiral selector and mobile phase variation were also studied.
Authors:Ankul Doshi, Bhavini Patel, and Chagan Patel
A simple, precise, and accurate high-performance thin-layer chromatography (HPTLC) method for the simultaneous determination of propranolol hydrochloride (PRP) and flunarizine dihydrochloride (FLU) in their combined tablet dosage form has been developed and validated. Propranolol hydrochloride and flunarizine dihydrochloride from the formulation were separated on silica gel 60 GF254 HPTLC plates with solutions in the proportion of methanol-chloroform-toluene-GAA (3:7.5:7.5:0.3 v/v) as mobile phase. Densitometric quantification was performed at 260 nm. Well-resolved bands were obtained with RF values 0.35 and 0.64 for propranolol hydrochloride and flunarizine dihydrochloride, respectively. The method was validated for precision, accuracy, and specificity. The calibration curve was found to be linear in the concentration range of 3000–15,000 ng band−1 and 750–3700 ng band−1 of PRP and FLU respectively. Correlation co-efficient by area is 0.9991 and 0.9995 for PRP and FLU, respectively. The method is selective and specific, with potential application in pharmaceutical analysis of these drugs in combined tablet dosage form.
Authors:A. Mohan, S. Dhayalamurthi, P. Anandan, and D. Saravanan
The present study reports the dissolution method for a novel fixed dose combination (FDC) containing etodolac (ET) and propranolol hydrochloride (PH) developed utilizing USP Apparatus 1 (basket) at 100 rpm with 1000 mL of phosphate buffer (pH 6.8; 0.05 M) medium at 37°C. An isocratic reversed-phase liquid chromatographic (RPLC) method was also developed for the simultaneous determination of ET and PH on an octadecylsilica column using phosphate buffer (pH 5.5) and acetonitrile (60:40, υ/υ) as the mobile phase with ultraviolet (UV) detection at 292 nm. Validation data were obtained, which demonstrated that the dissolution methodology is accurate, precise, linear, and rugged for the combination tablets.
Resolution of racemic metoprolol, propranolol, carvedilol, bisoprolol, salbutamol, and labetalol, commonly used β-blockers, into their enantiomers has been achieved by TLC on silica gel plates impregnated with optically pure L
-Glu and L
-Asp. Acetonitrile-methanol-water-dichloromethane and acetonitrile-methanol-water-glacial acetic acid mobile phases in different proportions enabled successful separation. The spots were detected with iodine vapor. The detection limits were 0.23, 0.1, 0.27, 0.25, 0.2, and 0.2 μg for each enantiomer of metoprolol, propranolol, carvedilol, bisoprolol, salbutamol, and labetalol, respectively.