1H and 13C NMR characteristics of β-blockers

The β-blockers are important drugs and decades of clinical experience proved their high medical status. However, to the best of our knowledge, there is no complete assignment of (1)H and (13)C NMR resonances of popular representatives: acebutolol, alpenolol, pindolol, timolol and propranolol and the published NMR data on carvedilol and atenolol are incorrect. Therefore, (1)H and (13)C NMR spectroscopy was applied for the characterization of a series of β-adrenolytics: carvedilol (1), pindolol (2), alprenolol (3), acebutolol (4), atenolol (5), propranolol (6) and timolol (7). Two-dimensional NMR experiments (COSY, HMQC, HMBC, NOESY) allowed the unequivocal assignment of (1)H and (13)C spectra for solution (DMSO-d(6) ). Salts and bases can be easily distinguished based on (13)C chemical shifts which are within 65.0-65.5 ppm (OC2) and 46.9-47.0 (NC3) for hydrochlorides and larger, ca. 68.4 ppm (OC2) and 50.3-52.6 (NC3) for bases. NMR data of 1-7 should be included in pharmacopoeias.     

Diazotised 4-Nitroaniline as a Chromogenic Reagent for the Determination of Indole Derivatives in Certain Pharmaceutical Preparations

Abstract

A sensitive colorimetric method has been devised for microdetermination of six indole derivatives; ergotamine tartrate, methylergometrine maleate, dihydroergocornine methanesulphonate, dihydroergocristine methanesulphonate, dihydroergocryptine methanesulphonate and pindolol, both in pure form and in pharmaceutical preparations. The method is based on the reaction of indole moiety with diazotised 4-nitroaniline in buffer solution of pH 6 to produce a stable yellow monoazo dye. Beer's law is obeyed over final concentration ranges 8–32 μgm1^?1 for ergotamine tartrate, 4–48 μgml^?1 for methylergometrine maleate, 8–56 μgml^?1 for dihydro-ergot alkaloids and 1–10 μgml^?1 for Pindolol with apparent molar absorptivity range (7.62 × 10³?2.61 × 10⁴) 1.mole^?1.cm^?1. A study has been made to determine the optimum conditions of the colour reaction.     

Spectrophotometric Determination of Some Cardiovascular Drugs Using P-Chloranilic Acid

Abstract

A simple and sensitive spectrophotometric method for the assay of some cardio-vascular drugs is described. The method is based on the interaction of the drug and p-chloranilic acid (p-CA) to give a stable and intensively coloured ion-pair salt. The drugs used are quinidine sulphate, prenylamine lactate, dipyridamol, hydralazine hydrochloride, tolazoline hydrochloride and pindolol. The optimum experimental conditions for colour development have been studied. Conformity to Beer's law enabled the determination of these drugs in their pharmaceutical preparations. The assay results are in accord with the pharmacopoeal assay results.     

Conductometric titration of pindolol and propranolol using ammonium reineckate and potassium tetracyanonickelate

A simple and sensitive conductometric method for the determination of 2–24 mg of pindolol and propranolol hydrochlorides using ammonium reineckate and potassium tetracyanonickelate in an ethanol-water mixture is described. The effect of the solvent ratio, reagent concentration, time and temperature on the shape of the titration curve is studied. Statistical treatment of the experimental results indicates that the method is precise and accurate. The accuracy of the method is indicated by the excellent recovery (98.2–101.2%) and the precision is supported by the low standard deviation value < 0.10. The sensitivity of the proposed method is discussed and the results are compared with the pharmacopoeial non-aqueous titration method.