Development of membrane electrodes for the selective determination of hyoscine butylbromide.

Four polyvinyl chloride (PVC) membrane sensors for the determination of hyoscine butylbromide are described and characterized. The sensors are based on the use of the ion association complexes of hyoscine cation with ammonium reineckate counter anions as ion exchange sites in the PVC matrix. The membranes incorporate ion association complexes of hyoscine with dibutylsebathete (sensor 1), dioctylphthalate (sensor 2), nitrophenyl octyl ether (sensor 3) and beta-cyclodextrin (sensor 4). The performance characteristics of these sensors were evaluated according to IUPAC recommendations, which reveal a fast, stable and linear response for hyoscine over the concentration range of 10(-5)-10(-2)M for sensors 1 and 2 and 10(-6)-10(-2) for sensors 3 and 4 with cationic slopes of -53.19, -55.17, -51.44 and -51.51mV per concentration decade for the four sensors, respectively. The direct potentiometric determination of hyoscine butylbromide using the proposed sensors gave average recoveries % of 99.92+/-1.11, 99.93+/-1.00, 99.94+/-1.18 and 99.87+/-1.39 for the four sensors, respectively. The sensors are used for determination of hyoscine butylbromide in laboratory prepared mixtures, pharmaceutical formulations in combination with ketoprofen and in plasma. Validation of the method shows suitability of the proposed sensors for use in the quality control assessment of hyoscine butylbromide. The developed method was found to be simple, accurate and precise when compared with a reported HPLC method.

Application of new membrane selective electrodes for the determination of drotaverine hydrochloride in tablets and plasma.

The construction and electrochemical response characteristics of poly vinyl chloride (PVC) membrane sensors for the determination of drotaverine hydrochloride were described. The sensors are based on the use of the ion association complexes of drotaverine cation with sodium phosphotungestate (Dro-PTA) or ammonium reineckate (Dro-R) counter anions as ion exchange sites in the PVC matrix. The performance characteristics of these sensors, which were evaluated according to IUPAC recommendations, reveal a fast, stable and linear response for drotaverine over the concentration range 10(-5) to 10(-2) M with cationic slopes of 49.55 and 51.36 mV per concentration decade. The direct potentiometric determination of drotaverine hydrochloride using the proposed sensors gave average recoveries of 99.95+/-0.71 and 100.04+/-0.60 for Dro-PTA and Dro-R, respectively. The sensors are used for determination of drotaverine hydrochloride in tablets, in its mixture with caffeine and paracetamol and in plasma. Validation of the method shows suitability of the proposed sensors for use in the quality control assessment of drotaverine hydrochloride. The developed method was found to be simple, accurate and precise when compared with a reported HPLC method.

Simultaneous high-performance liquid chromatographic assay of furosemide and propranolol HCL and its application in a pharmacokinetic study.

A practical, sensitive, selective and efficient reversed-phase high-performance liquid chromatographic (HPLC) method is reported for the determination of two commonly used antihypertensive drugs, furosemide and propranolol hydrochloride. The drugs were eluted through a Nucleosil C(18) column with a mobile phase composed of 0.02 M potassium dihydrogen phosphate and acetonitrile (80:20, v/v) adjusted to pH 4.5 and the effluent from the column was monitored at 235 nm. The present method enabled simple and isocratic HPLC with UV detection of these drugs in raw materials and in pharmaceutical formulations. These procedures were also applied for the assay of furosemide in rabbits' plasma, using propranolol hydrochloride as an internal standard. The linear concentration range of the assay was 0.1-200 and 5-200 microg ml(-1) for furosemide and propranolol hydrochloride, respectively. The inter and intra-day assay precision and accuracy showed reproducibility and good linearity (r(2)>0.99). The method retained its accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed method was statistically analysed and compared with those obtained by the reported methods.

Stability-indicating spectrophotometric and densitometric methods for determination of aceclofenac.

Three methods were developed for the determination of aceclofenac in the presence of its degradation product, diclofenac. In the first method, third-derivative spectrophotometry (D3) is used. The D3 absorbance is measured at 283 nm where its hydrolytic degradation product diclofenac does not interfere. The suggested method shows a linear relationship in the range of 4-24 micrograms mL-1 with mean percentage accuracy of 100.05 +/- 0.88. This method determines the intact drug in the presence of up to 70% degradation product with mean percentage recovery of 100.42 +/- 0.94. The second method depends on ratio-spectra first-derivative (RSD1) spectrophotometry at 252 nm for aceclofenac and at 248 nm for determination of degradation product over concentration ranges of 4-32 micrograms mL-1 for both aceclofenac and diclofenac with mean percentage accuracy of 99.81 +/- 0.84 and 100.19 +/- 0.72 for pure drugs and 100.17 +/- 0.94 and 99.73 +/- 0.74 for laboratory-prepared mixtures, respectively. The third method depends on the quantitative evaluation of thin-layer chromatography of aceclofenac using chloroform:methanol: ammonia (48:11.5:0.5 v/v/v) as a mobile phase. Chromatograms were scanned at 274 and 283 nm for aceclofenac and diclofenac, respectively. The method determined aceclofenac and diclofenac in concentration ranges of 2-10 and 1-9 micrograms spot-1 with mean percentage accuracy of 100.20 +/- 1.03 and 100.14 +/- 0.98 for pure drugs and 99.77 +/- 0.74 and 100.07 +/- 0.78 for laboratory-prepared mixtures, respectively. This method retains its accuracy in the presence of up to 80% degradation product for the studied drug. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The validity of the proposed methods was further assessed by applying a standard addition technique. The obtained results agreed statistically with those obtained by the reported method.

Investigation of ketoconazole copper(II) and cobalt(II) complexes and their spectrophotometric applications.

Ketoconazole, as a ligand, reacts quantitatively with copper(II) and cobalt(II) to form blue-colored, stable complexes in dichloromethane. These complexes can be spectrophotometrically measured at 720 and 612.5 nm in the case of Cu(II) or Co(II), respectively. Different factors affecting the reaction such as pH, reagent concentration, solvent effect, and time were studied. By using Job's method of continuous variation, the stoichiometry of the reaction was found to be in the ratio of 1:2, metal:drug, with Cu(II) and Co(II). The stability of the complexes formed was also studied. The reaction products were isolated for further investigation. The complexes have apparent molar absorptivities of 35.36 +/- 1.95 and 59.62 +/- 1.87 for Cu(II) and Co(II), respectively. Suggested procedures based on the stoichiometric reaction were successfully applied to the analysis of the pure drug and its pharmaceutical formulations. The validity of the procedures was further ascertained by the method of standard additions. The developed method was found to be simple, accurate, and precise when compared with the official method of the British Pharmacopoeia.

Bromometric determination of carbimazole.

Direct bromometric titration of carbimazole using N-bromosuccinimide (NBS) in the presence of methyl red as indicator and three indirect titrations using NBS, potassium bromate and dibromohydantoin (DBH) are developed. The direct procedure can be adopted for quantities of carbimazole ranging from 2-12 mg with mean accuracies of 100.2 +/- 0.5. The indirect procedures can be used for quantities of the drug ranging from 1-6 mg using NBS and DBH and 2-16 mg using potassium bromate with mean accuracies of 100.11 +/- 0.3, 100.49 +/- 0.31 and 100.26 +/- 0.51 respectively. The proposed procedures have been successfully applied for the analysis of the drug in tablet form and their validity has been checked using the standard addition technique. The reaction products were separated by TLC methods and their structure was elucidated using IR and NMR spectroscopy. The stoichiometry and the possible pathways of the reaction were postulated and presented.