Mohamed A. F. Elmosallamy

LC and TLC determination of cinnarizine in pharmaceutical preparations and serum

New high performance liquid chromatography (HPLC) and thin layer densitometry (TLC) methods are developed for quantification of cinnarizine in dosage forms in the presence of its photo-degradation products and related substances and in the presence of its metabolites in serum. Mobile phases consisting of benzene-methanol-formic acid (80:17:3) and methanol-acetate buffer of pH 4 (70:30) are satisfactorily used for resolution of cinnarizine from associated substances by TLC and HPLC techniques, respectively. The lower detection limits are 16 and 10 ng microl(-1) of cinnarizine with standard deviations of 1.3 and 1.1% with TLC and HPLC, respectively. The methods are used for assessment of drug purity, stability, bioavailability, bioequivalency and tablet dissolution rate. Four cinnarizine related substances and six drug degradation products are isolated and identified by infrared and mass spectrometry. The results obtained by both techniques are in good agreement and offer the advantages of reproducibility and accuracy.

Determination of cinnarizine in pharmaceutical preparations by spectrophotometry, atomic absorption spectrometry and potentiometry

New methods are developed for the determination of cinnarizine in various dosage forms. They are based on the reaction of cinnarizinium cation with cobalt tetrathiocyanate anion, whereby a sparingly soluble blue 2∶1 drug: reagent ion-pair complex is quantitatively formed. The complex is (a) extracted with nitrobenzene and spectrophotometrically measured at 622 nm; (b) extracted with nitrobenzene and nebulized in an air-acetylene flame for atomic absorption spectrometric monitoring of cobalt at 242.5 nm; and (c) dispersed in a PVC membrane plasticized with 2-nitrophenyloctyl ether and used as a sensor for direct potentiometric determination of the drug. Optimum reaction conditions and performances of the three analytical techniques are evaluated and compared. At the 25 mg level of cinnarizine, the three methods give results with equal accuracy and precision. The average recovery is 98–99% of the nominal and the mean standard deviation is 0.7%. No significant interferences are caused by drug excipients and diluents.

Miniaturized Verapamil Soild-State Potentiometric Sensors Based on Native Ionic Polymers

Abstract. Novel miniaturized carboxylated poly(vinyl chloride) and poly fluoro sulfonate (Nafion) matrix membrane sensors in an all-solid state graphite support were developed, electrochemically evaluated and used for the assay of verapamil drug. These sensors incorporate the native polymers without plasticizer and/or drug-ion pair complex. Upon soaking these sensors in verapamil test solution, electroactive self regenerated membranes are formed and a near-Nernstian potentiometric response is induced for verapamil over the concentration range 1×10−2–1×10−5 M with a cationic slope of 56–57 mV decade−1 of concentration. Inherent advantages of these sensors include fast response (<10 s), long life time (>6 months), good thermal stability (up to 60 °C), high sensitivity (down to 1 μg ml−1), extended working pH range (2–8) and reasonable selectivity. Verapamil could be determined in various dosage forms with an average recovery of 98.8% (st.dev. 0.8%) of the nominal concentration without any significant interferences from various excipients and diluents commonly used in drug formulations.