1013-1022.qxd

Abstract: The methods for controlling volatile impurities, including reagent and starting material, in Nepafenac active pharmaceutical ingredient, are reported. The proposed methods were developed using gas chromatography (GC) and gas chromatography with headspace injection (GC-HS) and validated according to the requirements of the ICH (International Conference of Harmonization) validation guidelines Q2R1 and the guideline for residual solvents Q3C

A Validated TLC-Densitometric Method for the Determination of Mesterolone in Bulk Material and in Tablets

Mesterolone is a synthetic androgenic steroid indicating a weak anabolic activity. A new, simple in use, and economical TLC-densitometric method in normal phase system (NP-TLC) has been developed and validated for the identification and quantitative determination of mesterolone in bulk drug and in tablet formulation. NP-TLC analysis was performed on aluminium plates precoated with silica gel 60F254 as the stationary phase using chloroform-acetone (40 : 10, v/v) as mobile phase. Densitometric analysis was carried out at λ=745 nm after staining with phosphomolybdic acid. These conditions were found to give visible (dark blue) spot and sharp peak, respectively, for mesterolone at RF  0.75±0.02 and enabled satisfactory separation of mesterolone from its related substance (potential impurity). The proposed NP-TLC-densitometric method was validated for specificity, linearity, precision, accuracy, robustness, and sensitivity according to ICH guideline and other validation requirements. The limit of detection (LOD) and limit of quantification (LOQ) were 61.0 ng·spot−1 and 184.0 ng·spot−1, respectively. The percent content of mesterolone in marketed tablet formulation was found to be 99.40% of label claim. The developed TLC-densitometric method can be successfully used in quality control of mesterolone in bulk material and also tablet formulation

Invasive electrophysiologySpectrum of atrial arrhythmias from the right upper pulmonary vein – successful isolation of the arrhythmogenic focus by RF ablation of atriovenous breakthroughs – a case report

We present a case of a 19-year-old patient with incessant arrhythmias originating from the right upper pulmonary vein (RUPV) presenting as frequent premature beats, automatic rhythms mimicking sinus rhythm (SR) and pulmonary vein tachycardias. Morphology of P’ wave resembled sinus P wave due to relatively short distance of the ectopic focus from the sinus node. Occasionally, when discharges from the focus were relatively slow (800-500 ms) and regular it was mimicking sinus rhythm. Activation preceding P’ wave during arrhythmia was recorded in RUPV as well as in superior vena cava. In this paper we discuss our approach that allowed localising the arrhythmogenic focus in the RUPV. After isolation of the RUPV sinus rhythm was restored with tachycardia at a cycle length of 320 ms continuing in the isolated vein

Synthesis and Biological Evaluation of New Amino Acid and Dipeptide Derivatives of Neocryptolepine as Anticancer Agents

The syntheses of neocryptolepine derivatives containing an amino acid or a dipeptide at the C-9 position and their evaluation for antitumor activity in vitro and in vivo are reported. To establish the influence of an amino acid or a peptide on the physicochemical properties of 5<i>H</i>-indolo­[2,3-<i>b</i>]­quinoline (DiMIQ), lipophilic and hemolytic properties were investigated. Most of the compounds displayed a high antiproliferative activity in vitro and strongly inhibited growth of tumor in mice compared to cyclophosphamide. The attachment of the hydrophilic amino acid or the peptide to the hydrophobic DiMIQ increased its hydrophilic properties and decreased its hemolytic activity. The glycylglycine conjugate (<b>7a</b>) was the most promising derivative. It strongly inhibited the growth of the tumor in mice (at dose 50 mg kg^–1 day^–1 it inhibited the tumor growth by 46–63% on days 11–16 and by 29–43% on days 18–23) and significantly decreased hemolytic activity and lowered the in vivo toxicity compared to DiMIQ