Erratum: Synthesis and characterization of diorganotin(IV) complexes of Schiff bases with ONO‐type donors and crystal structure of [N‐(2‐hydroxy‐4‐nitrophenyl)‐3‐ethoxysalicylideneiminato]diphenyltin(IV)

The article referenced above was first published online on 30 August 2007 with incorrect pagination; the pagination has now been corrected online and in print. Copyright © 2007 John Wiley & Sons, Ltd.     

A Positive Doubly Power Bounded Operator with a Nonpositive Inverse Exists on any Infinite-dimensional AL-Space

In this paper we construct a positive doubly power bounded operator with a nonpositive inverse on an AL-space.     

X-ray fluorescence intensity distribution in circular specimens

Summary The relative X-ray fluorescence (XRF) intensities for annular source and various annular specimen are measured with a Ge-Li detection system and calculated by the Monte Carlo numerical techniques (MCNT).Kα X-ray intensities of annular specimens with different radii prepared from a pure-molybdenum foil are measured and it is seen that the measured values are in good agreement with the values calculated by MCNT. The variation of the fluorescence intensity due to the collimator radius is also studied. The differences between the MCNT and experimental results are discussed in terms of the possible sources of errors.     

Peak area determination and energy dependence of gamma- and X-ray peak tailing

Two analytical shape functions representing the shapes of - and characteristic X-ray photopeak sides obtained with a Ge(Li) detector are described. The photopeak centroid is accurately determined by using these functions. Energy dependence of photopeak tailing at the lower energy side of the photopeaks are obtained by the least-squares fitting method. The present method can be used for the analysis of partly overlapped photopeaks, one side of which is well resolved, with a sufficient accuracy.     

Measurement of L&agr; and Lß X-ray fluorescence cross sections in Er, Ta, W and Au by 16.896–59.543 keV photons

La and Lb X-ray fluorescence cross sections in Er, Ta, W and Au at excitation energies of 16.896, 22.581, 25.770, 32.890, 38.184, 43.949, 50.214 and 59.5 keV were investigated. Measurements were made using a low energy Si(Li) detector coupled to a model 4096 computerized multi-channel analyser. The experimental results were compared with the theoretically calculated values of L X-rays fluorescence cross sections and other experimental results. Good agreement was observed between experimental and theoretical values.     

Quantum calculations of vibrational harmonic energy transfer in collinear collisions of X2Y2 + A and X2Y2 + A2

Quantum calculations of translational-vibrational energy transfer in atom-four-atom and diatom-four-atom collinear collisions are reported. Energy transfer shows a strong dependence on the reduced mass of the collision system and on whether the incoming particle is an atom or a molecule. Atom-molecule collisions are more efficient for energy transfer purposes.     

Thermosensitive mucoadhesive gel formulation loaded with 5-Fu: cyclodextrin complex for HPV-induced cervical cancer

Human Papilloma Virus (HPV) infections are the major cause of cervical cancers. To achieve a better therapeutic efficacy and patient compliance in the treatment for HPV-induced cervical cancers, anticancer agent 5-fluorouracil has been formulated in a vaginal gel using the thermosensitive polymer Pluronic^® F127 together with alternative mucoadhesive polymers e.g., hyaluronic acid, Carbopol 934 and hydroxypropylmethylcellulose. To increase its aqueous solubility and to achieve the complete release of 5-FU from the gel, the drug was incorporated as its inclusion complex with 1:1 molar ratio with either β-cyclodextrin or hydroxypropyl-β-cyclodextrin. Following the characterization of drug:CD complexes, thermosensitive gel formulations containing different mucoadhesive polymers and the drug in free or complexed form were characterized in vitro by determining the gelation temperature and the rheological behavior of different formulations along with the in vitro release profiles of these formulations in pH 5.5 citrate buffer. It was observed that complexation with cyclodextrin accelerated the release of 5-FU with the exception of formulation containing Carbopol 934 as mucoadhesive polymer. As far as rheological properties are concerned, favorable thermosensitive in situ gelling properties were obtained with formulations containing HPMC as mucoadhesive polymer. Complete release of 5-FU from gels were obtained with both complexes of β-CD and HP-β-CD and cytotoxicity studies against HeLa human cervical carcinoma cells demonstrated that 1% 5-FU:CD complexes were equally effective as 1% free 5-FU indicating better therapeutic efficacy with lower dose.     

Selective LC Determination of Cabergoline in the Bulk Drug and in Tablets: In Vitro Dissolution Studies

Cabergoline (CAB) is an ergot alkaloid derivative with dopamine agonist activity. A novel, simple, and rapid stability-indicating high-performance liquid chromatographic (HPLC) method for assay of CAB in tablets has been developed and validated. Chromatography was performed on a 4.6 mm i.d. × 250 mm, 5 μm particle, cyano column with acetonitrile–10 mM phosphoric acid, 35:65 (v/v), containing 0.04% triethylamine, as mobile phase, at a flow rate of 1.0 mL min^?1, and UV detection at 280 nm. Response was a linear function of concentration in the range 0.1–4 μg mL^?1 (r ² = 0.9999). The recovery of the method was good (99.45%) and RSD values for intra-day and inter-day precision were 0.24–0.88% and 0.66–1.19%, respectively. The method can be used for quality-control assay of CAB in tablets, for stability studies, and for in vitro dissolution studies.     

Anomalous NMR behavior of meso compounds with remote stereogenic centers on addition of chiral shift reagent or chiral solvating agent

A problem has arisen in using chiral shift reagents (CSR) and chiral solvating agents (CSA) to determine meso and racemic forms of diastereoisomers in which the stereogenic centers of the molecules are separated by achiral spacers. It is found that NMR signals of both meso and racemic forms of diastereoisomers may exhibit doubling on addition of CSR/CSA, which means that unequivocal assignments cannot be made without characterizing the effects for separate meso and racemic forms; this is particularly important for additions of CSR/CSA at relatively low concentrations, which always result in the splitting of some NMR signals of diastereoisomers. The phenomenon is demonstrated in the (31)P NMR spectra of meso and racemic forms of three spermine-bridged gem-disubstituted cyclotriphosphazatrienes, 1a-c, and compared with analogous achiral molecules, the per-substituted spermine-bridged cyclotriphosphazatrienes 2a-d. As expected, only one set of (31)P NMR signals was observed for the achiral compounds 2a-d, even on addition of CSA. Two sets of (31)P NMR ABX multiplets corresponding to meso and racemic diastereoisomers were observed for compounds 1a-c; on addition of CSA, the signals of at least one of the multiplets for each compound separated into more than the expected groups of three lines with an intensity distribution of 2:1:1. To understand this phenomenon, the meso and racemic forms of 1a and 1b and the meso form of 1c have been separated and characterized by X-ray crystallography. On addition of CSA to the racemic forms of 1a and 1b, the (31)P NMR spectrum shows the expected doubling of signals, but, unexpectedly, the same is observed for each of the meso forms of 1a-c. Analogous results using both CSA and CSR have been obtained for the meso and racemic forms of the diastereoisomeric piperazine-bridged macrocyclic-phosphazene compound, 3, whereas no effect was observed for the two meso forms of the doubly bridged macrocyclic-phosphazene compound 4. The phenomenon of doubling of the (31)P NMR signals of the meso form of singly bridged cyclotriphosphazatrienes, 1a-c and 3, is explained by consideration of the equilibrium in solution of independent complexation of a chiral ligand with molecules that have two chiral cyclophosphazene moieties separated by an achiral spacer group. The results show that the stereogenicity of such diastereoisomeric molecules in solution cannot be characterized unequivocally by NMR measurements on addition of either CSR or CSA.