Simultaneous determination of some active ingredients in cough-cold syrups by gas-liquid chromatography

A simple, efficient and accurate gas-liquid chromatography (GLC) method for the simultaneous determination of eight active ingredients in cough-cold syrups has been developed. The active ingredients under study were bromhexine, chlorpheniramine, codeine, dextromethorphan, diphenhydramine, ephedrine/pseudoephedrine, guaiphenesin and papaverine. Before injection, the active ingredients were first separated, from the excipients present in the cough-cold syrups, with chloroform, from alkaline medium. They were then separated by GLC on a glass column (5 ft x 2 mm i.d.) packed with 3% of OV-25 supported on Supelcoport (80-100 mesh). The column temperature was maintained at 170 degrees C for 1 min, then programmed to 265 degrees C at a rate of 10 degrees C min-1, and maintained at this temperature for 10 and 1 min, respectively, for samples with and without papaverine. The flow-rate of the nitrogen carrier gas was 30 ml min-1. A flame-ionisation detector was used for detection, and clomipramine hydrochloride was used as the internal standard. The recoveries of the drugs ranged from 96.0 to 99.7%, and the relative standard deviations for ten replicate determinations ranged from 0.49 to 4.7%. Results are reported for nine commercially available cough-cold syrups.     

Covalent crosslinking of 1-D photonic crystals of microporous Si by hydrosilylation and ring-opening metathesis polymerization

Free-standing porous Si multilayer dielectric mirrors, prepared by electrochemical etching of crystalline Si, are treated with a ruthenium ring-opening metathesis polymerization (ROMP) catalyst followed by norbornene to produce flexible, stable composite materials in which poly(norbornene) is covalently attached to the porous Si matrix.     

Synthesis and structural characterization of mono- and bisfunctional o-carboranes

Functionalized o-carboranes are interesting ligands for transition metals. Reaction of LiC2B10H11 with Me2NCH2CH2Cl in toluene afforded 1-Me2NCH2CH2-1,2-C2B10H11 (1). Treatment of 1 with 1 equiv. of n-BuLi gave [(Me2NCH2CH2)C2B10H10]Li ([1]Li), which was a very useful synthon for the production of bisfunctional o-carboranes. Reaction of [1]Li with RCH2CH2Cl afforded 1-Me2NCH2CH2-2-RCH2CH2-1,2-C2B10H10 (R = Me2N (2), MeO (3)). 1 and 2 were also prepared from the reaction of Li2C2B10H10 with excess Me2NCH2CH2Cl. Treatment of [1]Li with excess MeI or allyl bromide gave the ionic salts, [1-Me3NCH2CH2-2-Me-1,2-C2B10H10][I] (4) and [1-Me2N(CH2=CHCH2)CH2CH2-2-(CH2=CHCH2)-1,2-C2B10H10][Br] (6), respectively. Interaction of [1]Li with 1 equiv. of allyl bromide afforded 1-Me2NCH2CH2-2-(CH2=CHCH2)-1,2-C2B10H10 (5). Treatment of [1]Li with excess dimethylfulvene afforded 1-Me2NCH2CH2-2-C5H5CMe2-1,2-C2B10H10 (7). Interaction of [1]Li with excess ethylene oxide afforded an unexpected product 1-HOCH2CH2-2-(CH2=CH)-1,2-C2B10H10 (8). 1 and 3 were conveniently converted into the corresponding deborated compounds, 7-Me2NHCH2CH2-7,8-C2B9H11 (9) and 7-Me2NHCH2CH2-8-MeOCH2CH2-7,8-C2B9H10 (10), respectively, in MeOH-MeOK solution. All of these compounds were characterized by various spectroscopic techniques and elemental analyses. The solid-state structures of 4 and 6-10 were confirmed by single-crystal X-ray analyses.