W.L. Wilson

Nuclear magnetic resonance identification and estimation of solvent residues in cocaine

Abstract Nuclear magnetic resonance spectroscopy was used to determine solvent residues in illicit cocaine exhibits. An internal standard was employed for the quantitative estimation of each of the five most common solvents found in exhibits: benzene, toluene, acetone, methyl ethyl ketone and ethyl ether. Methylene chloride and ethyl acetate also were detected in cocaine exhibits for the first time.

Isolation and identification of a fluorophore from ampicillin degradation.

A fluorescent impurity in ampicillin has been isolated and identified as 2‐hydroxy‐3‐phenyl‐pyrazine. The product is formed under acidic conditions similar to those employed in some fluorometric assay procedures. The mechanism of the reaction is proposed to involve cyclization by condensation of the penilloaldehyde of ampicillin. The structure was confirmed by independent synthesis.

Chromatographic differentiation of erythromycin and its esters

Abstract A rapid identification method for the detection and quality control of the erythromycin antibiotics is described. Thin-layer chromatography on sodium acetate-buffered silica gel plates enabled the differentiation of erythromycin, erythromycin estolate and erythromycin ethyl succinate from some degradation products and pharmaceutical excipients. The comparative behavior of twenty other antibiotics under these conditions is also presented.

High Performance Liquid Chromatographic Analysis of Rifampin and Related Impurities in Pharmaceutical Formulations

Abstract High pressure liquid chromatography was employed for the assay of rifampin in capsules. A reverse phase RP-2 column and a mobile phase of 48% methanol, 5% tetrahydrofuran and 47% 0.05 M ammonium formate (pH 7.3) were used with detection at 254 nm. Rifampin was separated from all its major degradation products and quantitated.

High Performance Liquid Chromatographic Analysis of Penicillin V Solid Dosage Forms

Abstract An isocratic high performance liquid chromatographic (HPLC) method for the determination of Penicillin V in solid dosage forms is described. A reverse phase RP-8 column and a mobile phase of 52% methanol in 0.05 M phosphate buffer (pH 3.3) were employed. Detection was effected at 254 nm. The results obtained are compared with those from the iodometric method.

A Direct Synthesis of O6-Monoacetylmorphine from Morphine

ABSTRACTO6-Monoacetylmorphine was synthesized directly in good yield from morphine with glacial acetic acid using sulphuric acid as a catalyst. The product was characterized by PMR, IR, MS, and elemental microanalysis. This successful synthesis of O6-monoacetylmorphine from morphine shows that this compound can be included under the Narcotic Control Act as a regulated substance for legal purposes.