A highly sensitive gas chromatographic assay is described for the simultaneous determination of gallopamil, a calcium channel blocking agent, and its major metabolite, norgallopamil. A multi-step extraction procedure is employed followed by on-column capillary gas chromatographic analysis using nitrogen-selective detection. Acetylation of norgallopamil is performed to enable accurate quantifica...

We describe a "high-performance" liquid-chromatographic procedure for measuring 3-methoxy-4-hydroxymandelic acid (vanillylmandelic acid) in urine. The compound is quantitatively extracted from urine by use of an automated system, including an anion-exchange resin. After elution from the resin and concentration by air drying, the urine extract is chromatographed on an octyl silica column, with u...

We developed a reversed-phase chromatographic procedure for detecting benzodiazepines and other drugs in serum. A liquid-liquid extraction step with hexane/ethyl acetate isolates the drugs from serum; absolute recoveries are generally greater than 85%. Reconstituted extracts are chromatographed on a 4-microns (particle size) C18 column; 14 drugs and an internal standard (flunitrazepam) are sepa...

a new facile route for synthesis of 3- (aryl) -8, 9- di (alkyl) thieno [3,2-e] [1,2,4] triazolo pyrimidines derivative from the same starting material, 2- amino - 4,5 -di (alkyl) thiophene-3- carboxamide, has been developed through heterocyclization of the corresponding arylidene-hydrazino -5,6 -di (alkyl) thieno [2,3-d] pyrimidine under refluxing condition with acetic anhydride followed by air...

an efficient and simple one-pot approach for the synthesis of 3,4-dihydropyrimidin-2-(1h)-one derivatives using antimony trichloride (sbcl3) as a mild catalyst by means of three-component biginelli reaction between β-keto esters, aldehyde derivatives and urea/thiourea under thermal and solvent-free conditions with excellent yields and short reaction times is reported. this methodology offers se...

We describe a circular (radial) thin-layer chromatographic procedure for separating urinary oligosaccharides. Results were better than those obtained by a single linear development. Bands and specific patterns were finely resolved for various known oligosaccharidoses. The procedure provides a simple means of screening for these disorders.