Analytical Profiles of Drug Substances, Excipients, and by Klaus Florey (editor)

By Klaus Florey (editor)

Even though the reliable compendia outline a drug substance as to identification, purity, energy, and caliber, they often don't offer different actual or chemical information, nor do they checklist equipment of synthesis or pathways of actual or organic degradation and metabolism. Such details is scattered throughout the medical literature and the records of pharmaceutical laboratories. "Analytical Profiles of Drug components" brings this data jointly into one resource.

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5, 91 (1984). 30. R. M. G. Sankey, J. Pharm. , 33, 386 (1980). 31. J. J. J. Smith, B r . J. C l i n . , 9, 395 (1980). 32. J. A. A. C. H a r r i s o n , C l i n . Pharmacol. T h e r . , 22, 557 (1977). 33. B. F l o u v a t , A . P. Chau, M. V i a l l e t , X . Andre-Fouet, R. Woehrle and J. Gregoire, E u r . J. C l i n . , 19, 287 (1981). 34. A. Gulaid, I . M . M. W. Lewellen, E. Roberts, M. Sankey, J. Smith, R. J. Thomas, B r . J. C l i n . , 5, 261 (1978). 35. W. K i r c h , H. K o h l e r , G.

5: 13 C - NMR NOISE- DECOUPLED SPECTRUM OF AMOBARBITAL u) f w Q m Y) kL F i g . 13CNMR OFF- RESONANCE SPECTRUM OF AMOBARBITAL fn fn zcd .. r. 43 AMOBARBITAL Scheme: CH2ClCOOH + Monochloroacetic acid CH2CNCWH NaCN CH2CNCOOH Sod. cyanide ZC2HSOH * HC1 + cooc2q I P + - COOCZH5 I I COOC2Hs I + COOC2H5 + f“Z COOC2Hs NH4C1 Diethyl malonate COOC2Hs I I + 4 H2 COK2Hs Sodio-malonic ester COOC2Hs C H HC’ + NaBr COOC2Hs HCNa Cyanoacetic acid HCNa Na NaCl I C2HgBr ___f I COOC2H5 Ethyl bromide Diethyl ester of Ethyl malonic acid Diethyl ester o f ethyl-isopentyl malonic acid.

5 cm) of sephadex G 25 (particle size 100-300 pm) and elute with 0 . 0 1 M - H2S04. Discard the first 150 ml of eluate. Collect the next 200 ml, and extract the barbiturates therefrom into CHC13 ( 3 X 50 ml). r. spectrum from 4000 to 700 cm-l. AMOBARBITAL 49 Amylobarbitone can be identified from absorption bands in the regions 3200 to 3000 cm-l. Moss et al. (16) also analysed the drug using infrared spectroscopy. 1 PaDer ChromatoRraDhg Some paper chromatographic systems used for the determination of amobarbital have been summarised in Table ( 6 ) .

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