PIRACETAM - uspbpep.com

1 PiracetamEUROPEAN PHARMACOPOEIA R1 = R2 = H: (3S,4R)-3-[(1,3-benzodioxol-5-yloxy)meth yl]-4-phenylpiperidine (desfluoroparoxetine), ,R2=CH2-C6H5:(3S,4R)-3-[(1,3-benzodioxol -5-yloxy)methyl]-1-benzyl-4-(4-fluorophe nyl)piperidine(N-benzylparoxetine),F. R1=H,R2=CH2-C6H5:(3S,4R)-3-[(1,3-benzodi oxol-5-yloxy)methyl]-1-benzyl-4-phenylpi peridine(N-benzyldesfluoroparoxetine),B. 1,3-benzodioxol-5-ol (sesamol),D. (3R,4S)-3-[(1,3-benzodioxol-5-yloxy)meth yl]-4-(4-fluorophenyl)piperidine ((+)-trans-paroxetine),E. (3RS,4RS)-3-[(1,3-benzodioxol-5-yloxy)me thyl]-4-(4-fluorophenyl)piperidine (cis-paroxetine),G. 4-(4-fluorophenyl)-1-methyl-1,2,3,6-tetr ahydropyridine,H. R = CH2-C6H5:[(3S,4R)-1-benzyl-4-(4-fluoroph enyl)-piperidin-3-yl]methanol,I. R = H: [(3S,4R)-4-(4-fluorophenyl)piperidin-3-y l]methanol,J. (3S,4R)-3-[(1,3-benzodioxol-5-yloxy)meth yl]-4-(4 -fluorobiphenyl-3-yl) (2-Oxopyrrolidin-1-yl) : per cent to per cent (dried substance).

2 CHARACTERSA ppearance: white or almost white, :freelysolubleinwater,solubleinethanol (96 percent).It shows absorption spectrophotometry ( ).Comparison: PIRACETAM the spectra obtained in the solid state show differences,dissolvethesubstancetobeexam inedandthereferencesubstance separately inethanol (96 per cent) R,evaporateto dryness on a water-bath and record new spectra usingthe of ( )andcolourless ( , Method II).Dissolve g inwater Rand dilute to 10 ml with the ( ).Test solution (a). Dissolve mg of the substance to beexamined in a mixture of 10 volumes ofacetonitrile R1and90 volumes ofwater Rand dilute to ml with the samemixture of solution (b). Dilute ml of test solution (a) ml with a mixture of 10 volumes ofacetonitrile R1and90 volumes ofwater the information section on general monographs (cover pages)EUROPEAN PHARMACOPOEIA 80 Reference solution (a).

3 Dissolve5mgofthesubstancetobe examined and 10 l of2-pyrrolidone Rin a mixture of10 volumes ofacetonitrile R1and 90 volumes ofwater Rand dilute to ml with the same mixture of solution (b). Dilute ml of test solution (a) R1and 90 volumes ofwater R. Dilute ml of this solutionto ml with a mixture of 10 volumes ofacetonitrile R1and 90 volumes ofwater solution (c). Dissolve mg ofpiracetam CRSin a mixture of 10 volumes ofacetonitrile R1and 90 volumesofwater Dilute ml of this solution to ml with amixture of 10 volumes ofacetonitrile R1and 90 volumesofwater : size:l= , = , stationary phase:end-capped octadecylsilyl silica gelfor chromatography R(5 m).Mobile phase:mix10volumesofacetonitrile R1and90 volumes of a g/l solution ofdipotassium hydrogenphosphate R; phosphoric acid : spectrophotometer at 205 : 20 l of test solution (a) and reference solutions (a)and (b).

4 Run time: 8 times the retention time of retentionwith reference to PIRACETAM (retention time = about 4 min): impurity D = about ;impurity A = about ; impurity B = about ;impurity C = about suitability: reference solution (a): resolution: minimum between the peaks due topiracetam and impurity A, symmetry factor: maximum for the peak due : impurities A, B, C, D: for each impurity, not more thanthe area of the principal peak in the chromatogramobtained with reference solution (b) ( per cent), unspecified impurities: for each impurity, not morethan the area of the principal peak in the chromatogramobtained with reference solution (b) ( per cent), total: not more than 3 times the area of the principal peakin the chromatogram obtained with reference solution (b)( per cent), disregard limit: times the area of the principal peakin the chromatogram obtained with reference solution (b)( per cent).

5 Heavy metals( ): maximum 10 g in 20 ml ofwater with test A. Prepare the reference solution usinglead standard solution (1 ppm Pb) on drying( ): maximum per cent, determinedon g by drying in an oven at 100-105 ash( ): maximum per cent, determinedon chromatography ( ) as described in the test forrelated substances with the following : test solution (b) and reference solution (c).Calculate the percentage content of C6H10N2O2from the areasof the peaks and the declared content ofpiracetam from impurities: A, B, C, R = H: pyrrolidin-2-one (2-pyrrolidone),B. R = CH2-CO-O-CH3: methyl (2-oxopyrrolidin-1-yl)acetate,C. R = CH2-CO-O-C2H5: ethyl (2-oxopyrrolidin-1-yl)acetate,D. R = CH2-CO2H: (2-oxopyrrolidin-1-yl)acetic :0428 POLYSORBATE 80 Polysorbatum 80 DEFINITIONM ixture of partial esters of fatty acids, mainlyOleicacid (0799), with sorbitol and its anhydrides ethoxylatedwith approximately 20 moles of ethylene oxide for each moleof sorbitol and sorbitol : oily, yellowish or brownish-yellow, clear orslightly opalescent : dispersible in water, in anhydrous ethanol, inethyl acetate and in methanol, practically insoluble in fattyoils and in liquid : about 400 mPa s at 25 identication: A, :B,C,D, Infrared absorption spectrophotometry ( ).

6 Comparison:Ph. Eur. reference spectrum ofpolysorbate (seeTests).C. Saponification value (see Tests).D. Composition of fatty acids (see Tests).E. Dissolve g in 5 ml ofmethylene chloride thiocyanate Rand g ofcobalt nitrate with a glass rod. The solution becomes value( ): maximum g in 50 ml of the prescribed mixture of value( , Method A): 65 to g into a 100 ml beaker, dissolve withglacialacetic acid Rand dilute to 20 ml with the same solvent. Add1mlofsaturated potassium iodide solution Rand allow tostand for 1 min. Add 50 ml ofcarbon dioxide-free water Rand a magnetic stirring bar. Titrate M sodiumGeneralNotices(1)applytoallmonogra phsandothertexts4007