Ranitidini hydrochloridum - uspbpep.com

1 EUROPEAN PHARMACOPOEIA hydrochloride04/2005:0946 RANITIDINE HYDROCHLORIDER anitidini [2-[[[5-[(Dimethylamino)methyl]furan-2-y l]methyl]sulphan-yl]ethyl]-N -methyl-2-nitroethene-1,1-diamine : per cent to per cent (dried substance).CHARACTERSA ppearance: white or pale yellow, crystalline : freely soluble in water, sparingly soluble orslightly soluble in anhydrous ethanol, very slightly solublein methylene shows Infrared absorption spectrophotometry ( ).Comparison:ranitidine hydrochloride the spectra show differences, dissolve 10 mg of thesubstance to be examined and 10 mg of the referencesubstance separately in ml ofmethanol Rin anagate mortar.

2 Evaporate to dryness under a stream ofnitrogen R. Dry the residues under vacuum for 30 3 drops ofliquid paraffin Rto the residues andtriturate until the mull shows a milky the mulls between 2 plates transparent toinfrared radiation and record new It gives reaction (a) of chlorides ( ).TESTSS olution S. Dissolve g incarbon dioxide-free water of solution. Solution S is clear ( )andnotmore intensely coloured than reference solution BY5( ,Method II).pH( ): to for solution substances. Liquid chromatography ( ).Buffer solution. Dissolve g ofpotassium dihydrogenphosphate Rin 950 ml ofwater sodium hydroxide solution Rand dilute to 1000 mlwithwater solution.

3 Dissolve 13 mg of the substance to beexamined in mobile phase A and dilute to 100 ml with mobilephase solution (a). system suitability CRS(ranitidine with impurities A,D and H) in mobile phase A and dilute to 50 ml with mobilephase solution (b). ml with mobile phase solution (c). Dissolve the contents of a vial ofranitidine impurity J CRSin 2 ml of mobile phase A. ml of the solution to 50 ml with mobile phase A. : size:l= m, = mm, stationary phase:end-capped polar-embeddedoctadecylsilyl amorphous organosilica polymer R( m), temperature:35 phase: mobile phase A:acetonitrile R, buffer solution (2:98V/V), mobile phase B:acetonitrile R, buffer solution(22:78V/V),Time(min)Mobile phase A(per centV/V)Mobile phase B(per centV/V)0-10100 00 10010 - 15010015 - 160 100100 016 - 201000 Flow : spectrophotometer at 230.

4 10 l of the test solution, reference solutions (a),(b) and (c) and mobile phase A as a retentionwith reference to ranitidine (retentiontime = about min): impurity H = about ;impurity G = about ; impurity F = about ;impurity B = about ; impurity C = about ;impurity E = about ; impurity D = about ;impurity J = about ; impurity I = about ;impurity A = about suitability: resolution: minimum between the peaks due toimpurity J and ranitidine in the chromatogram obtainedwith reference solution (c), the chromatogram obtained with reference solution (a)is similar to the chromatogram supplied withranitidinefor system suitability CRS, the chromatogram obtained with the blank does notshow any peak with the same relative retention as thepeak due to impurity A in the chromatogram obtainedwith reference solution (a).

5 Limits: correction factor: for the calculation of content, multiplythe peak area of impurity J by 2, impurity A: not more than times the area of theprincipal peak in the chromatogram obtained withreference solution (b) ( per cent), impurities B, C, D, E, F, G, H, I, J:foreachimpurity,not more than times the area of the principal peak inthe chromatogram obtained with reference solution (b)( per cent), any other impurity: for each impurity, not morethan times the area of the principal peak in thechromatogram obtained with reference solution (b)( per cent), sum of impurities other than area of the principal peak in the chromatogramobtained with reference solution (b) ( per cent), disregard limit: times the area of the principal peakin the chromatogram obtained with reference solution (b)( per cent); disregard any peak due to the (1)applytoallmonographsandothertexts3001 RibavirinEUROPEAN PHARMACOPOEIA metals( ): maximum 20 g complies with limit test C.

6 Prepare the referencesolution using 2 ml oflead standard solution (10 ppm Pb) on drying( ): maximum per cent, determinedon g by drying under high vacuum at 60 ash( ): maximum per cent, determinedon g in 35 ml ofwater M sodium hydroxide, determining the end-pointpotentiometrically ( ). M sodium hydroxideis equivalent to mgof airtight container, protected from impurities: A, B, C, D, E, F, G, H, I, detectable impurities: ,N -bis[2-[[[5-[(dimethylamino)methyl]furan -2-yl]methyl]sulphanyl]ethyl]-2-nitroeth ene-1,1-diamine,B. R = S-CH2-CH2-NH2: 2-[[[5-[(dimethylamino)methyl]furan-2-yl ]methyl]sulphanyl]ethanamine,D.

7 R = S-CH2-CH2-NH-CO-CH2-NO2:N-[2-[[[5-[(dime thyl-amino)methyl]furan-2-yl]methyl]sulp hanyl]ethyl]-2-ni-troacetamide,F. R = OH: [5-[(dimethylamino)methyl]furan-2-yl]met hanol, [2-[[[5-[(dimethylamino)methyl]furan-2-y l]methyl]sulphinyl]ethyl]-N -methyl-2-nitroethene-1,1-diamine, [2-[[[5-[(dimethyloxidoamino)methyl]fura n-2-yl]methyl]sulphanyl]ethyl]-N -methyl-2-nitroethene-1,1-diamine,G. 3-(methylamino)-5,6-dihydro-2H-1,4-thiaz in-2-one-oxime, ,I. 2,2 -methylenebis[N-[2-[[[5-[(dimethylamino) methyl]furan-2-yl]methyl]sulphanyl]ethyl ]-N -methyl-2-nitroethene-1,1-diamine],J.

8 1,1 -N-[methylenebis(sulphanediylethylene)]b is(N -methyl-2-nitroethene-1,1-diamine), -D-Ribofuranosyl-1H-1,2, : per cent to per cent (dried substance).CHARACTERSA ppearance: white or almost white, crystalline : freely soluble in water, slightly soluble in ethanol(96 per cent), slightly soluble or very slightly soluble inmethylene the information section on general monographs (cover pages)