Amikacini sulfas - uspbpep.com

1 EUROPEAN PHARMACOPOEIA sulphateReference solution (c).Dissolve 5 mg ofamikacin CRSand5mgofamikacin impurity A CRSinwater Rand dilute to50 ml with the same solvent. Then prepare as prescribed fortest solution (a).Blank as described for test solution (a)using ml ofwater : size:l= , = ; stationary phase:octadecylsilyl silica gel forchromatography R(5 m); temperature:30 phase: mix 30 volumes of a g/l solution ofpotassium dihydrogen phosphate R, 22 g/l solution ofpotassium hydroxide R,and70volumesofmethanol rate:1 : spectrophotometer at 340 : 20 l of test solution (a) and reference solutions (a)and (c).Run time: 4 times the retention time of suitability: reference solution (c): resolution: minimum between the peaks due toamikacin and impurity A (see Figure ).Limits: impurity A: not more than the area of the principal peakin the chromatogram obtained with reference solution (a)(1 per cent); any other impurity:foreachimpurity,notmorethan times the area of the principal peak in thechromatogram obtained with reference solution (a)( per cent); sum of impurities other than area of the principal peak in the chromatogramobtained with reference solution (a) ( per cent); disregard limit: times the area of the principal peakin the chromatogram obtained with reference solution (a)( per cent); disregard any peak due to the ( ): maximum per cent, determined ash( )): maximum per cent, determinedon chromatography ( ) as described in the test forrelated substances with the following : test solution (b) and reference solution (b).

2 System suitability: repeatability: maximum relative standard deviation per cent after 6 injections of reference solution (b).Calculate the percentage content of C22H43N5O13from thedeclared content ofamikacin ,R2=acyl:4-O-(3-amino-3-deoxy- -D-glucopyranosyl)-6-O-(6-amino-6-deoxy- -D-glucopyranosyl)-1-N-[(2S)-4-amino-2-h ydroxybutanoyl]-2-deoxy-L-streptamine, ,R3=H:4-O-(3-amino-3-deoxy- -D-glucopyranosyl)-6-O-(6-amino-6-deoxy- -D-glucopyranosyl)-1,3-N-bis[(2S)-4-amin o-2-hydroxybutanoyl]-2-deoxy-L-streptami ne, ,R3=acyl:4-O-(6-amino-6-deoxy- -D-glucopyranosyl)-6-O-[3-[[(2S)-4-amino -2-hydroxybutanoyl]amino]-3-deoxy- -D-glucopyranosyl]-2-deoxy-D-streptamine , :1290corrected SULPHATEA mikacini sulfasC22H47N5O21S2Mr782[39831-55-5]DEFI NITION6-O-(3-Amino-3-deoxy- -D-glucopyranosyl)-4-O-(6-amino-6-deoxy- -D-glucopyranosyl)-1-N-[(2S)-4-amino-2-h ydroxybutanoyl]-2-deoxy-D-streptamine substance obtained from kanamycin product derived from a fermentation : per cent to per cent (dried substance).

3 : freely soluble in water, practically insoluble inacetone and in ethanol (96 per cent).IDENTIFICATIONA. Infrared absorption spectrophotometry ( ).Comparison:amikacin sulphate Thin-layer chromatography ( ).GeneralNotices(1)applytoallmonographsa ndothertexts1161 Amikacin sulphateEUROPEAN PHARMACOPOEIA solution. Dissolve 25 mg of the substance to beexamined inwater Rand dilute to 10 ml with the solution (a). Dissolve 25 mg ofamikacinsulphate CRSinwater Rand dilute to 10 ml with thesame solution (b).Dissolve 5 mg ofkanamycinmonosulphate CRSin 1 ml of the test solution and diluteto 10 ml withwater :TLC silica gel plate phase:thelowerlayerofamixtureofequal volumes ofconcentrated ammonia R,methanol Randmethylene chloride :5 :spraywithninhydrin solution R1and heatat110 suitability: reference solution (b): the chromatogram shows 2 clearly separated : the principal spot in the chromatogram obtainedwith the test solution is similar in position, colour andsize to the principal spot in the chromatogram obtainedwith the reference solution (a).

4 C. It gives reaction (a) of sulphates ( ).TESTSpH( ): to g incarbon dioxide-free water Rand dilute to10 ml with the same optical rotation( ): + 76 to + 84 (driedsubstance).Dissolve g inwater Rand dilute to ml with thesame ( ).Maintain the solutions at 10 solution (a).Dissolve g of the substanceto be examined inwater Rand dilute to ml withthe same solvent. In a ground-glass-stoppered vial, ,4,6-trinitrobenzene sulphonic acid Rand close the vial tightly. Shake vigorously for30 s and heat on a water-bath at 75 C for 2 h. Cool in coldwaterfor2minandadd2mlofglacial acetic acid for 30 solution (b). Dissolve mg of the substance to beexamined inwater Rand dilute to ml with the samesolvent. Then prepare as prescribed for test solution (a).Reference solution (a). Dissolve mg ofamikacinimpurity A CRSinwater Rand dilute to ml with thesame solvent. Then prepare as prescribed for test solution (a).Reference solution (b).Dissolve mg ofamikacinsulphate CRSinwater Rand dilute to ml with the samesolvent.

5 Then prepare as prescribed for test solution (a).Figure Chromatogram for the test for related substances of amikacin sulphate1162 See the information section on general monographs (cover pages)EUROPEAN PHARMACOPOEIA hydrochlorideReference solution (c).Dissolve 5 mg ofamikacinsulphate CRSand 5 mg ofamikacin impurity A CRSinwater Rand dilute to 50 ml with the same solvent. Thenprepare as prescribed for test solution (a).Blank solution. Prepare as described for test solution (a)using ml ofwater : size:l= , = ; stationary phase:octadecylsilyl silica gel forchromatography R(5 m); temperature:30 phase: mix 30 volumes of a g/l solution ofpotassium dihydrogen phosphate R, 22 g/l solution ofpotassium hydroxide R,and70volumesofmethanol rate:1 : spectrophotometer at 340 : 20 l of test solution (a) and reference solutions (a)and (c).Run time: 4 times the retention time of suitability: reference solution (c): resolution: minimum between the peaks due toamikacin and impurity A (see Figure ).

6 Limits: impurity A: not more than the area of the principal peakin the chromatogram obtained with reference solution (a)( per cent); any other impurity:foreachimpurity,notmorethan times the area of the principal peak in thechromatogram obtained with reference solution (a)( per cent); sum of impurities other than times the area of the area of the principal peak inthe chromatogram obtained with reference solution (a)( per cent); disregard limit: times the area of the principal peakin the chromatogram obtained with reference solution (a)( per cent); disregard any peak due to the blank andany peak eluting before the principal : per cent to per cent (dried substance).Dissolve g in 100 ml ofwater Rand adjust the solutionto pH 11 usingconcentrated ammonia M barium chlorideand about mg ofphthaleinpurple M sodium edetateadding 50 mlofethanol (96 per cent) Rwhen the colour of the solutionbegins to change and continue the titration until theviolet-blue colour M barium chlorideis equivalent to mg ofsulphate (SO4).

7 Loss on drying( ): maximum per cent, determinedon g by drying in an oven at 105 C at a pressure notexceeding kPa for 3 ( ). If intended for use in the manufactureof parenteral dosage forms without a further appropriateprocedure for the removal of pyrogens, it complies with thetest for pyrogens. Inject per kilogram of the rabbit s mass5 ml of a solution containing 25 mg of the substance to beexamined inwater for injections chromatography ( ) as described in the test forrelated substances with the following : test solution (b) and reference solution (b).System suitability: repeatability: maximum relative standard deviation per cent after 6 injections of reference solution (b).Calculate the percentage content of C22H47N5O21S2from thedeclared content ofamikacin sulphate the substance is sterile, store in a sterile, airtight,tamper-proof ,R2=acyl:4-O-(3-amino-3-deoxy- -D-glucopyranosyl)-6-O-(6-amino-6-deoxy- -D-glucopyranosyl)-1-N-[(2S)-4-amino-2-h ydroxybutanoyl]-2-deoxy-L-streptamine, ,R3=H:4-O-(3-amino-3-deoxy- -D-glucopyranosyl)-6-O-(6-amino-6-deoxy- -D-glucopyranosyl)-1,3-N-bis[(2S)-4-amin o-2-hydroxybutanoyl]-2-deoxy-L-streptami ne, ,R3=acyl:4-O-(6-amino-6-deoxy- -D-glucopyranosyl)-6-O-[3-[[(2S)-4-amino -2-hydroxybutanoyl]amino]-3-deoxy- -D-glucopyranosyl]-2-deoxy-D-streptamine , :0651 AMILORIDE HYDROCHLORIDEA miloridi hydrochloridumC6H9Cl2N7O, [17440-83-4]DEFINITION3,5-Diamino-N-carb amimidoyl-6-chloropyrazine-2-carboxamide hydrochloride : per cent to per cent (anhydroussubstance).

8 CHARACTERSA ppearance: pale yellow or greenish-yellow : slightly soluble in water and in (1)applytoallmonographsandothertexts1163