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    0 Drug Monographs

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    venishetty

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    P2010 DICLOFENAC soprUM. Mobile phase. A mixture of 7 volumes of 28.M ammonia, 25, Yolumes of methanol and 68 volumes of ehlorafinm Test solution. Shake a quantity of the powdered tablets containing 0.75 g of Dinzoxide with 40 ml of 0.1 M sodium ‘hydroxide for 30 minutes, filter and dite the fluate to 30m with O1 M sodin hydroxide Reference soltion. Dilute 1 ml ofthe test solution to 200 nt With 0.1 M sodium Iytroxide, Apply tothe plate 5 yl ofeach Solution After development, Ay the plat in air and examine in ultraviolet ight at 254 nm, Any secondary spet inthe chromatogram obtained with the test solution is not more intense than the spot in the chromatogram obiained withthe reference solution (05 per cent). Other tests. Comply with the tess stated under Tablets Assay. Weigh and powder 20 tablets, Weigh accurately a ‘Quantity ofthe powder containing shout 0.05 g of Diazoxide, ‘844 70 ml of methanol, shake for 1 hour, add sufficient ‘methanol produce 100 ml, mix an filter, Dilute Srl of the filrate to 250 ml with 0.1 sodium hydroxide. Measure the absorbance ofthe resulting solution atthe maximum at about 280 nm (2.4.7). Caleulat the content of CH,CIN,O;S taking ‘585s the specific absorbance at 280 nm. Diclofenac Sodium COONa 4 i { COO C.CLNNAD, Mol We3i81 Diclofenac Sodium is sodium 2-[(2,6-dichlorophenyl)- amino)phenylacetate, Diclofenac Sodium contains not less than 98.5 per cent and ‘notmore than 101.0 pr cent of C,.H,ClINNaO,, caleulated on the dried basis, Category. Analgesic; anti-inflammatory, Dose. Orally or by intaniascalar injection, 251075 mg. Description. whitetoslighly yellowish erystelline powder; slighly hygroscopic, Identification ‘Test A may be omined if tests B, C, and D are carried out. Tests Band Cay be omited if tes¢A and D are carried out, ‘A. Determine by infared absorption spectrophotometry (2.4.6). Compare the specteum with that obtained with diclofenac sodium RS or with the reference spectrum of diclofenac sodium, B.ToI mlofa04 percent wiv solution in methanol add 1 of nitric acid a dat red eolour develops. CCIn the test for Related substances, the principal peak inthe chvomatogram obtained with the test solution corresponds to the peak in the chromatogram obtained with the reference solution, D.A1 percent w/v solution gives the rection of sodium salts 030), Tests Appearance of solution. A 5.0 per cent wiv solution in ‘methanol is clear (2.4.1), and not more intensely coloured than reference solution BYS6 (24.1). pH (2424), 6.51085, determined ona 1.0 percent wy solution. Light absorption (2.4.7). Absorbance of a 5.0 per cent wiv solution in methanol at about 440 nm, not more than 0.050. Related substances. Determine by liquid chromatography 2419. Test solution. Dissolve 50 mg of the substance under examination in methano! and dilute to 50 mal with the same solvent, Reference solution. A 0.0002 pet cent wly solution of diclofenac sodium RS is methancl. Chromatographic system ~ a siainless stee}columa 25 cm x 4,6 mm, packed with end-capped octysilanc bonded to porous silica (5pm), mobile phase: a mixture of 34 volumes ofa solution Cconttning 05 g per le of phosphoric acid and 0.8 g per Lue of sodium ditytrogen phosphate adjusted to pH 25 with phosphoric acid, and 66 volumes of ‘methanol, = flow ate. Tl per minute, ~ spectrophotometer set at 254 nm, ~ injection volume. 20). Inject the test solution and the reference solution, In the chromatogram obtained withthe test solution: the area of any ‘peak othe than the principal peak isnot greater than the ares of the principal pea inthe chromatogram obtained with the reference solution (0.2 percent); the sum of the areas ofall peaks other than the principal peak is not greater than 25 times that of the principal peak in the chromatogram obtsined withthe reference solution (05 pet cea) Igoore any Peak with an area ess than 0:25 times te aeaof the principal Peskin the chromatogram obtained withthe reference solution. 1199 DICLOFENAC NECTION Heavy metals 2.3.13), 1.0 g complies with the limit test for ‘heavy metals, Method B (10 ppm). Lasson drying (24.19), Not more than 0.5 per een determined (on 1.0 g by drying.in an oven at 105° for Shouts, Assay. Weigh accurately about 0.2 g and dissolve in SO ml of ambydrous glacial acetic acd. Titate with 0.1 M perchlorte GE determining the end-point potentiometrically (2.425) Cary outa blank titration, tiny of 2d M perchloric acids equivalent 1 0.03181 g of CicHeChNNa0,, Storage. Store protected from light Diclofenac Injection Diclofenac Sodium Injection Diclofenac Injections a sterile solution of Diclofenac Sodium ‘a Wter foc njctons.Itmay contain Propylene Glycol, Benay Alcohol and sufficient Sodium Hydroxide to adjust the pH of the solution, Diclofenac Injection contains not less than 95.0 per cent and ‘ot more than 105.0 percent ofthe stated amount of diclofenae sodium, C.cHoChNNaQ,, ii Usual strength. 25 ng perm Deseription. A cleas, colouriess to yellowish qui. Identification Determine by thin-layer chromatography (24,17), costing the plete with silica gel GF254. Mobile phase. A mixture of 90 volumes of chloroform, 5 volumes of acetone and $ volumes of formic acid ine ~-Saturated chamber Test solution, Dilute a suitable volume of the injec containing 25 mg of Diclofenac Sodium to 10 ml ‘methanol, Reference solution. A0.25 per cent w/y solution of diclofenac sediur RS in methanol. Apply tothe plate 2 ofeach solution, After development, Ary the platen a current of warnh air and examine in ulravioley ght at 254.nm, Aliematively, spray with a5 pee cent wiy soluion of potassium diehromate in sulphuric ald (20 per ent By both methods of visualisation, the principal spon the choinatogram obtained withthe est solution carrespond to that in the chromatogram obtained with the reference solution, ith P2010 Tests PH (2.424).8.1 109.0. Other. tests. Complies with the tests stated under Parenteral Preparations (Injections). Assay. Detemincby liquid chromatography (24,14, Test solution. Dilute & suitable volume of the injection containing 25 mg of Diclofenac Sodium to 10.0 ml with the mobile phase, ‘Reference solution. AO25 pet cent wiv solution of dielofenae sodivun RS in the mobile phase. Chromatographie system ~ Astainless steel column 12.5 em x4.6 mm, packed with ‘etylailane bonded to porous silica (Sn), ~ mobile phase: a mixture of 60 volumes of methanol and 40 volumes of 0.1 M sodium acetate solution, ~ flowrate, 1 ml per minute, = spectrophotometer set at 254 nm, ~ injection volume. 104 Injee alternately the test solotion and the reference solution and record the chromatograms for 25 times the retention time ‘of the principal peak. I necessary adjust the concentration af ‘methanol inthe mobile phase to obtain the resolution of the Peak due to diclofenac sodium. Calculate the content of CHisClNN2Osia the injection, Diclofenac Tablets Diclofenac Sodium Tablets Diclofenac Tablets contain not less than 90.0 per cont and not ‘mote than 110.0 percent ofthe stated amount of diclofenae sodiuro, CHCLANNaO,, The tablets may be eteric-coated, Identification Determine thin-layer chromatography (2.4.17, coating the late with sia gel 60 F254 or using a precoated sion gel 60 F254 ple. ‘Mobile phaseAmmixtureoF 10 volumes of toluene, 10 volumes of hexane and 10 volumes of anhydrous formic eld Test solution, Shake a quantity of the powdered tablets containing 5O mg of Diclofenac Sodium with S ml of methanat, ceutrfuge and use the supernatant liquid, Reference solution. A per cont wiy solution of delojenae sodium RS in methonol, 1200 w7010 CHTIRIZINE INYDROCHLORIDE, The contents of the sealed container comply with the requirements stated under Parenteral Preparations (Peters for Injection) and with the follwing requirements Tdentiicatton A Determine by infared absorption spectrophotomety (24.6), Compare the spectrum with that obtained wi cephaloridine (a-form) RS or eephalordine (bform) RS ‘oF withthe reference spectrum of cephaloridine (form) or cephalridine (S-form), 3, Mix 20 mp wit few drops of an 80 per cen viv slution of sulphur acd containing 1 per cent vy of mitre acid; a uit green color is produced, ©."To 805 per cent wy solution add 1 ml of chloramine salutlon ond 2 rl of 0.1 M sodiane hydroxide; dll red colour 1s produced which persists for 1 minute, _D. Gives the raetions of penicillins and e=phalosporins (23.1). Tests Appearance of solution (2.4.1). Solution A is leat, pI (2.4.24), 40 t0 6.0, determined in a 10.0 per eent w/v solution (solution A) prepared by dissolving in carbon dloxlde:free water, warring to 20° and cooling to 20°, Specific optical rotation (2.4.22). +46.0° to +50.0°, determined at 25° ina 1.0 per cent wi solution, [Light absorption, When examined in the range 230 nm to ‘360 nm (24,7) 20.0012 per cent wiv solution shows absorption ‘maxims at ebout 240 nm and 255 nim; absorbanee at the ‘maximum at about 240 nm, 0.43 (0 OB, The ratio of the borbance atthe maximum at about 240 nm to that at about 255 nin is not more than 1.0. Pyridine. Dissolve about 25 mg, in 10 ml of water snd ad 25 ml of x bufer solution prepared by adjusting a5 percent ‘wy volun of dlsodlum lnydrogen phosphate wo pl 6.0 with phosphorle acid and adding | per cent viv of anil, Add 1.25 ml ofa solution prepared by decolorisng a 0.5 per cent viv tolution of bromine with potassium cyanide solution, shaking and allowing, to stand for 2 minutes, and sufficient vnater\o produce 25 ml and allow to stand for 25 minutes, Measure the absorbance of the resulting solution at the ‘maximurn at about 462 nun, using ax the blank a solution prepared in sinilse mannerbutomiting he bubstanee under examination (24,7), The abmorbance is rot more than that of solution prepared by treating 2.5 ml of 0.005 per cent wiv ‘olution of pyridine in a similar mamer, Sulphated ash (2.3.18). Not moce than 0:2 per cent ‘Wier (2:38). Not moe than 0 per cent ww (ufon and not ‘note than 30 per cent wi (B-form, determined on 0.25 g, Uses the solvent w inure of equal yolumes of dehydrated ‘methanol ant dehydrated pysidine in pluce of methanal, nine the weight te contents of 10 containers Weigh accurately a quantity of the mixed contents of the 10 coniners conning about 00mg of eephaloridine and Aisaolve in sulficient water to produce 500 mi. Transfer 100roltoa stopered flak, ad a of 1M sodium hydroxide snd ll to stand for 9 minutes, Ad 20m of abutfer solution containing 35.0 per eet of sodlum acetate and 62.4 per cent vl of glacial acetle act, 5 lof 1M hydrochloric acid and25.0ml of 0.01 M adie, clove the flak with avet stopper and allo to stand for3 hours ina water-bath at 30°, protected {rom light Tat the oxcess of fodine with O02 M godt Ahlosulphate using starch solution, alded towards the end of the tvation, as ines. To a furer 10.0 lof the soltion sd 20 ml ofthe buer solution and 250 lof 0.01 M iodine, allow to stand for 3 hours in a water-bath at 30°, protected foon igh. Tiat the exeess of iodine with 0.02 Mf sodium ‘Hlosulphae sing starch soluion, added towards the end of the ivatin, a indicator, The diflerence between the tivation represents the volume of 0.91 M indine equivalent to the cephalordine present, Caleulate the content of CHyNyOS: ftom the difference obtained by simultaneously earryng out the Astay using cephaloldine (B-form) RS instead of the substance under examination, Cephaoridin intended for sein the manufacture of preter preparations complies with the following additional tess, Pyrogens, Complies withthe test for pyrogens (2.2.8), using not ess than SO mg perk ofthe rabbit's weight, dissolved in 1 mi of Water for Injections. Sterility 22.11). Complies withthe test foreterity, Storage, Stor protected fom light and moisture at a temperature not exceeding 30°. The constituted solution should be used within 24 hours when stored ata temperature rotexceeding20° or within days when storedin refrigerator @08"), Labeling The label sates (1) the weight of Cephaloriine contained inthe sealed container; (2) whether the contents ‘are Cephaloridine (o-form) or Cephalordine (6-frm), Celirizine Hydrochloride CttzineDinydroeoide cl rw 60H Ol NJ » 2HCI CyyHsCINO,211CL Mol. Wt. 461.8 1037 CEMRIZINE HYDROCLORIDE Cetrizine Hydrochloride is [2-(4-[(4-chloropheny!) phenylmethy1}-L-piperazinylethoxylecetic acid dihydrochloride, CCeirizine Hydrochloride contains not less than 99.0 per cent and not more than 100.5 per cent of CyHfyCIN;O;2HCl, calculated on the dried basis, Category. Anthistaminie, Description. A white or almost white powder, Identification A. Determine by infrared absorption spectrophotometry (2.4.6), Compare the spectrum with that obtained with cetricine indrochloride RS or with the reference spectrum Of cetirizine hydrochloride. B. Dissolve 20.0 mg in $0 ml of 1.03 percent wiy solution of| Jydrochlorie acid and dilute o 100.0 tml wit the same acid. Dilute 10.0 ml of this solution to 100.0 mi with the acid ‘When examined in the range 210 nm to 350 nm (24:7), the ‘esting solution shows an-absorption maximuoy at about 231 nm. The specific absorbance at 231 nmis 359 03381, C. Determine by thin-layer chromatography (2.4.17), coating the plate with silica gel GF254, Mobite pase. mixture of 1 volume of ammonia, 10 volumes of methanol and 90 volumes of dichloromethane Test solution. Dissolve 10 mg of the substance under ‘examination in garerand duce 10S ml withthe same solvent Reference solution (a). Dissolve 10 mg of cetirizine 'ydrochloriée RS in water and dilute to ml with the same solvent. Reference solution (6). Dissolve 10 mg of eblorphenamine ‘maleate RS in water and dilute o 5m with the same solvent To.LanLofthe-slution add iat eferessaien a) eereanpe ee OsI-times the ares of Apply tothe plate 5 1 ofeach solution. After development, sy ina curent of cold air and examine in ulzavolet light 254 nm. The prinipalspotin the chromatogram obtained with the test solution corresponds to the principal spot in the chromatogram obtained with reference solution (a). The test {snot valid unless the chromatogram obtained with reference solution (b) shows 2 clearly separated spots, D.It gives eaction A of chlorides (23.1). Tests Appearance of solution, A'.0perceatviy solatonin carbon {lotde free water (sludon A) is clea (2.4.1) and not men ‘nensely coloured than reference solution BYS? (2.4.1), Assay. P2010 pIL(2.4.24), 1.2 00 1.8, determined in solution A. Related substances. Determine by liquid chromatography 4.14, Test solution, Dissolve 20 mg of the substance under ‘examination in the mobile phase and dilute to 100 ml withthe mobile phase. Reference solution (a). 8 solution containing 0.02 per cent wiv each of cetirizine ditydrochloride RS and (RS)-[-((4- shlorophenyliphenslmethyl|piperazine RS ( cetirizine ‘impurity Ain the mobile phase. Dilute 1m ofthe solution to 100. with te mobile phase, Reference solution (b). Dike 2m ofthe test solution to 50 ml with the mobile phase, Dilute 5 mi of the solution to 100 ml ‘withthe mobile phase. Chromatographic system - ~ A stainless steel column 25 om x 4.6 mim, pecked with silica get (5 ur), ~ mobile phase: amixwre of 0,4 volume of dilute sulphuric acid, 6.6 volumes of water and 93 volumes of ‘acetonitrile, ~ flowrate. ml perminate, ~ spectrophotometer set at 230 am. ~ injection volume. 2042, Inject reference solution (a). The test is not valid unless the resolution between the peaks due to cetirizine and impurity A ‘snotless than 2 and the tailing factors are not more than 2 0. Inject the test solution and reference solution (b). Run the chromatogram for3 times the retention time of cetieizine. In {he chromatogram obtained withthe test solution, the area of ‘any impurity peak is not more than 0.5 times the azea of the principal peak in the chromatogram obtained with refercnce solution () (0.1 per cent). The sum of the areas ofall such Peaks snot more than 1.5 times the area of the principal peak tn he chromatogram obtained with reference solution (0) (03 ! peak in the chromatogram obtained with reference solution (b) (0.02 per cent). Sulphated ash (2.3.18). Not more than 0.2 per cent Kross on drying (2.4.19. Not more than 0.5 per cent, Aetermined on 1.0 g by drying in an oven at 100° 105" accurately about O.1g, dissolve in 20mlata smianure of 30 volumes of water and 70 volumes of acetone. {fixate with 0.24 sod hydroxide to the second point of {Mlerlon, Determine the end-point potentiometcally (24.25) Carry outa blank titration, Conc Ad M sodium hydride is equivalent 1 0.01539 g of CaltyChN,0,, 1038 2010 CETIRIZINE TABLETS Storage, Store protected rom light, Cetirizine Syrup Cotirizine Oral Liquid CCtirizine Syrup contains not less than 90.0 percent and not ‘more than 1100 per cent of the stated amount of cetirizine hydrochloride C,,HCINO,, 2HCL. ‘Usual strength. 5 mg per ml. Identification Inthe Assay, the principal peak inthe chromatogram obtained with the test solution corresponds to the peak in the ‘chromatogram obtained with the reference solution, Tests PH@424). 451055. ‘Other fests. Complies with the tests stated under Oral Liquids. ‘Assay. Determine by liquid chromatography (24.14). Solent mixture, 60 volumes of water and 40 volumes of ‘acetonirie, Test solution, Weigh accurately a quantity of the syrup containing 5 mg of Cetirizine Hydrochloride, dissolve in 100.0 ml of the solventamixture and filter. ‘Reference solution. 40.005 percent wiv solution of cetirizine

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