Ranitidine Hydrochloride CAS 66357-59-3 Kev Ntsuam Xyuas 97.5 ~ 102.0%

Ranitidine Hydrochloride
C13H22N4O3S · HCl 350.87
1,1-Ethenediamine, N-[2-[[[[5-[(dimethylamino)methyl]-2-furanyl]-methyl]thio]ethyl]-N¢-methyl-2-nitro-, monohydrochloride.
N-[2-[[[5-[(Dimethylamino)methyl]-2-furanyl]methyl]thio]ethyl]-N¢-methyl-2-nitro-1,1-ethenediamine, hydrochloride [66357-59-3 ].
Ranitidine Hydrochloride muaj tsis tsawg dua 97.5 feem pua ​​thiab tsis ntau tshaj 102.0 feem pua ​​​​ntawm C13H22N4O3S·HCl, xam rau ntawm lub hauv paus qhuav.
Ntim thiab khaws cia-Txuag hauv cov thawv nruj, lub teeb-tiv taus.
USP Reference cov qauv <11>-
USP Ranitidine Hydrochloride RS
USP Ranitidine Resolution Mixture RS
Nws yog ib qho kev sib xyaw ntawm ranitidine hydrochloride thiab plaub yam impurities: ranitidine-N-oxide, ranitidine complex nitroacetamide, ranitidine diamine hemifumarate, thiab ranitidine amino cawv hemifumarate.
Ranitidine-N-oxide: N, N-dimethyl[5-[[[[2-[[[1-(methylamino)-2-nitroethenyl]amino]ethyl]sulphanyl]methyl]furan-2-yl]methanamine N-oxide.
Ranitidine complex nitroacetamide: N-[2-[[[[5-[(dimethylamino)methyl]furan-2-yl]methyl]sulphanyl]ethyl]-2-nitroacetamide.
Ranitidine diamine hemifumarate (muaj feem xyuam nrog A): 5-[[(2-aminoethyl)thio]methyl]-N, N-dimethyl-2-furanmethanamine, hemifumarate ntsev.
Ranitidine amino cawv hemifumarate: [5-[(dimethylamino)methyl]furan-2-yl]methanol.
Kev txheeb xyuas-
A: Infrared Absorption <197M>.
B: Ultraviolet Absorption <197U>-
Kev daws: 10 µg per mL.
Nruab nrab: dej.
Absorptivities ntawm 229 nm thiab 315 nm, xam ntawm lub hauv paus qhuav, tsis txawv ntau tshaj 3.0%.
C: Ib qho kev daws teeb meem ntawm nws ua tau raws li qhov yuav tsum tau ua ntawm kev sim rau Chloride <191>.
pH <791>: nruab nrab ntawm 4.5 thiab 6.0, hauv kev daws (1 ntawm 100).
Poob ntawm ziab <731>-Sry hauv lub tshuab nqus tsev ntawm 60 rau 3 teev: nws poob tsis ntau tshaj 0.75% ntawm nws qhov hnyav.
Residue ntawm ignition <281>: tsis ntau tshaj 0.1%.
Chromatographic purity-
Diluent, Txawb theem, Kev daws teeb meem, thiab Chromatographic system-Ua raws li qhia hauv Kev Tshawb Fawb.
Standard tov-Npaj raws li qhia rau Standard npaj nyob rau hauv lub Assay.
Test solution-Npaj raws li qhia rau Assay npaj hauv Assay.
Cov txheej txheem-Kev txhaj tshuaj sib npaug (kwv yees li 10 µL) ntawm cov txheej txheem kev daws teeb meem thiab cov tshuaj ntsuam xyuas rau hauv chromatograph, sau cov chromatograms, thiab txheeb xyuas qhov ncov ranitidine thiab cov peaks vim impurities thiab degradation cov khoom teev nyob rau hauv cov lus hauv qab no.
Lub Sijhawm Retention Relative Name
Ranitidine yooj yim nitroacetamide1 0.14
Ranitidine Oxime2 0.21
Ranitidine amino cawv 3 0.45
Ranitidine diamine 4 0.57
Ranitidine S-oxide 5 0.64
Ranitidine N-oxide 6 0.72
Ranitidine complex nitroacetamide7 0.84
Ranitidine formaldehyde adduct8 1.36
Ranitidine bis-compound9 1.75
1 N-Methyl-2-nitroacetamide.
2 3-(Methylamino)-5,6-dihydro-2H-1,4-thiazin-2-ib oxime.
3 {5-[(Dimethylamino)methyl]furan-2-yl}methanol.
4 5-{[(2-Aminoethyl)thio]methyl}-N,N-dimethyl-2-furanmethanamine (ranitidine ntsig txog compound A).
5 N-{2-[({5-[(Dimethylamino)methyl]-2-furanyl}methyl)sulfinyl]ethyl}-N¢-methyl-2-nitro-1,1-ethenediamine (ranitidine ntsig txog compound C).
6 N,N-Dimethyl(5-{[(2-{[1-(methylamino)-2-nitroethenyl]amino}ethyl)
sulphanyl]methyl}furan-2-yl) methanamine N-oxide.
7 N-{2-[({5-[(Dimethylamino)methyl]furan-2-yl}methyl)sulphanyl]ethyl}-2-nitroacetamide.
8 2,2¢-Methylenebis(N-{2-[({5-[(dimethylamino)methyl]furan-2-yl}methyl)sulphanyl]ethyl}-N¢-methyl-2-nitroethene-1,1- diamine).
9 N,N¢-bis{2-[({5-[(Dimethylamino)methyl]-2-furanyl}methyl)thio]ethyl}-2-nitro-1,1-ethenediamine (ranitidine ntsig txog compound B).
Ntsuas cov lus teb rau lub ncov loj, thiab xam cov feem pua ​​​​ntawm txhua qhov impurity nyob rau hauv ib feem ntawm Ranitidine Hydrochloride coj los ntawm cov mis:
100CV / W (ri / rS)
nyob rau hauv uas C yog qhov concentration, nyob rau hauv mg ib mL, ntawm ranitidine hydrochloride nyob rau hauv tus txheej txheem tov;V yog qhov ntim, nyob rau hauv mL, ntawm Test tov;W yog qhov hnyav, hauv mg, ntawm Ranitidine Hydrochloride coj los npaj cov tshuaj ntsuam xyuas;ri yog lub ntsiab lus teb rau txhua qhov impurity tau los ntawm Kev Ntsuas Kev daws;thiab rS yog ranitidine ncov cov lus teb tau los ntawm cov qauv kev daws teeb meem: tsis pub ntau tshaj 0.3% ntawm ranitidine bis-compound pom, tsis pub ntau tshaj 0.1% ntawm lwm yam impurity pom, thiab tsis pub ntau tshaj 0.5% ntawm tag nrho cov impurities yog pom. .Kev qhia theem rau impurities yog 0.05%.
Assay-
Phosphate buffer-Qhov chaw kwv yees li 1900 mL ntawm cov dej hauv 2.0-L volumetric hwj, raug ntxiv 6.8 mL ntawm phosphoric acid, thiab sib tov.Ua kom raug ntxiv 8.6 mL ntawm 50% sodium hydroxide tov, thiab dilute nrog dej rau ntim.Yog tias tsim nyog, kho nrog 50% sodium hydroxide tov lossis phosphoric acid rau pH ntawm 7.1, thiab lim.
Kev daws A-Npaj sib xyaw ntawm Phosphate tsis thiab acetonitrile (98: 2).
Kev daws B-Npaj ib qho sib xyaw ntawm Phosphate tsis thiab acetonitrile (78:22).
Txawb theem-Siv sib txawv sib txawv ntawm cov tshuaj A thiab tshuaj B raws li qhia rau Chromatographic system.Hloov kho yog tias tsim nyog (saib System Suitability hauv Chromatography 621).
Diluent-Siv Solution A.
Cov txheej txheem kev npaj-Dissolve ib qho hnyav hnyav ntawm USP Ranitidine Hydrochloride RS hauv Diluent kom tau txais cov kev daws teeb meem uas paub txog qhov concentration ntawm 0.125 mg ntawm ranitidine hydrochloride ib mL.
Kev daws teeb meem-Hloov txog 1.3 mg ntawm USP Ranitidine Resolution Mixture RS rau 10-mL ntim ntim, thiab yaj hauv thiab dilute nrog Diluent rau ntim.[ceeb toom—USP Ranitidine Resolution Mixture RS muaj ranitidine hydrochloride thiab plaub yam impurities: ranitidine amino cawv hemifumarate, ranitidine diamine hemifumarate, ranitidine N-oxide, thiab ranitidine complex nitroacetamide.]
Kev tshuaj ntsuam xyuas-Hloov txog 25 mg ntawm Ranitidine Hydrochloride, ntsuas kom raug, mus rau 200-mL ntim ntim.Dissolve nyob rau hauv thiab dilute nrog Diluent rau ntim, thiab mix.
Chromatographic system (saib Chromatography <621>)-Cov kua chromatograph yog nruab nrog 230-nm detector thiab 4.6-mm × 10-cm kem uas muaj 3.5-µm packing L1 uas ruaj khov ntawm pH 1 txog 12. Tus nqi ntws yog txog 1.5 mL ib feeb.Lub kem kub yog tswj ntawm 35. Lub chromatograph yog programmed raws li nram no.
Sijhawm (feeb) Tshuaj A (%) Tshuaj B (%) Elution
0-10 100® 0 0®100 linear gradient
10-15 0 100 isocratic
15-16 0®100 100®0 linear gradient
16-20 100 0 re-equilibrationChromatograph qhov kev daws teeb meem, thiab txheeb xyuas cov peaks siv lub rooj ntawm impurities thiab degradation khoom (pom saum toj no): kev daws teeb meem, R, nruab nrab ntawm lub ncov rau ranitidine N-oxide thiab ranitidine complex nitroacetamide tsis tsawg tshaj li. 1.5.Chromatograph tus txheej txheem npaj, thiab sau cov lus teb ncov raws li qhia rau Kev Ua Haujlwm: tus qauv sib txawv ntawm qhov sib txawv rau kev txhaj tshuaj tsis ntau tshaj 1.0%.
Cov txheej txheem-Kev txhaj tshuaj sib npaug (kwv yees li 10 µL) ntawm Standard npaj thiab Assay npaj rau hauv chromatograph, sau cov chromatograms, thiab ntsuas qhov chaw rau lub ncov loj.Xam cov feem pua ​​​​ntawm C13H22N4O3S·HCl hauv feem ntawm Ranitidine Hydrochloride coj los ntawm cov mis:
100 (CS / CU) (rU / rS)
nyob rau hauv uas CS thiab CU yog cov concentrations, nyob rau hauv mg per mL, ntawm ranitidine hydrochloride nyob rau hauv Standard npaj thiab Assay npaj, feem;thiab rU thiab rS yog cov lus teb siab kawg uas tau txais los ntawm Assay npaj thiab Standard npaj, feem.