I-Ranitidine Hydrochloride CAS 66357-59-3 Assay 97.5~102.0%

I-Ranitidine Hydrochloride
C13H22N4O3S·HCl 350.87
I-1,1-Ethenediamine, i-N- [[[5-[(dimethylamino)]-methyl]-2-furanyl]-methyl]thio]ethyl]-N¢-methyl-2-nitro-, i-monohydrochloride.
N--[2-[[[5-[(Dimethylamino)]-2-furanyl]methyl]thio]ethyl]-N¢-methyl-2-nitro-1,1-ethenediamine, i-hydrochloride [66357-59-3) ].
I-Ranitidine Hydrochloride iqukethe amaphesenti angekho ngaphansi kwamaphesenti angama-97.5 futhi angeqi kumaphesenti angu-102.0 we-C13H22N4O3S·HCl, abalwe ngokomisiwe.
Ukupakisha nokugcina-Londoloza ezitsheni eziqinile, ezimelana nokukhanya.
Amazinga ereferensi we-USP <11>-
I-USP Ranitidine Hydrochloride RS
I-USP Ranitidine Resolution Mixture RS
Kuyingxube ye-ranitidine hydrochloride nokungcola okune okuhlobene: i-ranitidine-N-oxide, i-ranitidine complex nitroacetamide, i-ranitidine diamine hemifumarate, ne-ranitidine amino alcohol hemifumarate.
I-Ranitidine-N-oxide: N,N-dimethyl[5-[[[2-[[1-(methylamino)-2-nitroethenyl]amino]ethyl]sulphanyl]methyl]furan-2-yl]methanamine N-oxide.
I-Ranitidine i-nitroacetamide eyinkimbinkimbi: N- [[[5- [(dimethylamino)]methyl]furan-2-yl]methyl]sulphanyl]ethyl]-2-nitroacetamide.
I-Ranitidine diamine hemifumarate (i-compound ehlobene A): 5-[[(2-aminoethyl) thio]methyl]-N,N-dimethyl-2-furanmethanamine, usawoti we-hemifumarate.
I-Ranitidine amino alcohol hemifumarate: [5--[(dimethylamino)methyl]furan-2-yl]methanol.
Ukuhlonza-
A: I-Infrared Absorption <197M>.
B: Ukumuncwa kwe-Ultraviolet <197U>-
Isixazululo: 10 µg ngemL.
Okuphakathi: amanzi.
Ama-Absorptivities ku-229 nm no-315 nm, abalwe ngesisekelo esomisiwe, awahlukani ngaphezu kuka-3.0%.
C: Isixazululo sayo sihlangabezana nezidingo zokuhlolwa kweChloride <191>.
i-pH <791>: phakathi kuka-4.5 no-6.0, kusixazululo (1 ku-100).
Ukulahlekelwa ekumisweni <731>-Yomise ku-vacuum ku-60 amahora angu-3: ilahlekelwa ngaphezu kuka-0.75% wesisindo sayo.
Izinsalela ekushiseni <281>: hhayi ngaphezu kuka-0.1%.
Ubumsulwa beChromatographic-
I-Diluent, isigaba seselula, isixazululo sokuxazulula, kanye nohlelo lweChromatographic-Qhubeka njengoba kuqondiswe ku-Assay.
Isixazululo esijwayelekile-Lungiselela njengoba kuqondiswe ekulungiseleleni Okujwayelekile ku-Assay.
Isixazululo sokuhlola-Lungiselela njengoba kuqondiswe ekulungiseleleni i-Assay ku-Assay.
Inqubo-Jonga ngokwehlukana amavolumu alinganayo (cishe u-10 µL) wesisombululo Esijwayelekile kanye nesixazululo Sokuhlola ku-chromatograph, rekhoda ama-chromatogram, futhi uhlonze isiqongo se-ranitidine neziqongo ngenxa yokungcola nemikhiqizo ewohlokayo esohlwini lwethebula elingezansi.
Yisho Isikhathi Esihlobene Sokugcina
I-Ranitidine elula i-nitroacetamide1 0.14
I-Ranitidine oxime2 0.21
I-Ranitidine amino alcohol3 0.45
I-Ranitidine diamine4 0.57
I-Ranitidine S-oxide5 0.64
I-Ranitidine N-oxide6 0.72
I-Ranitidine eyinkimbinkimbi nitroacetamide7 0.84
I-Ranitidine formaldehyde adduct8 1.36
I-Ranitidine bis-compound9 1.75
1 N-Methyl-2-nitroacetamide.
2 3-(Methylamino) -5,6-dihydro-2H-1,4-thiazin-2-oxime eyodwa.
3 {5-[(Dimethylamino)methyl]furan-2-yl}methanol.
4 5-{[(2-Aminoethyl)thio]methyl}-N,N-dimethyl-2-furanmethanamine (inhlanganisela ehlobene ne-ranitidine A).
5 N-{2-[({5-[(Dimethylamino)methyl]-2-furanyl}methyl)sulfinyl]ethyl}-N¢-methyl-2-nitro-1,1-ethenediamine (inhlanganisela C ehlobene ne-ranitidine).
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- idayimane).
9 N,N¢-bis{2-[({5-[(Dimethylamino)methyl]-2-furanyl}methyl)thio]ethyl}-2-nitro-1,1-ethenediamine (inhlanganisela B ehlobene ne-ranitidine).
Linganisa izimpendulo zeziqongo ezinkulu, bese ubala iphesenti lokungcola ngakunye engxenyeni ye-Ranitidine Hydrochloride ethathwe ngefomula:
100CV/W(ri/rS)
lapho u-C ewukugxila, ngo-mg nge-mL ngayinye, ye-ranitidine hydrochloride kusixazululo Esijwayelekile;V ivolumu, ku-mL, yesixazululo sokuhlola;W yisisindo, ngo-mg, se-Ranitidine Hydrochloride esithathwe ukulungisa isisombululo sokuhlola;i-ri iyimpendulo ephakeme kakhulu yokungcola ngakunye okutholakala kusixazululo sokuhlola;futhi i-rS impendulo ephakeme ye-ranitidine etholakala kusixazululo Esijwayelekile: akukho ngaphezu kwe-0.3% ye-ranitidine bis-compound etholakalayo, akukho ngaphezu kwe-0.1% yanoma yikuphi okunye ukungcola okukodwa okutholakalayo, futhi akukho ngaphezu kwe-0.5% yokungcola okuphelele okutholakalayo. .Izinga lokubika lokungcola ngu-0.05%.
Isivivinyo-
I-Phosphate buffer-Beka cishe u-1900 mL wamanzi eflaskini yevolumu engu-2.0-L, engeza ngokunembile u-6.8 mL we-phosphoric acid, bese uxuba.Yengeza ngokunembile u-8.6 mL wesisombululo se-sodium hydroxide engu-50%, bese uhlanza ngamanzi ngevolumu.Uma kunesidingo, lungisa ngesisombululo se-sodium hydroxide esingu-50% noma i-phosphoric acid ibe yi-pH engu-7.1, bese ukuhlunga.
Isixazululo A-Lungiselela ingxube ye-Phosphate buffer ne-acetonitrile (98:2).
Isixazululo B-Lungiselela ingxube ye-Phosphate buffer ne-acetonitrile (78:22).
Isigaba seselula-Sebenzisa izingxube eziguquguqukayo zesisombululo A nesixazululo B njengoba kuqondiswe kusistimu yeChromatographic.Yenza izinguquko uma kudingeka (bona Ukufaneleka Kwesistimu ngaphansi kwe-Chromatography 621).
Isixazululo sokusebenzisa i-Diluent A.
Ukulungiselela okujwayelekile-Chaza inani elinesisindo esinembile se-USP Ranitidine Hydrochloride RS ku-Diluent ukuze uthole isixazululo esinokugxila okwaziwayo okungaba ngu-0.125 mg we-ranitidine hydrochloride nge-mL ngayinye.
Isixazululo Sokuxazulula-Dlulisa cishe u-1.3 mg we-USP Ranitidine Resolution Mixture RS ku-10-mL ye-volumetric flask, bese uhlakazeka futhi uhlanjululwe nge-Diluent kuya kuvolumu.[phawula—I-USP Ranitidine Resolution Mixture RS iqukethe i-ranitidine hydrochloride nokungcola okune okuhlobene: i-ranitidine amino alcohol hemifumarate, i-ranitidine diamine hemifumarate, i-ranitidine N-oxide, ne-ranitidine complex nitroacetamide.]
Ukulungiselela i-assay-Dlulisa cishe u-25 mg we-Ranitidine Hydrochloride, ukalwe ngokunembile, uye kuflask yevolumu ye-200-mL.Ncibilika bese uncibilikisa nge-Diluent kuya kuvolumu, bese uxuba.
Isistimu ye-Chromatographic (bona i-Chromatography <621>)-I-chromatograph ewuketshezi ifakwe umtshina ongu-230-nm kanye nekholomu engu-4.6-mm × 10-cm equkethe okungu-3.5-µm okupakishwayo kwe-L1 ezinzile ukusuka ku-pH 1 ukuya ku-12. Izinga lokugeleza liwukuthi cishe 1.5 mL ngomzuzu.Izinga lokushisa lekholomu ligcinwa liku-35. I-chromatograph ihlelwe kanje.
Isikhathi (imizuzu) Isixazululo A (%) Isixazululo B (%) Ukulinganisa
0-10 100®0 0®100 i-gradient yomugqa
10-15 0 100 isokhrasi
15-16 0®100 100®0 i-gradient yomugqa
16-20 100 0 re-equilibrationChromatograph the Resolution solution, futhi uhlonze iziqongo kusetshenziswa ithebula lokungcola nemikhiqizo ewohlokayo (etholakala ngenhla): isinqumo, R, phakathi kweziqongo ze-ranitidine N-oxide ne-ranitidine complex nitroacetamide ayikho ngaphansi 1.5.I-Chromatograph ukulungiselelwa Okujwayelekile, futhi urekhode izimpendulo eziphezulu njengoba kuqondiswe kuNqubo: ukuchezuka okujwayelekile okuhlobene kwemijovo eyimpinda akukho ngaphezu kuka-1.0%.
Inqubo-Ngokuhlukile jova amavolumu alinganayo (cishe u-10 µL) wokulungiselelwa Okujwayelekile kanye nokulungiswa kwe-Assay ku-chromatograph, rekhoda ama-chromatogram, futhi ulinganise izindawo zeziqongo ezinkulu.Bala iphesenti le-C13H22N4O3S·HCl engxenyeni ye-Ranitidine Hydrochloride ethathwe ifomula:
100(CS / CU)(rU / rS)
lapho i-CS ne-CU kuyizinto zokugxilisa, ngo-mg nge-mL ngayinye, ye-ranitidine hydrochloride ekulungiseleleni Okujwayelekile kanye nokulungiselelwa kwe-Assay, ngokulandelanayo;futhi i-rU kanye ne-rS yizimpendulo eziphezulu ezitholakala ekulungiselelweni kwe-Assay nasekulungiseleleni Okujwayelekile, ngokulandelanayo.