Ketorolac Tromethamine CAS 74103-07-4 Kuchena >99.0% (HPLC)

Ketorolac Tromethamine ine kwete pasi pe98.5 muzana uye kwete kupfuura 101.5 muzana yeC15H13NO3 · C4H11NO3, yakaverengerwa pane yakaomeswa.
Kurongedza uye kuchengetedza-Chengetedza mumidziyo yakasimba, isingagadzike chiedza.Chengetedza pa25°, kufamba kunobvumirwa pakati pe15° ne30°
USP Reference mwero <11>-
USP Ketorolac Tromethamine RS
Identification-
A: Infrared Absorption <197K>.
B: Ultraviolet Absorption <197U>-
Mhinduro: 10 µg pamL
Pakati: methanol.
C: Tromethamine test-Gadzirira Mushonga Wenguva yeUSP Ketorolac Tromethamine RS mumusanganiswa we dichloromethane uye methanol (2: 1) ine 5 mg per mL.Saizvozvo gadzirira mhinduro yekuyedza yeKetorolac Tromethamine ine 5 mg per mL.Isa 40-µL mavhoriyamu eStandard solution uye mhinduro yebvunzo kune yakatetepa-layer chromatographic plate (ona Chromatography <621>) yakaputirwa ne0.25-mm layer yemusanganiswa wechromatographic silica gel.Isa ndiro yacho mukamuri yechromatographic yakamboenzaniswa nemusanganiswa we dichloromethane, acetone, uye glacial acetic acid (95: 5: 2).Nama kamuri, uye gadzira chromatogram kusvika chinonyungudutsa chemberi chafamba chinenge zvikamu zvitatu kubva muzvina zvehurefu hwendiro.Bvisa ndiro kubva mukamuri, uye bvumira solvent kuti ibude.Pfaya ndiro ine mushonga wedoro uchangobva kugadzirirwa une 30 mg ye ninhydrin pa mL, uye kupisa ndiro iyo inenge 150 ° kwemaminitsi maviri kusvika mashanu.Mavara eyero ane pink kusvika kune yepepuru miganhu anokura pandiro munzvimbo dzakashandiswa Standard solution uye mhinduro yebvunzo.
pH <791>: pakati pe5.7 ne6.7, mune mhinduro (1 mu100).
Kurasikirwa pakuomeswa <731> -Dry it in vacuum pa 60 ° kwemaawa matatu: inorasikirwa kwete kupfuura 0.5% yehuremu hwayo.
Residue pakudzima <281>: kwete kupfuura 0.1%.
Heavy metals, Nzira II <231>: 0.002%.
Chromatographic kuchena-
Nharembozha nhanho, musanganiswa weSolvent, Kugadzirira kwakajairwa, Resolution solution, uye Chromatographic system-Pfuura sezvakarairwa muAssay.
Test solution-Shandisa gadziriro yeAssay.
Procedure-Chromatograph mhinduro yeTest sezvakarairwa Procedure muAssay, ichibvumira chromatography kuti iwedzere kusvika katatu nguva yekuchengetedza ketorolac.Edza mhinduro dzemapikisi ese.Verengai muzana yekusachena kwega kwega muchikamu cheKetorolac Tromethamine inotorwa neformula:
100rfi (ri / rs)
umo rfi ndiyo mhinduro yekusachena yega yega peak maererano neiyo ketorolac;ri ndiyo mhinduro yepamusoro yekusachena kwega kwega;uye rs ndiyo hwerengedzo yemhinduro dzese dzepamusoro dzenhongonya dzetsvina uye hombe ketorolac peak.Rfi values ​​ndeye 0.52 ye ketorolac 1-keto analog, 0.67 ye ketorolac 1-hydroxy analog, 2.2 yepeak yekusachena ine nguva yekuchengetedza ye 0.54 maererano neiyo ketorolac, uye 0.91 yekusachena kwepamusoro pane imwe nguva yekuchengetedza. ye0.66.Kwete kupfuura 0.1% ye ketorolac 1-keto analog kana ketorolac 1-hydroxy analog inowanikwa;kwete kupfuura 0.5% yeimwe tsvina inowanikwa;uye huwandu hwese hutsvina haupfuuri 1.0%.
Kuongorora-
Nharembozha chikamu-Dissolve 5.75 g ye monobasic ammonium phosphate mu1000 mL yemvura, uye gadzirisa nephosphoric acid kusvika pH ye3.0.Gadzirira musanganiswa wakanatswa uye wakasvibiswa weiyi buffer solution uye tetrahydrofuran (70:30).Ita zvigadziriso kana zvichidikanwa (ona System Suitability pasi peChromatography <621>) kuti uwane nguva yekuchengetedza ketorolac yemaminitsi masere kusvika gumi nemaviri.
Solvent musanganiswa-Gadzirira musanganiswa wemvura uye tetrahydrofuran (70:30).
Kugadzirira kwakajairwa-Kunyungudutsa huremu hwakayerwa nemazvo hweUSP Ketorolac Tromethamine RS mumusanganiswa weSolvent kuti uwane mhinduro ine huwandu hunozivikanwa hunosvika 0.4 mg per mL.[Cherechedza-Chengetedza mhinduro iyi kubva kuchiedza.]
Kugadzirira kweAssay-Kutamisa inenge 20 mg yeKetorolac Tromethamine, yakayerwa nemazvo, kune 50-mL volumetric flask, dilute nemusanganiswa weSolvent kusvika kuhuwandu, uye sanganisa.[Cherechedza-Chengetedza mhinduro iyi kubva kuchiedza.]
Resolution solution-Mune 250-mL separator mix 100 mL yemvura, 100 mL ye dichloromethane, 30 mg ye USP Ketorolac Tromethamine RS, uye 1 mL ye1 N hydrochloric acid.Isa chivharo, zunza, uye bvumira kuti zvidimbu zviparadzanise.Chinja iyo yepasi dichloromethane layer kune yakamiswa borosilicate girazi flask, uye urase iyo yepamusoro layer.Ratidza mushonga wedichloromethane kujekesa zuva kwemaminetsi gumi kusvika gumi nemashanu.Fambisa 1.0 mL yemushonga mubhodhoro, nyungudika mumhepo yazvino kana murukova rwenitrogen kusvika pakuoma, wedzera 1.0 mL yemusanganiswa weSolvent, uye swirl kunyungudika.[Cherechedza-Iyi mhinduro inogona kuchengetwa pasi pefiriji uye kushandiswa chero bedzi chromatogram yakawanikwa sezvakange yakarongedzerwa kuMaitiro inokodzera kuziva nhongonya nekuda kwe ketorolac 1-keto analog uye ketorolac 1-hydroxy analog, uye nekuyera kwechigadziro. pakati pe ketorolac 1-keto analog uye ketorolac.]
Chromatographic system (ona Chromatography <621>)—Iyo chromatograph yemvura ine 313-nm detector uye 4.6-mm × 25-cm column ine 5-µm packing L7 uye inochengetwa patembiricha isingaperi ingangoita 40°.Chiyero chekuyerera chinenge 1.5 mL paminiti.Chromatograph the Resolution solution, uye rekodha mhinduro dzepamusoro sekutaurirwa kweNzira: nguva dzekuchengetedza dzinenge 0.63 ye ketoroac 1-hydroxy analog, 0.89 ye ketorolac 1-keto analog, uye 1.0 ye ketorolac;uye chisarudzo, R, pakati pe ketorolac 1-keto analog uye ketorolac haisi pasi pe 1.5.Chromatograph the Standard kugadzirira, uye rekodha mhinduro dzepamusoro sekurairwa kwaProcedure: iyo column inoshanda haisi pasi pe5500 theoretical plates;uye kutsauswa kwakajairwa kwemajekiseni ekudzokorora hakupfuuri 1.5%.
Maitiro-Kuparura jekiseni mavhoriyamu akaenzana (angangoita 10 µL) eGwaro gadziriro uye gadziriro yeAssay muchromatograph, rekodha machromatogram, uye kuyera mhinduro dzepamusoro-soro.Verenga huwandu, mu mg, hweC15H13NO3 · C4H11NO3 muchikamu cheKetorolac Tromethamine chakatorwa neformula:
50C(rU / rS)
umo C ndiyo yekuisa, mu mg per mL, yeUSP Ketorolac Tromethamine RS muStandard gadziriro;uye rU uye rS ndiyo ketorolac peak mhinduro dzakawanikwa kubva muAssay gadziriro uye Standard gadziriro, zvichiteerana.