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

Ketorolac Tromethamine wuxuu ka kooban yahay wax aan ka yarayn 98.5 boqolkiiba oo aan ka badnayn 101.5 boqolkiiba C15H13NO3 · C4H11NO3, oo lagu xisaabiyo sal qallalan.
Baakadaha iyo kaydinta-Ku xafid weelasha cidhiidhiga ah, iftiinka u adkaysta.Ku kaydi 25°, tamashlaha waa la ogolyahay inta u dhaxaysa 15° iyo 30°
Heerarka Tixraaca USP <11>-
USP Ketorolac Tromethamine RS
Aqoonsiga -
J: Nuugista Infrared <197K>.
B: Nuugista Ultraviolet <197U>-
Xalka: 10 µg halkii ml
Dhexdhexaad: methanol.
C: Tijaabada Tromethamine-U diyaari xalka caadiga ah ee USP Ketorolac Tromethamine RS isku dar ah dichloromethane iyo methanol (2:1) oo ka kooban 5 mg halkii ml.Sidoo kale diyaari xal tijaabo ah Ketorolac Tromethamine oo ka kooban 5 mg halkii ml.Codso mugga 40-µL ee xalalka caadiga ah iyo xalka tijaabada saxan koromograafi ah oo khafiif ah (fiiri Chromatography <621>) oo lagu dahaadhay lakabka 0.25-mm ee isku dhafka silica chromatographic.Saxanka dhig qol koromograafi ah oo hore loogu simay isku darka dichloromethane, acetone, iyo glacial acetic acid (95:5:2).Xir qolka, oo samee chromatogram-ka ilaa uu afka hore ee dareeruhu uu dhaqaaqo qiyaastii saddex meelood meel dhererka saxanka.Saxanka ka saar qolka, oo u ogolow dareeraha inuu uumi baxo.Ku buufin saxanka xal khamri ah oo dhowaan la diyaariyey oo ka kooban 30 mg oo ninhydrin ah halkii mL, oo ​​ku kululee saxanka ilaa 150 ° 2 ilaa 5 daqiiqo.Dhibco jaale ah oo leh soohdin casaan iyo guduud ah ayaa ku soo koraya saxanka meelaha lagu dabaqay xalka caadiga ah iyo xalka tijaabada.
pH <791>: inta u dhaxaysa 5.7 iyo 6.7, ee xal (1 in 100).
Luminta qallajinta <731>-Ku qalaji meel faakuum ah 60° 3 saacadood: waxay luminaysaa wax aan ka badnayn 0.5% miisaankeeda.
Hadhaaga dabka <281>: aan ka badnayn 0.1%.
Biraha culus, Habka II <231>: 0.002%.
Daahirnimada Chromatographic-
Marxaladda wareegta, isku darka xalinta, diyaarinta caadiga ah, xalinta xallinta, iyo nidaamka Chromatographic-ku soco sida lagu faray Imtixaanka.
Tijaabi xalka-Isticmaal diyaarinta Assay.
Habka-Chromatograph ee xalka Tijaabada sida lagu faray Habka Assay, taasoo u oggolaanaysa chromatography inuu kordhiyo ilaa saddex jeer wakhtiga haynta ketorolac.Cabir jawaabaha dhammaan meelaha ugu sarreeya.Xisaabi boqolkiiba nijaasta shakhsi kasta ee qaybta Ketorolac Tromethamine ee ay qaadatay qaacidada:
100rfi (ri / rs)
taas oo rfi ay tahay jawaabta ugu sarreysa ee nijaasta shaqsi kasta marka loo eego kan ketorolac;ri waa jawaabta ugu sarreysa ee wasakh kasta;iyo rs waa wadarta dhammaan jawaabaha ugu sarreeya ee meelaha ugu sarreeya ee wasakhaysan iyo ketorolac ugu sarreeya.Qiimayaasha rfi waa 0.52 ketorolac 1-keto analooga, 0.67 ee ketorolac 1-hydroxy analooga, 2.2 ee ugu sarreysa wasakhda leh ee haynta wakhtiga 0.54 marka loo eego kan ketorolac, iyo 0.91 marka loo eego heerka ugu sarreeya ee wasakhda wakhtiga haynta qaraabo ah. ee 0.66.In aan ka badnayn 0.1% analooga ketorolac 1-keto ama analooga ketorolac 1-hydroxy waa la helay;aan ka badnayn 0.5% wasakh kasta oo kale ayaa la helaa;iyo wadarta dhammaan wasakhda aan ka badnayn 1.0%.
Imtixaan-
Marxaladda wareegta-Ku mil 5.75 g oo ah monobasic ammonium phosphate 1000 ml oo biyo ah, oo ku hagaaji aashitada phosphoric pH ah 3.0.U diyaari isku dhafka la sifeeyay oo soo degsaday ee xalkan kaydinta iyo tetrahydrofuran (70:30).Samee hagaajin haddii loo baahdo (fiiri Habboonaanta Nidaamka ee hoos timaada Chromatography <621>) si aad u gaadho wakhtiga haynta ketorolac ee ku saabsan 8 ilaa 12 daqiiqo.
Isku darka dareeraha-diyaari isku dhafka biyaha iyo tetrahydrofuran (70:30).
Diyaarinta caadiga ah-Tirada si sax ah u milmaan tirada USP Ketorolac Tromethamine RS ee isku-darka Solvent si aad u hesho xal la og yahay oo ku saabsan 0.4 mg halkii ml.[FIIRO GAAR AH-Xalkan ka ilaali iftiinka.]
Diyaarinta Assay-Ku wareeji qiyaastii 20 mg ee Ketorolac Tromethamine, oo si sax ah loo miisaamay, ilaa 50-mL weel mug leh, ku milo isku darka Solvent ilaa mugga, oo qas.[FIIRO GAAR AH-Xalkan ka ilaali iftiinka.]
Xallinta xallinta-In kala-soocida 250-mL isku darka 100 ml oo biyo ah, 100 ml dichloromethane, 30 mg USP Ketorolac Tromethamine RS, iyo 1 mL oo ah 1 N hydrochloric acid.Geli joojiyaha, rux, oo u ogolow lakabyada inay kala tagaan.U wareeji lakabka hoose ee dichloromethane kuna wareeji weelka galaaska borosilicate ee joogsan, oo tuur lakabka sare.U soo bandhig xalka dichloromethane iftiinka qorraxda tooska ah 10 ilaa 15 daqiiqo.Ku wareeji 1.0 mL ee xalka dhalo, ku uumi hawo hadda jirta ama qulqulka nitrogen si uu u engego, ku dar 1.0 mL oo isku dar ah Solvent, oo u wareeg si aad u milanto.[FIIRO GAAR AH-Xalkan waxaa lagu kaydin karaa qaboojiyaha hoostiisa waxaana loo isticmaali karaa ilaa inta chromatogram-ka la helay sida lagu faray Habraaca uu ku habboon yahay in lagu aqoonsado meelaha ugu sarreeya sababtoo ah ketorolac 1-keto analoogga iyo ketorolac 1-hydroxy analog, iyo cabbirka xallinta Inta u dhaxaysa ketorolac 1-keto analooga iyo ketorolac.]
Nadaamka Chromatographic (eeg Chromatography <621>)—Kromaatograph-ka dareeraha ah waxa uu ku qalabaysan yahay 313-nm detector iyo 4.6-mm × 25-cm tiir oo ka kooban 5-µm baakad L7 waxaana lagu hayaa heerkul joogto ah oo qiyaastii 40° ah.Heerka socodka waa qiyaastii 1.5 mL daqiiqadii.Chromatograph ee xallinta xallinta, oo qor jawaabaha ugu sarreeya sida lagu faray Habraaca: waqtiyada haynta qaraabo waxay ku dhow yihiin 0.63 ee ketoroac 1-hydroxy analooga, 0.89 ee ketorolac 1-keto analoogga, iyo 1.0 ee ketorolac;iyo xallinta, R, inta u dhaxaysa ketorolac 1-keto analoogga iyo ketorolac aan ka yarayn 1.5.Chromatograph ee heerka diyaarinta, oo qor jawaabaha ugu sarreeya sida lagu faray Habka: waxtarka tiirka kama yara 5500 taarikada aragtida;iyo leexashada heerka qaraabo ee cirbadaha soo noqnoqda kama badna 1.5%.
Habka-Si gooni ah u duri mugga siman (qiyaastii 10 µL) ee diyaarinta Heerka iyo diyaarinta Assay chromatograph-ka, duub chromatogram-yada, oo cabbir jawaabaha meelaha ugu sarreeya.Xisaabi tirada, mg, ee C15H13NO3 · C4H11NO3 ee qaybta Ketorolac Tromethamine ee ay qaadatay qaacidada:
50C (rU / rS)
taas oo C ay tahay xoojinta, mg per mL, ee USP Ketorolac Tromethamine RS ee diyaarinta Standard;iyo rU iyo rS waa jawaabaha ketorolac ugu sarreeya ee laga helay diyaarinta Assay iyo diyaarinta Heerka, siday u kala horreeyaan.