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

Ketorolac Tromethamine ya ƙunshi ba kasa da 98.5 bisa dari kuma bai wuce 101.5 bisa dari na C15H13NO3 · C4H11NO3, lasafta a kan busasshen tushe.
Marufi da ajiya-Ajiye a cikin matsatsi, kwantena masu jure haske.Ajiye a 25°, balaguron balaguro ya halatta tsakanin 15° da 30°
Matsayin Magana na USP <11>-
USP Ketorolac Tromethamine RS
Ganewa-
A: Ciwon Infrared <197K>.
B: Ƙarfafawar Ultraviolet <197U>-
Magani: 10 μg kowace ml
Matsakaici: methanol.
C: Gwajin Tromethamine-Shirya daidaitaccen bayani na USP Ketorolac Tromethamine RS a cikin cakuda dichloromethane da methanol (2: 1) mai ɗauke da 5 MG kowace ml.Hakazalika shirya maganin gwajin Ketorolac Tromethamine dauke da 5 MG kowace ml.Aiwatar da juzu'i 40-µL na daidaitaccen bayani da maganin gwajin zuwa farantin chromatographic na bakin ciki-Layer (duba Chromatography <621>) mai rufi da 0.25-mm Layer na chromatographic silica gel cakuda.Sanya farantin a cikin ɗakin chromatographic a baya wanda aka daidaita tare da cakuda dichloromethane, acetone, da glacial acetic acid (95: 5: 2).Rufe ɗakin, kuma haɓaka chromatogram har sai gaban ƙarfi ya motsa kusan kashi uku cikin huɗu na tsawon farantin.Cire farantin daga ɗakin, kuma ƙyale sauran ƙarfi ya ƙafe.Fesa farantin tare da sabon shiri na barasa mai dauke da 30 MG na ninhydrin a kowace ml, kuma a zafi farantin a kusan 150 ° na minti 2 zuwa 5.Rawaya spots tare da ruwan hoda zuwa shunayya iyakoki suna tasowa akan farantin a cikin wuraren da aka yi amfani da daidaitaccen bayani da maganin gwajin.
pH <791>: tsakanin 5.7 da 6.7, a cikin wani bayani (1 a 100).
Asarar bushewa <731> - bushe shi a cikin injin daskarewa a 60 ° na tsawon awanni 3: bai wuce 0.5% na nauyinsa ba.
Ragowa akan kunnawa <281>: bai wuce 0.1% ba.
Karfe masu nauyi, Hanyar II <231>: 0.002%.
Tsaftar Chromatographic-
Lokacin Wayar hannu, Cakudar Solvent, Daidaitaccen shiri, Maganin ƙuduri, da tsarin Chromatographic-Ci gaba kamar yadda aka umurce a cikin Assay.
Maganin gwaji-Yi amfani da shirye-shiryen Assay.
Tsari-Chromatograph Maganin Gwajin kamar yadda aka umurce shi don Tsari a cikin Assay, yana barin chromatography ya ƙara zuwa sau uku lokacin riƙe ketorolac.Auna martanin duk kololuwa.Yi ƙididdige yawan ƙazantar kowane mutum a cikin ɓangaren Ketorolac Tromethamine wanda aka ɗauka ta dabara:
100rfi (ri / rs)
wanda rfi shine matakin mayar da martani na kowane kololuwar ƙazanta dangane da na ketorolac;ri shine kololuwar amsa ga kowane kazanta;kuma rs shine jimlar duk kololuwar martani na kololuwar ƙazanta da babban kololuwar ketorolac.Ma'aunin rfi shine 0.52 na ketorolac 1-keto analog, 0.67 na ketorolac 1-hydroxy analog, 2.2 don ƙarancin ƙazanta yana da lokacin riƙewa na 0.54 dangane da na ketorolac, da 0.91 don ƙazanta kololuwa a lokacin riƙewar dangi. daga 0.66.Ba fiye da 0.1% na ketorolac 1-keto analog ko na ketorolac 1-hydroxy ana samun su;ba fiye da 0.5% na duk wani ƙazanta da aka samu ba;kuma jimillar duk najasa bai wuce 1.0% ba.
Assay-
Lokacin wayar hannu-Narke 5.75 g na monobasic ammonium phosphate a cikin 1000 ml na ruwa, kuma daidaita tare da phosphoric acid zuwa pH na 3.0.Shirya cakuda da aka tace da kuma gurɓatacciyar wannan maganin buffer da tetrahydrofuran (70:30).Yi gyare-gyare idan ya cancanta (duba Dacewar Tsarin ƙarƙashin Chromatography <621>) don cimma lokacin riƙewa na ketorolac na kusan mintuna 8 zuwa 12.
Cakuda mai narkewa-Shirya cakuda ruwa da tetrahydrofuran (70:30).
Daidaitaccen shiri-Yawan narkar da adadin USP Ketorolac Tromethamine RS daidai gwargwado a cikin cakudawar Solvent don samun maganin sananniya na kusan 0.4 MG kowace ml.[NOTE-Kare wannan maganin daga haske.]
Shirye-shiryen Assay-Canja wurin kusan 20 MG na Ketorolac Tromethamine, daidai aunawa, zuwa filaye mai girma na 50-mL, tsoma tare da cakuda Solvent zuwa girma, da haɗuwa.[NOTE-Kare wannan maganin daga haske.]
Maganin ƙuduri-A cikin mai raba 250-ml na ruwa 100 ml na ruwa, 100 ml na dichloromethane, 30 MG na USP Ketorolac Tromethamine RS, da 1 ml na 1 N hydrochloric acid.Saka abin tsayawa, girgiza, kuma ba da damar yadudduka su rabu.Canja wurin ƙananan dichloromethane Layer zuwa gilashin borosilicate mai tsayawa, kuma jefar da babban Layer.Fitar da maganin dichloromethane zuwa hasken rana kai tsaye na mintuna 10 zuwa 15.Canja wurin 1.0 ml na maganin zuwa vial, ƙafe a cikin iska a halin yanzu ko a cikin rafi na nitrogen zuwa bushewa, ƙara 1.0 ml na cakuda Solvent, da juyawa don narkewa.[NOTE-Wannan maganin ana iya adana shi a cikin firiji kuma a yi amfani dashi muddin chromatogram da aka samu kamar yadda aka umurce shi don Tsarin tsari ya dace don gano kololuwa saboda ketorolac 1-keto analog da ketorolac 1-hydroxy analog, kuma don auna ƙuduri. tsakanin ketorolac 1-keto analog da ketorolac.]
Tsarin Chromatographic (duba Chromatography <621>)) -Cromatograph na ruwa yana sanye da na'urar ganowa na 313-nm da ginshiƙin 4.6-mm × 25-cm wanda ya ƙunshi 5-µm packing L7 kuma ana kiyaye shi a koyaushe a zazzabi na kusan 40°.Matsakaicin kwarara shine kusan 1.5 ml a minti daya.Chromatograph da Resolution bayani, da rikodin mafi girman martani kamar yadda aka umurce don Tsara: lokutan riƙewa na dangi kusan 0.63 na ketoroac 1-hydroxy analog, 0.89 na ketorolac 1-keto analog, da 1.0 don ketorolac;da ƙuduri, R, tsakanin ketorolac 1-keto analog da ketorolac bai kasance ƙasa da 1.5 ba.Chromatograph da Daidaitaccen shiri, da yin rikodin martanin kololuwa kamar yadda aka umurce su don Tsari: ingancin ginshiƙi baya ƙasa da faranti na ka'idar 5500;kuma madaidaicin ma'auni na dangi don kwafin injections bai wuce 1.5%.
Tsari-Na dabam allura daidai juzu'i (kimanin 10 µL) na daidaitaccen shiri da shirye-shiryen Assay a cikin chromatograph, yi rikodin chromatograms, da auna martani ga manyan kololuwa.Yi ƙididdige adadin, a cikin MG, na C15H13NO3 · C4H11NO3 a cikin ɓangaren Ketorolac Tromethamine wanda aka ɗauka ta dabara:
50C (rU / rS)
wanda C shine maida hankali, a cikin MG da ml, na USP Ketorolac Tromethamine RS a cikin Shirye-shiryen Standard;da rU da rS sune martanin kololuwar ketorolac da aka samu daga shirye-shiryen Assay da Daidaitaccen shiri, bi da bi.