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

Ketorolac Tromethamine lili osachepera 98,5 peresenti osati oposa 101,5 peresenti ya C15H13NO3 · C4H11NO3, masamu pa zouma maziko.
Kupaka ndi kusunga-Sungani zotengera zolimba, zosagwira kuwala.Sungani pa 25 °, maulendo amaloledwa pakati pa 15 ° ndi 30 °
Miyezo yolozera ya USP <11>-
USP Ketorolac Tromethamine RS
Chizindikiritso-
A: Infrared mayamwidwe <197K>.
B: Mayamwidwe a Ultraviolet <197U>-
Yankho: 10 µg pa mL
Chapakati: methanol.
C: Tromethamine test-Konzani njira Standard ya USP Ketorolac Tromethamine RS mu osakaniza dichloromethane ndi methanol (2: 1) munali 5 mg pa mL.Mofananamo kukonzekera mayeso njira ya Ketorolac Tromethamine munali 5 mg pa mililita.Ikani ma voliyumu a 40-µL a yankho la Standard ndi yankho loyesa ku mbale yopyapyala ya chromatographic (onani Chromatography <621>) yokutidwa ndi wosanjikiza wa 0.25-mm wa chromatographic silica gel osakaniza.Ikani mbaleyo mu chipinda cha chromatographic chomwe kale chinali chosakanikirana ndi dichloromethane, acetone, ndi glacial acetic acid (95:5:2).Tsekani chipindacho, ndipo pangani chromatogram mpaka kutsogolo kwa zosungunulira kusuntha pafupifupi magawo atatu mwa anayi a utali wa mbaleyo.Chotsani mbale m'chipindacho, ndipo mulole zosungunulira zisungunuke.Thirani mbaleyo ndi mankhwala oledzeretsa omwe angokonzedwa kumene okhala ndi 30 mg wa ninhydrin pa mL, ndi kutentha mbaleyo pafupifupi 150 ° kwa mphindi ziwiri kapena zisanu.Mawanga achikasu okhala ndi malire apinki mpaka ofiirira amakula pambale m'malo omwe njira ya Standard ndi yankho loyesa linagwiritsidwa ntchito.
pH <791>: pakati pa 5.7 ndi 6.7, mu yankho (1 mu 100).
Kutaya pakuyanika <731> -Iwunitsani mu vacuum pa 60 ° kwa maola atatu: imataya osapitirira 0.5% ya kulemera kwake.
Zotsalira pakuyatsa <281>: osapitirira 0.1%.
Zitsulo zolemera, Njira II <231>: 0.002%.
Chromatographic chiyero -
Mobile phase, Solvent mix, Standard kukonzekera, Resolution solution, ndi Chromatographic system-Pitirizani monga momwe zalembedwera mu Assay.
Njira yothetsera-Gwiritsani ntchito kukonzekera kwa Assay.
Procedure-Chromatograph The Test solution monga momwe amachitira mu Assay, kulola chromatography kuti ipitirire katatu kuposa nthawi yosungira ketorolac.Yezerani mayankho a nsonga zonse.Kuwerengera kuchuluka kwa zodetsa za munthu aliyense mu gawo la Ketorolac Tromethamine yotengedwa ndi chilinganizo:
100rfi (ri / rs)
momwe rfi ndi yankho la munthu aliyense pachimake chonyansa chokhudzana ndi ketorolac;ri ndiye yankho lapamwamba pa chodetsa chilichonse;ndipo rs ndiye chiŵerengero cha mayankho onse apamwamba a nsonga zonyansa ndi nsonga yayikulu ya ketorolac.Miyezo ya rfi ndi 0,52 ya analogi ya ketorolac 1-keto, 0,67 ya analogi ya ketorolac 1-hydroxy, 2.2 pachimake chonyansa chokhala ndi nthawi yosungira 0,54 poyerekeza ndi ketorolac, ndi 0,91 pachimake chonyansa panthawi yosunga. pa 0,66.Osapitirira 0,1% ya ketorolac 1-keto analogi kapena ketorolac 1-hydroxy analogi amapezeka;osapitirira 0.5% ya zonyansa zina zilizonse zomwe zimapezeka;ndipo kuchuluka kwa zonyansa zonse sikuposa 1.0%.
Kuyesa-
Mobile phase-Sungani 5.75 g wa monobasic ammonium phosphate mu 1000 ml ya madzi, ndi kusintha ndi asidi phosphoric kuti pH ya 3.0.Konzani osakaniza osefedwa ndi degassed wa buffer yankho ndi tetrahydrofuran (70:30).Sinthani ngati kuli kofunikira (onani Kukwanira Kwadongosolo pansi pa Chromatography <621>) kuti mukwaniritse nthawi yosungira ketorolac pafupifupi mphindi 8 mpaka 12.
Kusakaniza kosungunulira-Konzani madzi osakaniza ndi tetrahydrofuran (70:30).
Standard kukonzekera-Quantitatively Sungunulani molondola kulemera kuchuluka kwa USP Ketorolac Tromethamine RS mu zosungunulira osakaniza kupeza yankho kukhala odziwika ndende pafupifupi 0,4 mg wa pa mililita.[Dziwani-Tetezani yankho ili ku kuwala.]
Kukonzekera koyesa-Kusamutsa pafupifupi 20 mg wa Ketorolac Tromethamine, woyezedwa molondola, ku botolo la volumetric 50-mL, sungunulani ndi zosungunulira zosakaniza mpaka voliyumu, ndi kusakaniza.[Dziwani-Tetezani yankho ili ku kuwala.]
Resolution solution-Mu 250-mL separator mix 100 ml ya madzi, 100 ml ya dichloromethane, 30 mg ya USP Ketorolac Tromethamine RS, ndi 1 mL ya 1 N hydrochloric acid.Ikani choyimitsira, gwedezani, ndi kulola kuti zigawozo zilekanitse.Chotsani gawo lapansi la dichloromethane ku botolo lagalasi loyimitsidwa la borosilicate, ndikutaya wosanjikiza wapamwamba.Onetsani njira ya dichloromethane kuti muwongolere kuwala kwa dzuwa kwa mphindi 10 mpaka 15.Chotsani 1.0 mL ya yankho ku vial, sungunuke mumlengalenga kapena mumtsinje wa nayitrogeni kuti uume, onjezerani 1.0 mL ya zosungunulira zosakaniza, ndi kuzungulira kuti zisungunuke.[DZIWANI-Iyi yankho likhoza kusungidwa mufiriji ndikugwiritsidwa ntchito malinga ngati chromatogram yomwe inapezedwa monga momwe idalangizidwira Njira ndiyoyenera kuzindikira nsonga za ketorolac 1-keto analogi ndi ketorolac 1-hydroxy analogi, ndi kuyeza chiganizo. pakati pa ketorolac 1-keto analog ndi ketorolac.]
Chromatographic system (onani Chromatography <621>)— Chromatograph yamadzimadzi imakhala ndi chowunikira cha 313-nm ndi ndime ya 4.6-mm × 25-cm yomwe ili ndi 5-µm yopakidwa L7 ndipo imasungidwa kutentha kosasintha kwa pafupifupi 40°.Kuthamanga kwa madzi ndi pafupifupi 1.5 ml pa mphindi.Chromatograph the Resolution solution, ndi kulemba mayankho pachimake monga momwe adanenera Ndondomeko: nthawi yosungirako ndi pafupifupi 0,63 ya analogi ya ketoroac 1-hydroxy, 0,89 ya ketorolac 1-keto analogi, ndi 1.0 ya ketorolac;ndi kusamvana, R, pakati pa ketorolac 1-keto analogi ndi ketorolac si osachepera 1.5.Chromatograph the Standard kukonzekera, ndikujambulitsa mayankho apamwamba monga momwe adayankhidwira Ndondomeko: magwiridwe antchito amzanja si ochepera 5500 theoretical plates;ndipo kupatuka kofanana kwa jakisoni wobwereza sikudutsa 1.5%.
Kachitidwe-Papatula jekeseni ma voliyumu ofanana (pafupifupi 10 µL) a Kukonzekera Kwanthawi zonse ndi kukonzekera kwa Assay mu chromatograph, lembani ma chromatogram, ndikuyesa mayankho a nsonga zazikulu.Werengetsani kuchuluka, mu mg, wa C15H13NO3·C4H11NO3 mu gawo la Ketorolac Tromethamine yotengedwa ndi formula:
50C(rU / rS)
momwe C ndi ndende, mu mg pa mL, wa USP Ketorolac Tromethamine RS mu kukonzekera Standard;ndi rU ndi rS ndi mayankho apamwamba a ketorolac omwe amapezeka kuchokera ku Assay kukonzekera ndi kukonzekera Standard, motsatira.