Enalapril Maleate CAS 76095-16-4 Assay 98.0~102.0% API High Purity

Enalapril Maleate
C20H28N2O5·C4H4O4 492.52
l-Proline, 1-[N-[1-(ethoxycarbonyl)-3-phenylpropyl]-l-alanyl]-, (S)-, (Z)-2-butenedioate (1:1).
1-[N-[(S)-1-Carboxy-3-phenylpropyl]-l-alanyl] -l-proline 1'-ethyl ester, maleate (1: 1) [76095-16-4].
I-Enalapril Maleate iqulethe ngaphantsi kweepesenti ze-98.0 kwaye ingabi ngaphezu kwe-102.0 ipesenti ye-C20H28N2O5 · C4H4O4, ibalwa kwisiseko esomileyo.
Ukupakishwa kunye nokugcinwa-Londoloza kwizikhongozeli ezivaliweyo kakuhle, kwaye ugcine kwiqondo lokushisa elilawulwayo.
Imigangatho yezalathiso ye-USP <11>-
USP Enalapril Maleate RS Cofa ukujonga iSakhiwo
Isazisi-
A: I-Infrared Absorption <197M>.
B: Ixesha lokugcinwa kwencopho enkulu kwichromatogram yoLungiselelo lwe-Assay ihambelana naleyo kwichromatogram yoLungiselelo oluMgangatho, njengoko lufunyenwe kwi-Assay.
Ukujikeleza okuthe ngqo <781S>: phakathi kwe -41.0 kunye -43.5.
Isisombululo sovavanyo: 10 mg nge-mL, kwi-methanol.
Ilahleko ekumiseni <731>-Yomisa kwi-vacuum kwixinzelelo elingadluli kwi-5 mm ye-mercury kwi-60 kwiiyure ze-2: ilahlekelwa ngaphezu kwe-1.0% yobunzima bayo.
Intsalela ekutshiseni <281>: hayi ngaphezulu kwe-0.2%.
Iintsimbi ezinzima, Indlela II <231>: 0.001%.
Iikhompawundi ezinxulumene-
pH 6.8 Phosphate buffer, pH 2.5 Phosphate buffer, Solution A, Solution B, Mobile phase, Diluent, Enalapril diketopiperazine solution, Isisombululo sokufaneleka kweSistim, kunye neChromatographic system- Qhubeka njengoko kuchazwe kwi-Assay.
Isisombululo esisemgangathweni-Nyibilikisa isixa esinomlinganiso ngokuchanekileyo we-USP Enalapril Maleate RS kwiDiluent, kwaye nciphisa ngokobungakanani, kwaye ngokwenyathelo xa kuyimfuneko, ngeDiluent ukufumana isisombululo esinoxinzelelo olwaziwayo malunga ne-3 µg ngemL.
Isisombululo sovavanyo-Sebenzisa ukulungiswa koVavanyo.
Inkqubo-Ngokwahlukileyo tofa imithamo elinganayo (malunga nama-50 µL) yoMgangatho wesisombululo kunye nesisombululo soVavanyo kwichromatograph, urekhode iichromatograms, kwaye ulinganise iimpendulo zengingqi yencopho.Bala ipesenti yokungahlambuluki ngakunye kwisahlulo se-Enalapril Maleate esithathwe ngefomula:
100(CS / CT)(ri / rS)
apho i-CS i-concentration, kwi-mg nge-mL, ye-USP Enalapril Maleate RS kwisisombululo soMgangatho;I-CT yingqwalasela, kwi-mg nge-mL, ye-Enalapril Maleate kwisisombululo soVavanyo;ri yindawo encopho yokungcola ngakunye okufunyenwe kwisisombululo soVavanyo;kunye ne-rS yindawo ephezulu ye-enalapril efunyenwe kwisisombululo esiPhakathi: akukho ngaphezu kwe-1.0% yokungcola okunexesha lokugcinwa kwesalamane malunga ne-1.10 ifunyenwe;hayi ngaphezulu kwe-0.3% yako nakuphi na okunye ukungcola komntu okufunyenweyo;kwaye akukho ngaphezu kwe-2% yokungcola okupheleleyo okufunyenweyo.
Isivavanyi-
pH 6.8 Phosphate buffer-Dibanisa i-2.8 g ye-monobasic sodium phosphate malunga ne-900 mL yamanzi kwi-1000-mL ye-volumetric flask.Lungisa kunye ne-9 M isisombululo se-sodium hydroxide kwi-pH malunga ne-6.8, hlambulula ngamanzi ukuya kumthamo, kwaye udibanise.
pH 2.5 Phosphate buffer-Dibanisa i-2.8 g ye-monobasic sodium phosphate malunga ne-900 mL yamanzi kwi-1000-mL ye-volumetric flask.Lungisa nge-asidi ye-phosphoric ukuya kwi-pH malunga ne-2.5, nciphisa ngamanzi ukuya kwivolumu, kwaye udibanise.
Isisombululo A-Lungisa umxube ohluziweyo kunye ne-degassed pH 6.8 Phosphate buffer kunye ne-acetonitrile (19: 1).
Isisombululo B-Lungisa umxube ohluziweyo kunye ne-degassed ye-acetonitrile kunye ne-pH 6.8 i-Phosphate buffer (33:17).
Isigaba esiphathwayo-Sebenzisa imixube eguquguqukayo yeSisombululo A kunye neSisombululo B njengoko kumiselwe inkqubo yeChromatographic.Yenza uhlengahlengiso xa kukho imfuneko (jonga ukufaneleka kweNkqubo phantsi kweChromatography 621).
I-Diluent-Lungisa umxube we-pH 2.5 Phosphate buffer kunye ne-acetonitrile (95: 5).
Isisombululo se-Enalapril diketopiperazine-Beka ngononophelo malunga ne-20 mg ye-USP Enalapril Maleate RS kwi-100-mL yebeaker ukwenza ingqumba emazantsi ebhekile.Beka ibhekile kwipleyiti eshushu malunga nesiqingatha sobona bushushu beqondo lobushushu beqondo eliphezulu.Fudumeza malunga nemizuzu emi-5 ukuya kweli-10 de okuqinileyo kunyibilike.Kwangoko susa ibhekile kwipleyiti eshushu, kwaye uyivumele iphole.[Qaphela-Kuphephe ukutshisa kakhulu ukukhusela ukuthotywa okubangelwa bubushushu, okuya kubangela umbala omdaka.] Kwintsalela epholileyo kwi-beaker yongeza i-50 mL ye-acetonitrile, kwaye i-sonicate imizuzu embalwa ukunyibilika.Isisombululo sikholisa ukuba, kwi-mL nganye, phakathi kwe-0.2 mg kunye ne-0.4 mg ye-enalapril diketopiperazine.
Ukulungiswa okusemgangathweni-Nxibilikisa isixa esikaliniweyo ngokuchanekileyo se-USP Enalapril Maleate RS kwi-Diluent, kwaye nciphisa ngokobuninzi, kunye ne-stepwise ukuba kuyimfuneko, kunye ne-Diluent ukufumana isisombululo esinoxinzelelo olwaziwayo malunga ne-0.3 mg nge-mL.
Isisombululo sokufaneleka kwenkqubo-Yongeza i-1 mL yesisombululo se-Enalapril diketopiperazine kwisahlulo se-50-mL yoLungiso oluMgangatho, kunye nokuxuba.
Ukulungiswa kwe-Assay- Dlulisa malunga ne-30 mg ye-Enalapril Maleate, ilinganiswe ngokuchanekileyo, kwi-flask ye-volumetric ye-100-mL, chitha kwaye udibanise nge-Diluent ukuya kwivolumu, kwaye udibanise.
Inkqubo yeChromatographic (jonga iChromatography <621>) -I-chromatograph yolwelo ixhotyiswe nge-215-nm detector kunye nekholamu ye-4.1-mm × 15-cm equlethe ukupakisha i-L21.Izinga lokuhamba malunga ne-1.5 mL ngomzuzu.Ubushushu bekholomu bugcinwa kwi-70. I-chromatograph ihlelwe ngolu hlobo lulandelayo.
Ixesha (imizuzu) Isisombululo A(%) Isisombululo B (%) Ululo
0 95 5 ulungelelwaniso
0-20 95→40 5→60 umgca wodidi
20-25 40 60 isokhrasi
25-26 40→95 60→5 umgca wodidi
26-30 95 5 isokhrasi
I-Chromatograph isisombululo sokufaneleka kweSistim, kwaye urekhode iimpendulo eziphezulu njengoko zichazwe kwiNkqubo: amaxesha okugcinwa okuhambelanayo malunga ne-1.0 ye-enalapril kunye ne-2.1 ye-enalapril diketopiperazine;kunye nesisombululo, R, phakathi kwe-enalapril kunye ne-enalapril diketopiperazine ayikho ngaphantsi kwe-3.5.I-Chromatograph Ukulungiswa koMgangatho, kwaye urekhode iimpendulo eziphakamileyo njengoko ziqondiswe kwiNkqubo: ukutenxa komgangatho ohambelanayo we-replicate injection ayikho ngaphezu kwe-1.0%.
Inkqubo- Ngokwahlukileyo tofa imithamo elinganayo (malunga nama-50 µL) yoLungiselelo oluMgangatho noLungiselelo loVavanyo kwichromatograph, urekhode iichromatogram, kwaye ulinganise iimpendulo zeencopho ezinkulu.Bala ubuninzi, kwi-mg, ye-C20H28N2O5·C4H4O4 kwisahlulo se-Enalapril Maleate esithathwe ngefomula:
100C(rU / rS)
apho i-C igxininise, kwi-mg nge-mL, ye-USP Enalapril Maleate RS kulungiselelo loMgangatho;kunye ne-rU kunye ne-rS yincopho yeempendulo ezifunyenwe kulungiselelo loVavanyo kunye nolungiselelo loMgangatho, ngokulandelelanayo.