Enalapril Maleate CAS 76095-16-4 Assay 98.0 ~ 102.0% API Siab 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, txiv neej (1: 1) [76095-16-4].
Enalapril Maleate muaj tsis pub tsawg dua 98.0 feem pua ​​thiab tsis ntau tshaj 102.0 feem pua ​​​​ntawm C20H28N2O5·C4H4O4, xam ntawm lub hauv paus qhuav.
Ntim thiab khaws cia-Txuag hauv cov thawv kaw kom zoo, thiab khaws cia ntawm chav tsev kub.
USP Reference cov qauv <11>-
USP Enalapril Maleate RS Nyem rau Saib Cov Qauv
Kev txheeb xyuas-
A: Infrared Absorption <197M>.
B: Lub sijhawm khaws cia ntawm lub ncov loj hauv chromatogram ntawm Assay kev npaj sib raug rau qhov ntawd nyob rau hauv chromatogram ntawm Standard npaj, raws li tau txais hauv Assay.
Kev sib hloov tshwj xeeb <781S>: nruab nrab ntawm -41.0 thiab -43.5.
Test tov: 10 mg ib mL, hauv methanol.
Poob ntawm ziab <731>-Sry hauv lub tshuab nqus tsev ntawm lub siab tsis tshaj 5 hli mercury ntawm 60 rau 2 teev: nws poob tsis ntau tshaj 1.0% ntawm nws qhov hnyav.
Residue ntawm ignition <281>: tsis ntau tshaj 0.2%.
Cov hlau hnyav, Txoj Kev II <231>: 0.001%.
Related compounds-
pH 6.8 Phosphate buffer, pH 2.5 Phosphate buffer, tshuaj A, tshuaj B, Txawb theem, Diluent, Enalapril diketopiperazine tov, System suitability tov, thiab Chromatographic system - Ua raws li qhia hauv Assay.
Cov txheej txheem kev daws teeb meem-Dissolve ib qho hnyav hnyav ntawm USP Enalapril Maleate RS hauv Diluent, thiab dilute kom muaj nuj nqis, thiab stepwise yog tias tsim nyog, nrog Diluent kom tau txais cov tshuaj uas muaj kev paub txog ntawm li 3 µg ib mL.
Test solution-Siv qhov Assay npaj.
Cov txheej txheem-Kev txhaj tshuaj sib npaug (kwv yees li 50 µL) ntawm cov txheej txheem kev daws teeb meem thiab cov tshuaj ntsuam xyuas rau hauv chromatograph, sau cov chromatograms, thiab ntsuas cov lus teb hauv cheeb tsam siab.Xam cov feem pua ​​​​ntawm txhua qhov impurity hauv ib feem ntawm Enalapril Maleate coj los ntawm cov mis:
100 (CS / CT) (ri / rS)
nyob rau hauv uas CS yog qhov concentration, nyob rau hauv mg ib mL, ntawm USP Enalapril Maleate RS nyob rau hauv tus txheej txheem tov;CT yog qhov concentration, hauv mg ib mL, ntawm Enalapril Maleate hauv cov tshuaj ntsuam xyuas;ri yog thaj chaw ncov ntawm txhua qhov impurity tau los ntawm Kev Ntsuas Kev Ntsuas;thiab rS yog thaj chaw ncov ntawm enalapril tau los ntawm cov txheej txheem kev daws teeb meem: tsis pub ntau tshaj 1.0% ntawm cov impurity uas muaj cov txheeb ze tuav lub sijhawm kwv yees li 1.10;tsis pub ntau tshaj 0.3% ntawm lwm tus neeg impurity raug pom;thiab tsis pub ntau tshaj 2% ntawm tag nrho cov impurities pom.
Assay-
pH 6.8 Phosphate buffer-Dissolve 2.8 g ntawm monobasic sodium phosphate nyob rau hauv li 900 mL dej hauv 1000-mL volumetric hwj.Kho nrog 9 M sodium hydroxide tov rau pH txog 6.8, dilute nrog dej rau ntim, thiab sib tov.
pH 2.5 Phosphate buffer-Dissolve 2.8 g ntawm monobasic sodium phosphate nyob rau hauv txog 900 mL dej hauv 1000-mL volumetric hwj.Kho nrog phosphoric acid rau pH txog 2.5, dilute nrog dej rau ntim, thiab sib tov.
Tshuaj A-Npaj lim thiab degassed sib tov ntawm pH 6.8 Phosphate tsis thiab acetonitrile (19:1).
Tshuaj B-Npaj lim thiab degassed sib tov ntawm acetonitrile thiab pH 6.8 Phosphate tsis (33:17).
Txawb theem-Siv sib txawv sib txawv ntawm cov tshuaj A thiab tshuaj B raws li qhia rau Chromatographic system.Hloov kho yog tias tsim nyog (saib System Suitability hauv Chromatography 621).
Diluent-Npaj sib tov ntawm pH 2.5 Phosphate tsis thiab acetonitrile (95: 5).
Enalapril diketopiperazine tov- Ua tib zoo tso li 20 mg ntawm USP Enalapril Maleate RS hauv 100-mL beaker los tsim ib mound rau hauv qab ntawm lub beaker.Muab lub khob rau ntawm lub phaj kub ntawm ib nrab ntawm qhov siab tshaj plaws kub phaj kub qhov chaw.Tshav kub li 5 mus rau 10 feeb kom txog thaum cov khoom yog yaj.Tam sim ntawd tshem lub beaker los ntawm lub phaj kub, thiab cia kom txias.[ceeb toom-Tsis txhob overheating los tiv thaiv tshav kub-induced degradation, uas yuav ua rau ib tug xim av xim.] mus rau lub txias residue nyob rau hauv lub beaker ntxiv 50 mL ntawm acetonitrile, thiab sonicate rau ob peb feeb kom yaj.Cov tshuaj feem ntau muaj, hauv txhua mL, ntawm 0.2 mg thiab 0.4 mg ntawm enalapril diketopiperazine.
Cov txheej txheem kev npaj-Dissolve ib qho raug hnyav kom muaj nuj nqis ntawm USP Enalapril Maleate RS hauv Diluent, thiab dilute kom muaj nuj nqis, thiab stepwise yog tias tsim nyog, nrog Diluent kom tau txais cov kev daws teeb meem uas paub txog txog 0.3 mg ib mL.
Kev ua kom haum rau kev daws teeb meem-Ntxiv 1 mL ntawm Enalapril diketopiperazine tov rau 50-mL ib feem ntawm Cov Txheej Txheem Npaj, thiab sib tov.
Kev tshuaj ntsuam xyuas- Hloov txog 30 mg ntawm Enalapril Maleate, ntsuas kom raug, mus rau 100-mL ntim ntim, yaj hauv thiab dilute nrog Diluent rau ntim, thiab sib tov.
Chromatographic system (saib Chromatography <621>)-Cov kua chromatograph yog nruab nrog 215-nm ntes thiab 4.1-mm × 15-cm kem uas muaj cov ntim L21.Tus nqi ntws yog li 1.5 mL ib feeb.Lub kem kub yog khaws cia ntawm 70. Lub chromatograph yog programmed raws li nram no.
Sijhawm(feeb) daws A(%) daws B(%) Elution
0955 sib
0-20 95 → 40 5 → 60 linear gradient
20-25 40 60 ib
25-26 40 → 95 60 → 5 linear gradient
26-30 95 5 ib
Chromatograph qhov kev daws teeb meem tsim nyog, thiab sau cov lus teb siab kawg raws li tau hais tseg rau Txoj Cai: cov sij hawm khaws cov txheeb ze yog kwv yees li 1.0 rau enalapril thiab 2.1 rau enalapril diketopiperazine;thiab kev daws teeb meem, R, nruab nrab ntawm enalapril thiab enalapril diketopiperazine tsis tsawg dua 3.5.Chromatograph tus txheej txheem npaj, thiab sau cov lus teb ncov raws li qhia rau Kev Ua Haujlwm: tus qauv sib txawv ntawm qhov sib txawv rau kev txhaj tshuaj tsis ntau tshaj 1.0%.
Cov txheej txheem - Cais cov ntim sib npaug (kwv yees li 50 µL) ntawm Cov Qauv Npaj thiab Kev Ntsuas Kev Ntsuas rau hauv cov chromatograph, sau cov chromatograms, thiab ntsuas cov lus teb rau qhov loj peaks.Xam qhov ntau, hauv mg, ntawm C20H28N2O5·C4H4O4 hauv feem ntawm Enalapril Maleate coj los ntawm cov mis:
100C (rU / rS)
nyob rau hauv uas C yog qhov concentration, nyob rau hauv mg ib mL, ntawm USP Enalapril Maleate RS nyob rau hauv tus txheej txheem npaj;thiab rU thiab rS yog cov lus teb siab kawg uas tau txais los ntawm Assay npaj thiab Standard npaj, feem.