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].
Enalapril Maleate ili ndi osachepera 98.0 peresenti komanso osapitirira 102.0 peresenti ya C20H28N2O5 · C4H4O4, yowerengedwa pa zouma.
Kupaka ndi kusungirako-Sungani zotengera zotsekedwa bwino, ndi kusunga kutentha kwa chipinda.
Miyezo yolozera ya USP <11>-
USP Enalapril Maleate RS Dinani kuti muwone Kapangidwe
Chizindikiritso-
A: Infuraredi mayamwidwe <197M>.
B: Nthawi yosungira pachimake chachikulu mu chromatogram ya Kukonzekera kwa Assay ikufanana ndi yomwe ili mu chromatogram ya Kukonzekera kwa Standard, monga momwe zapezedwa mu Assay.
Kuzungulira kwachindunji <781S>: pakati pa -41.0 ndi -43.5.
Njira yothetsera mayeso: 10 mg pa mL, mu methanol.
Kutaya pa kuyanika <731> -Kuwumitsa mu vacuum pa kuthamanga kosapitirira 5 mm wa mercury pa 60 kwa maola 2: imataya osapitirira 1.0% ya kulemera kwake.
Zotsalira pakuyatsa <281>: osapitirira 0.2%.
Zitsulo zolemera, Njira II <231>: 0.001%.
Zogwirizana nazo-
pH 6.8 Phosphate buffer, pH 2.5 Phosphate buffer, Solution A, Solution B, Mobile phase, Diluent, Enalapril diketopiperazine solution, System suitability solution, ndi Chromatographic system— Pitirizani motsatira ndondomeko ya Assay.
Sungunulani muyezo woyezera bwino wa USP Enalapril Maleate RS mu Diluent, ndi kusungunula mochulukira, komanso pang'onopang'ono ngati kuli kofunikira, ndi Diluent kuti mupeze yankho lodziwika bwino la pafupifupi 3 µg pa mL.
Njira yothetsera-Gwiritsani ntchito kukonzekera kwa Assay.
Kachitidwe-Mosiyanirana jekeseni ma voliyumu ofanana (pafupifupi 50 µL) a njira Yoyezera ndi Mayeso mu chromatograph, lembani ma chromatogram, ndi kuyeza mayankho amdera lapamwamba.Kuwerengera kuchuluka kwa zodetsa zilizonse mu gawo la Enalapril Maleate zomwe zatengedwa ndi formula:
100 (CS / CT) (ri / rS)
momwe CS ndi ndende, mu mg pa mL, ya USP Enalapril Maleate RS mu Standard solution;CT ndiye ndende, mu mg pa mL, ya Enalapril Maleate mu Mayeso njira;ri ndi malo okwera kwambiri a zonyansa zilizonse zomwe zimapezedwa kuchokera ku Test solution;ndipo rS ndi malo apamwamba kwambiri a enalapril omwe amachokera ku Standard solution: osapitirira 1.0% ya zonyansa zilizonse zomwe zimakhala ndi nthawi yosungirako pafupifupi 1.10 imapezeka;osapitirira 0.3% ya zonyansa zina zilizonse zomwe zimapezeka;ndipo zosaposa 2% ya zonyansa zonse zimapezeka.
Kuyesa-
pH 6.8 Phosphate buffer-Sungani 2.8 g ya monobasic sodium phosphate pafupifupi 900 ml ya madzi mu botolo la volumetric 1000-mL.Sinthani ndi 9 M sodium hydroxide solution ku pH ya pafupifupi 6.8, chepetsani ndi madzi mpaka voliyumu, ndikusakaniza.
pH 2.5 Phosphate buffer-Sungani 2.8 g ya monobasic sodium phosphate pafupifupi 900 ml ya madzi mu botolo la volumetric 1000-mL.Sinthani ndi asidi wa phosphoric kukhala pH ya pafupifupi 2.5, tsitsani ndi madzi mpaka voliyumu, ndikusakaniza.
Yankho A-Konzani zosakaniza zosefedwa ndi zowonongeka za pH 6.8 Phosphate buffer ndi acetonitrile (19:1).
Yankho B-Konzani zosakaniza zosefedwa ndi zowonongeka za acetonitrile ndi pH 6.8 Phosphate buffer (33:17).
Mobile phase-Gwiritsani ntchito zosakanikirana zosakanikirana za Solution A ndi Solution B monga momwe zalembedwera pa Chromatographic system.Sinthani ngati kuli kofunikira (onani Kukwanira Kwadongosolo pa Chromatography 621).
Diluent-Konzani chisakanizo cha pH 2.5 Phosphate buffer ndi acetonitrile (95:5).
Enalapril diketopiperazine solution-Ikani mosamala pafupifupi 20 mg ya USP Enalapril Maleate RS mu beaker ya 100-mL kuti mupange chulu pansi pa beaker.Ikani beaker pa mbale yotentha pafupifupi theka la kutentha kwapamwamba kwambiri.Kutenthetsa kwa mphindi 5 mpaka 10 mpaka cholimba chisungunuke.Nthawi yomweyo chotsani beaker mu mbale yotentha, ndikulola kuti izizizire.[Zindikirani-Pewani kutenthedwa kuti muteteze kuwonongeka kochititsa kutentha, komwe kungapangitse mtundu wa bulauni.] Kuti utakhazikika zotsalira mu beaker kuwonjezera 50 mL wa acetonitrile, ndi sonicate kwa mphindi zingapo kupasuka.Njira yothetsera vutoli imakhala, mu mL iliyonse, pakati pa 0.2 mg ndi 0.4 mg wa enalapril diketopiperazine.
Kukonzekera kokhazikika-Sungani muyeso woyezedwa bwino wa USP Enalapril Maleate RS mu Diluent, ndikuchepetsani mochulukira, komanso pang'onopang'ono ngati kuli kofunikira, ndi Diluent kuti mupeze yankho lomwe lili ndi ndende yodziwika pafupifupi 0.3 mg pa ml.
Njira yothetsera kuyenerera kwa dongosolo-Onjezani 1 mL ya yankho la Enalapril diketopiperazine ku gawo la 50-mL la kukonzekera Kwachizolowezi, ndikusakaniza.
Kukonzekera kuyesa- Tumizani pafupifupi 30 mg ya Enalapril Maleate, yoyezedwa molondola, ku botolo la volumetric 100-mL, sungunulani ndi kusungunula ndi Diluent ku voliyumu, ndi kusakaniza.
Chromatographic system (onani Chromatography <621>) - Chromatograph yamadzimadzi imakhala ndi chowunikira cha 215-nm ndi ndime ya 4.1-mm × 15-cm yomwe ili ndi zonyamula L21.Kuthamanga kwa madzi ndi pafupifupi 1.5 ml pa mphindi.Kutentha kwapakati kumasungidwa pa 70. Chromatograph imakonzedwa motere.
Nthawi(mphindi) Yankho A(%) Yankho B(%) Kuwunika
0 95 5 kufananiza
0-20 95→40 5→60 mzere wa mzere
20-25 40 60 isocratic
25-26 40→95 60→5 mzere wozungulira
26-30 95 5 isocratic
Chromatograph njira yothetsera kuyenerera kwa System, ndikulemba mayankho apamwamba monga momwe adayankhidwira Ndondomeko: nthawi yosungirako ndi pafupi 1.0 ya enalapril ndi 2.1 ya enalapril diketopiperazine;ndipo kusamvana, R, pakati pa enalapril ndi enalapril diketopiperazine sikuchepera 3.5.Chromatograph the Standard kukonzekera, ndikujambulitsa mayankho apamwamba monga momwe adayankhidwira kachitidwe: kupotokola kofanana kwa jakisoni wobwereza sikudutsa 1.0%.
Kachitidwe- Lowetsani padera mavoliyumu ofanana (pafupifupi 50 µL) a Kukonzekera Kwanthawi zonse ndi kukonzekera kwa Assay mu chromatograph, lembani ma chromatogram, ndikuyesa mayankho a nsonga zazikulu.Werengetsani kuchuluka, mu mg, wa C20H28N2O5·C4H4O4 mu gawo la Enalapril Maleate yotengedwa ndi formula:
100C(rU / rS)
momwe C ndi ndende, mu mg pa mL, wa USP Enalapril Maleate RS mu kukonzekera Standard;ndi rU ndi rS ndiwo mayankho apamwamba omwe apezedwa kuchokera ku kukonzekera kwa Assay ndi kukonzekera kwa Standard, motsatana.