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 iqukethe okungengaphansi kwamaphesenti angama-98.0 futhi angabi ngaphezu kwamaphesenti angu-102.0 we-C20H28N2O5·C4H4O4, abalwe ngokomisiwe.
Ukupakisha nokugcina-Londoloza ezitsheni ezivalwe kahle, futhi ugcine ekamelweni lokushisa elilawulwayo.
Amazinga ereferensi we-USP <11>-
USP Enalapril Maleate RS Chofoza ukuze Ubuke Isakhiwo
Ukuhlonza-
A: I-Infrared Absorption <197M>.
B: Isikhathi sokugcinwa sesiqongo esikhulu ku-chromatogram yokulungiselelwa kwe-Assay sihambisana naleso esiku-chromatogram yokulungiselelwa Okujwayelekile, njengoba kutholwe ku-Assay.
Ukuzungezisa okuqondile <781S>: phakathi -41.0 kanye -43.5.
Isixazululo sokuhlola: 10 mg nge-mL, ku-methanol.
Ukulahlekelwa ekumisweni <731>-Yomise ku-vacuum ngengcindezi engeqile ku-5 mm we-mercury ku-60 amahora angu-2: ilahlekelwa ngaphezu kuka-1.0% wesisindo sayo.
Izinsalela ekushiseni <281>: hhayi ngaphezu kuka-0.2%.
Izinsimbi ezinzima, Indlela II <231>: 0.001%.
Izinhlanganisela ezihlobene-
I-pH 6.8 i-Phosphate buffer, i-pH 2.5 i-Phosphate buffer, Isixazululo A, Isixazululo B, Isigaba seselula, i-Diluent, isixazululo se-Enalapril diketopiperazine, Isixazululo sokufaneleka kwesistimu, kanye nesistimu ye-Chromatographic— Qhubeka njengoba kushiwo ku-Assay.
Isixazululo esijwayelekile-Chaza isamba esikalwe ngokunembile se-USP Enalapril Maleate RS ku-Diluent, futhi uhlambulule ngobuningi, nangesinyathelo esilandelanayo uma kudingeka, nge-Diluent ukuze uthole isixazululo esinokugxila okwaziwayo okungaba ngu-3 µg ngemL ngayinye.
Isixazululo sokuhlola-Sebenzisa ukulungiswa kwe-Assay.
Inqubo-Ngokuhlukile jova amavolumu alinganayo (cishe u-50 µL) wesisombululo Esijwayelekile kanye nesixazululo sokuhlola ku-chromatograph, rekhoda ama-chromatogram, futhi ulinganise izimpendulo zendawo ephakeme.Bala iphesenti lokungcola ngakunye engxenyeni ye-Enalapril Maleate ethathwe ifomula:
100(CS / CT)(ri / rS)
lapho i-CS iwukugxila, ngo-mg ngemL ngayinye, ye-USP Enalapril Maleate RS kusixazululo Esijwayelekile;I-CT ukugxila, ku-mg nge-mL ngayinye, ye-Enalapril Maleate kusixazululo sokuhlola;i-ri iyindawo ephakeme kakhulu yokungcola ngakunye okutholakala kusixazululo sokuhlola;futhi i-rS iyindawo ephakeme kakhulu ye-enalapril etholakala kusixazululo Esijwayelekile: akutholakali ngaphezu kuka-1.0% wanoma yikuphi ukungcola okunesikhathi sokugcina esihlobene esingaba ngu-1.10;hhayi ngaphezu kuka-0.3% wanoma yikuphi okunye ukungcola komuntu okutholakele;futhi akukho ngaphezu kuka-2% wokungcola okuphelele okutholakele.
Isivivinyo-
pH 6.8 Phosphate buffer-Dissolve 2.8 g of monobasic sodium phosphate cishe u-900 mL wamanzi ku-1000-mL volumetric flask.Lungisa ngesisombululo se-9 M sodium hydroxide sibe pH engaba ngu-6.8, hlambulula ngamanzi uye kuvolumu, bese uxuba.
pH 2.5 Phosphate buffer-Dissolve 2.8 g of monobasic sodium phosphate cishe ku-900 mL wamanzi kuflask yevolumu yevolumu engu-1000-mL.Lungisa nge-phosphoric acid ibe i-pH engaba ngu-2.5, nciphisa ngamanzi abe yivolumu, bese uxuba.
Isixazululo A-Lungiselela ingxube ehlungiwe negasisiwe ye-pH 6.8 Phosphate buffer kanye ne-acetonitrile (19:1).
Isixazululo B-Lungiselela ingxube ehlungiwe negasisiwe ye-acetonitrile ne-pH 6.8 Phosphate buffer (33:17).
Isigaba seselula-Sebenzisa izingxube eziguquguqukayo zesisombululo A nesixazululo B njengoba kuqondiswe kusistimu yeChromatographic.Yenza izinguquko uma kudingeka (bona Ukufaneleka Kwesistimu ngaphansi kwe-Chromatography 621).
I-Diluent-Lungiselela ingxube ye-pH 2.5 Phosphate buffer kanye ne-acetonitrile (95:5).
Isixazululo se-Enalapril diketopiperazine-Beka ngokucophelela cishe u-20 mg we-USP Enalapril Maleate RS kubhikha oyi-100-mL ukuze wenze indunduma phansi kwebhekha.Beka ibhikha epuletini elishisayo cishe engxenyeni eyodwa yobukhulu bokushisa kwepuleti elishisayo.Shisisa cishe imizuzu emi-5 kuya kweyi-10 kuze kube yilapho okuqinile kuncibilika.Khipha ibhikha ngokushesha ku-hot plate, bese uvumela ukuthi liphole.[Qaphela-Gwema ukushisa ngokweqile ukuze uvimbele ukuwohloka okubangelwa ukushisa, okungase kubangele umbala onsundu.] Ezingxenyeni ezisele ezipholile ku-beaker engeza u-50 mL we-acetonitrile, bese u-sonicate imizuzu embalwa ukuze uncibilike.Isixazululo ngokuvamile siqukethe, ku-mL ngayinye, phakathi kuka-0.2 mg no-0.4 mg we-enalapril diketopiperazine.
Ukulungiselela okujwayelekile-Chaza inani elinesisindo esinembile le-USP Enalapril Maleate RS ku-Diluent, futhi uhlambulule ngobuningi, nangesinyathelo esilandelanayo uma kudingeka, nge-Diluent ukuze uthole isixazululo esinokugxila okwaziwayo okungaba ngu-0.3 mg nge-mL ngayinye.
Isixazululo sokufaneleka kwesistimu-Engeza i-1 mL yesisombululo se-Enalapril diketopiperazine engxenyeni engu-50-mL yokulungiselela Okujwayelekile, bese uxuba.
Ukulungiswa kwe-assay- Dlulisa cishe u-30 mg we-Enalapril Maleate, ukalwe ngokunembile, uye ku-100-mL ye-volumetric flask, ncibilikisa futhi uhlambulule nge-Diluent kuya kuvolumu, bese uxuba.
Isistimu ye-Chromatographic (bona i-Chromatography <621>)-I-chromatograph ewuketshezi ifakwe umtshina ongu-215-nm kanye nekholomu engu-4.1-mm × 15-cm equkethe ukupakisha kwe-L21.Izinga lokugeleza licishe libe ngu-1.5 mL ngomzuzu.Izinga lokushisa lekholomu ligcinwa liku-70. I-chromatograph ihlelwe kanje.
Isikhathi(amaminithi) Isixazululo A(%) Isixazululo B(%) Ukulinganisa
0 95 5 ukulinganisa
0-20 95→40 5→60 igradient yomugqa
20-25 40 60 isocratic
25-26 40→95 60→5 igradient yomugqa
26-30 95 5 isocratic
I-Chromatograph isixazululo sokufaneleka Kwesistimu, futhi urekhode izimpendulo eziphezulu njengoba kuqondiswe Enqubweni: izikhathi zokugcinwa okuhlobene zicishe zibe ngu-1.0 we-enalapril kanye no-2.1 we-enalapril diketopiperazine;futhi isinqumo, R, phakathi kwe-enalapril ne-enalapril diketopiperazine singekho ngaphansi kuka-3.5.I-Chromatograph ukulungiselelwa Okujwayelekile, futhi urekhode izimpendulo eziphezulu njengoba kuqondiswe kuNqubo: ukuchezuka okujwayelekile okuhlobene kwemijovo eyimpinda akukho ngaphezu kuka-1.0%.
Inqubo- Jova ngokwehlukana amavolumu alinganayo (cishe u-50 µL) wokulungiselela Okujwayelekile kanye nokulungiswa kwe-Assay ku-chromatograph, rekhoda ama-chromatogram, futhi ulinganise izimpendulo zeziqongo ezinkulu.Bala inani, ngo-mg, le-C20H28N2O5·C4H4O4 engxenyeni ye-Enalapril Maleate ethathwe ngefomula:
100C(rU / rS)
lapho u-C eyingqikithi, ngo-mg ngemL ngayinye, ye-USP Enalapril Maleate RS ekulungiseleleni Okujwayelekile;futhi i-rU kanye ne-rS yizimpendulo eziphezulu ezitholakala ekulungiselelweni kwe-Assay nasekulungiseleleni Okujwayelekile, ngokulandelanayo.