I-Levodopa (L-DOPA) CAS 59-92-7 99.0~100.5% USP BP EP Standard Anti-Parkinson's Disease High Purity

Ukujikeleza kokubona [EP]
Chaza inani elilingana no-0.200g we-dreied substance kanye no-5g we-hexamethylenetetramine R ku-10ml we-1mol/L hydrochloric acid futhi uhlambulule ku-25.oml nge-asidi efanayo.Vumela ikhambi ukuthi lime livikelekile ekukhanyeni amahora angu-3.I-engeli yokujikeleza kwe-optical ingu -1.27° ukuya ku- -1.34°
Ukubukeka Kwesixazululo
Khipha u-1.0g ku-1mol/L i-hydrochloric acid bese unciphisa ibe ngu-25ml nge-solvnet efanayo.Isixazululo asinawo umbala ogqamile kunesixazululo sereferensi BY6.
Izinto Ezihlobene [EP]
Hlola nge-chromatography yongqimba oluncane, usebenzisa i-cellulose ye-chromatography R njengento enamathelayo.
Isixazululo sokuhlola-Chaza u-0.1g wento ezohlolwa ku-5ml we-anhydrous formic acid R bese uhlanza ube ngu-10ml nge-methanol R. Lungiselela ngokushesha ngaphambi kokusetshenziswa.
Isixazululo sereferensi (a)-Hlanganisa u-0.5ml wesixazululo sokuhlola sibe ngu-100ml nge-methanol R.
Isixazululo sereferensi (b) -Diza i-30mg ye-tyrosine R ku-1ml ye-anhydrous formic acid R bese unciphisa ku-100ml nge-methanol R. Hlanganisa i-1ml yalesi sixazululo ne-1ml yesisombululo sokuhlola.
Gcoba ngokuhlukile epuletini njengamabhande angu-20mm ubude, u-1oμl wesixazululo sokuhlola, u-10μl wesixazululo sereferensi (a) kanye no-20μl wesixazululo sereferensi (b).Yomisa emoyeni.Yakha phezu kwendlela od 15cm usebenzisa ingxube yevolumu ye-butanol R engu-50, imiqulu engama-25 ye-glacial acetic acid R kanye namavolumu angama-25 amanzi.Yomisa ipuleti emoyeni ofudumele bese ufutha ngengxube esanda kulungiselelwa enevolumu elinganayo yesisombululo esingu-10% m/v se-ferric chloride R kanye nesixazululo esingu-5 m/v se-postassium ferricyanide R. Hlola ama-chromatoframs ngokushesha.Noma iyiphi indawo ku-chromatogram etholwe nesixazululo sokuhlola, ngaphandle kwendawo eyinhloko, ayinamandla kakhulu kunendawo eku-chromatogram etholwe ngesixazululo sereferensi (a) esiboniswayo.Ukuhlola akuvumelekile ngaphandle kokuthi i-chromatogram etholwe nesixazululo sereferensi (b) ibonisa, ngenhla kwendawo eyinhloko, indawo ehlukile eqine kakhulu kune-chromatogram etholwe ngesixazululo sereferensi (a).
I-UV Spectrum [EP]
Khipha u-30.0mg ku-0.1mol/L i-hydrochloric acid bese unciphisa ku-100.oml nge-asidi efanayo.Nciphisa u-10.0ml walesi sixazululo ku-100.0ml ngo-0.1mol/L we-hydrochloric acid.Uma sihlolwa phakathi kuka-230nm no-350nm, isixazululo sibonisa ukumuncwa okukodwa okuphezulu ku-280nm.Ukumunca okuthile kulobu bukhulu kungu-137 kuya ku-147, kubalwa ngokubhekisela entweni eyomisiwe.
Ukulahlekelwa Ekumisweni
Thatha lo mkhiqizo, womile kuya esisindweni esingaguquki ku-105°C, ukuncipha kwesisindo akumele kudlule u-1.0% (Umthetho ojwayelekile 0831).
Izinsalela ekushiseni (Sulfated)
Thatha i-l.0g ye-Levodopa futhi uyihlole ngokomthetho (Umthetho ojwayelekile 0841).Okusele akumele kudlule u-0.1%.
Izinsimbi Ezisindayo
Izinsalela ezishiywe ngaphansi kwento yokuthatha insalela yokubasa ngeke ziqukathe izingxenye ezingaphezu kweziyi-10 esigidini sensimbi esindayo lapho ihlolwa ngokomthetho (Izimiso Ezijwayelekile 0821, Law II).
Ukuhlolwa kwe-pH
0.10g ku-10ml we-H2O enyakaza imizuzu engu-15.
Ukuzimisela kokuqukethwe
Thatha lo mkhiqizo mayelana ne-0.lg, ukunemba isisindo, engeza i-anhydrous formic acid 2ml ukuze uhlakaze, engeza i-glacial acetic acid 20ml, shake, engeza i-crystal violet inkomba amaconsi angu-2, ne-perchloric acid titration solution (0.1 mol / L) titration kusixazululo eluhlaza, futhi umphumela we-titration ulungiswa ngokuhlolwa okungenalutho.I-1 ml ngayinye yesisombululo se-perchloric acid titration (0.1 mol/L) ihambisana no-19.72mg we-C9H11N04.

Indlela Yokuhlola ye-JP17

I-Levodopa, uma yomisiwe, iqukethe okungenani i-98.5% ye-Levodopa (C9H11NO4).
I-Levodopa yenzeka imhlophe noma impunga kancane emhlophe, amakristalu noma impushana ecwebezelayo.Ayinaphunga.Incibilika ngokukhululekile ku-formic acid, inyibilika kancane emanzini, futhi ayincibiliki ku-ethanol (95).Incibilika ku-dilute hydrochloric acid.I-pH yesisombululo esigcwele se-Levodopa iphakathi kuka-5.0 no-6.5.Iphuzu elincibilikayo: cishe ku-275℃ (ngokubola).
Ukuhlonza
(1) Ku-5 mL wesixazululo se-Levodopa (1 ku-1000) engeza i-1mL ye-ninhydrin TS, bese ushisa imizuzu emi-3 ekugezeni kwamanzi: umbala onsomi uyavela.
(2) Ku-2 mL wesixazululo se-Levodopa (1 ku-5000) engeza u-10 mL we-4-aminoantipyrine TS, bese unyakazisa: umbala obomvu uyavela.
(3) Chaza u-3 mg we-Levodopa ku-0.001 mol/L i-hydrochloric acid TS ukwenza u-100 mL.Nquma i-spectrum yokumuncwa kwesixazululo njengoba kuqondiswe ngaphansi kwe-Ultravioletvisible Spectrophotometry <2.24>, bese uqhathanisa i-spectrum ne-Reference Spectrum: yomibili i-spectra ibonisa ukuqina okufanayo kokumuncwa ngamaza amaza afanayo.
I-Absorbance <2.24> E 1%1cm (280 nm): 136-146 (ngemuva kokumiswa, 30 mg, 0.001 mol/L hydrochloric acid TS, 1000 mL).
I-Optical Rotation <2.49> [a]20D:-11.5° ~-13.0°(ngemuva kokoma, 2.5 g, 1 mol/L hydrochloric acid TS, 50 mL, 100 mm).
Ubumsulwa
(1) Ukucaca kanye nombala wesixazululo-Chaza u-1.0 g we-Levodopa ku-20 mL we-1 mol/L i-hydrochloric acid TS: isixazululo sicacile futhi asinambala.
(2) I-Chloride <1.03>-Chaza u-0.5 g we-Levodopa ku-6 mLof dilute nitric acid, bese wengeza amanzi ukuze wenze u-50 mL.Yenza ukuhlolwa usebenzisa lesi sixazululo njengesixazululo sokuhlola.Lungiselela ikhambi lokulawula ngo-0.30 mL we-0.01 mol/L hydrochloricacid VS (hhayi ngaphezu kuka-0.021%).
(3) I-Sulfate <1.14>-Diluza u-0.40 g we-Levodopa ku-1 mL we-dilute hydrochloric acid kanye no-30 mL wamanzi, bese wengeza amanzi ukuze wenze u-50 mL.Yenza ukuhlolwa usebenzisa lesi sixazululo njengesixazululo sokuhlola.Lungiselela ikhambi lokulawula ngo-0.25 mL ka-0.005 mol/L sulfuric acid VS (hhayi ngaphezu kuka-0.030%).
(4) Izinsimbi Ezisindayo <1.07>-Qhubeka ne-1.0 g ye-Levodopa ngokweNdlela yesi-2, futhi wenze ukuhlolwa.Lungiselela isixazululo sokulawula ngo-2.0 mL Wesixazululo Esijwayelekile Sokuhola (hhayi ngaphezu kuka-20 ppm).
(5) I-Arsenic <1.11>-Dissolve 1.0 g ye-Levodopa ku-5 mLof dilute hydrochloric acid, futhi wenze ukuhlolwa ngalesi sixazululo njengesixazululo sokuhlola (hhayi ngaphezu kuka-2 ppm).
(6) Izinto ezihlobene-Chaza u-0.10 g we-Levodopa ku-10 mL we-sodium disulfite TS, futhi usebenzise lesi sixazululo njengesampula yesixazululo.Ipayipi elingu-1 mL lesixazululo sesampula, engeza i-sodium disulfite TS ukwenza u-25 mL ngqo.Ipayipi elingu-1 mL lalesi sixazululo, engeza i-sodium disulfite TS ukwenza u-20 mL ngqo, bese usebenzisa lesi sixazululo njengesixazululo esijwayelekile.Yenza ukuhlolwa ngalezi zixazululo njengoba kuqondiswe ngaphansi kwe-Thin-layer Chro-matography<2.03>.Faka i-5mL ngayinye yesixazululo sesampula kanye nesisombululo esijwayelekile epuletini le-cellulose le- thin-layerchromatography.Yakha ipuleti ngengxube ye-1-butanol, amanzi, i-acetic acid (100) ne-methanol (10:5:5:1) ebangeni elingama-cm ayi-10, bese womisa ipuleti ngomoya.Isixazululo se-ninhydrin ngokufafaza ku-acetone (1 ku-50) epuletini bese sishisisa ku-90℃ imizuzu eyi-10: amachashaza ngaphandle kwendawo eyinhloko evela kusixazululo sesampula awashubi kakhulu kunendawo evela esixazululweni esijwayelekile.
Ukulahlekelwa Ekumisweni <2.41> Kungabi ngaphezu kuka-0.30%(1 g, 105℃,3 amahora).
Insalela Ekuthutheni <2.44> Ayidluli ku-0.1% (1 g).
I-Assay Kala ngokunembile cishe u-0.3 g we-Levodopa, omisiwe ngaphambilini, ncibilika ku-3 mL we-formic acid, engeza u-80 mL we-acetic acid (100), bese u-titrate u-<2.50> ngo-0.1 mol/L perchloric acid VS kuze kushintshe umbala wesixazululo. kusuka kokunsomi kuya kokuluhlaza okwesibhakabhaka kuya kokuluhlaza (inkomba: amaconsi ama-3 e-crystalviolet TS).Yenza isinqumo esingenalutho, futhi wenze noma yikuphi ukulungisa okudingekayo.
I-mL ngayinye ka-0.1 mol/L perchloric acid VS＝19.72 mg ye-C9H11NO4
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