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

Ukujikeleza kwaMacho [EP]
Dissolve ubuninzi obulingana ne-0.200g ye-dreied substance kunye ne-5g ye-hexamethylenetetramine R kwi-10ml ye-1mol / L i-hydrochloric acid kwaye ihlambulule kwi-25.oml nge-asidi efanayo.Vumela isisombululo ukuba sime sikhuselekile ekukhanyeni kwe-3h.I-angle yokujikeleza kwe-optical -1.27 ° ukuya -1.34 °
Imbonakalo yesisombululo
Disslove 1.0g kwi-1mol / L i-hydrochloric acid kwaye uhlambulule kwi-25ml kunye ne-solvnet efanayo.Isisombululo asinambala kakhulu kunesisombululo sereferensi BY6.
Izinto eziyeleleneyo [EP]
Jonga ngekhromatografi ecekethekileyo, usebenzisa i-cellulose yechromatography R njengento yokwambathisa.
Isisombululo sovavanyo-Dibanisa i-0.1g yezinto eziza kuhlolwa kwi-5ml ye-anhydrous formic acid R kwaye udibanise kwi-10ml nge-methanol R. Lungiselela ngokukhawuleza ngaphambi kokusetyenziswa.
Isisombululo sereferensi (a) -Dilute i-0.5ml yesisombululo sovavanyo kwi-100ml nge-methanol R.
Isisombululo sokubhekisela (b) -Dibanisa i-30mg ye-tyrosine R kwi-1ml ye-anhydrous formic acid R kwaye udibanise kwi-100ml nge-methanol R. Hlanganisa i-1ml yesi sisombululo kunye ne-1ml yesisombululo sovavanyo.
Faka isicelo ngokwahlukileyo kwipleyiti njengeebhendi ezingama-20mm ubude, i-1oμl yesisombululo sovavanyo, i-10μl yesisombululo sereferensi (a) kunye ne-20μl yesisombululo sereferensi (b).Yomisa emoyeni.Phuhlisa phezu kwendlela od 15cm usebenzisa umxube 50 imithamo butanol R, 25 imiqulu glacial acetic acid R kunye 25 imithamo yamanzi.Yomisa ipleyiti kumoya ofudumeleyo wangoku kwaye utshise ngomxube olungiselelwe ngokutsha womthamo olinganayo we-10 ekhulwini m/v isisombululo se-ferric chloride R kunye ne-5 yepesenti yesisombululo se-postassium ferricyanide R. Hlola i-chromatoframs ngokukhawuleza.Naliphi na ibala elikwichromatogram elifunyenwe ngesisombululo sovavanyo, ngaphandle kwendawo eyintloko, alikho likhulu kunebala elikwichromatogram elifunyenwe ngesisombululo sereferensi (a) libonisa.Uvavanyo alusebenzi ngaphandle kokuba ichromatogram efunyenwe ngesisombululo sereferensi (b) ibonisa, ngaphezulu kwendawo eyintloko, indawo eyahlukileyo eqine ngakumbi kunechoko kwichromatogram efunyenwe ngesisombululo sereferensi (a).
I-UV Spectrum [EP]
I-Disslove 30.0mg kwi-0.1mol / L i-hydrochloric acid kwaye idibanise kwi-100.oml nge-asidi efanayo.Nciphisa i-10.0ml yesi sisombululo kwi-100.0ml kunye ne-0.1mol / L i-hydrochloric acid.Ukuhlolwa phakathi kwe-230nm kunye ne-350nm, isisombululo sibonisa ubuninzi be-absorption eyodwa kwi-280nm.I-absorbection ethile kulo buninzi i-137 ukuya kwi-147, ibalwa ngokubhekiselele kwizinto ezomileyo.
Ilahleko ekomisweni
Thatha le mveliso, yomile ukuya kwisisindo esingaguqukiyo kwi-105 ° C, ukulahleka kwesisindo akuyi kudlula i-1.0% (Umgaqo jikelele we-0831).
Intsalela ekutshisweni (iSulfated)
Thatha i-l.0g ye-Levodopa kwaye uyijonge ngokomthetho (umgaqo jikelele we-0841).Intsalela eshiyekileyo ayisayi kudlula i-0.1%.
Iintsimbi ezinzima
Intsalela eshiywe phantsi kwento yokuthatha intsalela yokutshisa ayiyi kuqulatha ngaphezu kweengxenye ze-10 kwisigidi sentsimbi enzima xa ihlolwe ngumthetho (iMigaqo Jikelele 0821, uMthetho II).
Uvavanyo lwe-pH
I-0.10g kwi-10ml ye-H2O ishukuma imizuzu eyi-15.
Ukuzimisela komxholo
Thatha le mveliso malunga ne-0.lg, ukulinganisa ngokuchanekileyo, ukongeza i-anhydrous formic acid 2ml ukuchithwa, ukongeza i-glacial acetic acid 20ml, ukugubha, ukongeza isalathisi se-crystal violet i-2 ihla, kunye ne-perchloric acid titration solution (0.1 mol / L) i-titration kwisisombululo eluhlaza, kwaye umphumo we-titration ulungiswa ngovavanyo olungenanto.I-1 ml nganye yesisombululo se-perchloric acid titration (0.1 mol / L) ihambelana ne-19.72mg ye-C9H11N04.

Indlela yoVavanyo lweJP17

I-Levodopa, xa yomisiwe, iqulethe ngaphantsi kwe-98.5% ye-Levodopa (C9H11NO4).
Inkcazelo I-Levodopa yenzeka imhlophe okanye ingwevu kancinane emhlophe, iikristale okanye umgubo wecrystalline.Ayinavumba.Inyibilika ngokukhululekileyo kwifomic acid, inyibilika kancinane emanzini, kwaye ayinyibiliki kwi-ethanol (95).Inyibilika kwi-dilute hydrochloric acid.I-pH yesisombululo esigcweleyo seLevodopa siphakathi kwe-5.0 kunye ne-6.5.Indawo yokunyibilika: malunga ne-275℃ (ngokubola).
Ukuchongwa
(1) Ukuya kwi-5 mL yesisombululo se-Levodopa (1 kwi-1000) yongeza i-1mL ye-ninhydrin TS, kunye nokufudumala kwemizuzu emi-3 kwindawo yokuhlamba amanzi: umbala omfusa uyavela.
(2) Kwi-2 mL yesisombululo se-Levodopa (1 kwi-5000) yongeza i-10 mL ye-4-aminoantipyrine TS, kwaye ugubungele: umbala obomvu ukhula.
(3) Dissolve 3 mg Levodopa in 0.001 mol / L hydrochloric acid TS ukwenza 100 mL.Gqiba i-spectrum yokufunxa isisombululo njengoko ilawulwa phantsi kwe-Ultravioletvisible Spectrophotometry <2.24>, kwaye uthelekise i-spectrum kunye ne-Reference Spectrum: zombini i-spectra ibonisa ubunzima obufanayo bokuxutywa kwi-wavelengths efanayo.
I-Absorbance <2.24> E 1% 1cm (280 nm): 136-146 (emva kokumisa, 30 mg, 0.001 mol / L i-hydrochloric acid TS, 1000 mL).
Ukujikeleza kwe-Optical <2.49> [a] 20D: -11.5 ° ~-13.0 ° (emva kokumisa, 2.5 g, 1 mol / L i-hydrochloric acid TS, 50 mL, 100 mm).
Ubunyulu
(1) Ukucaca kunye nombala wesisombululo-Dibanisa i-1.0 g yeLevodopa kwi-20 mL ye-1 mol / L i-hydrochloric acid TS: isisombululo sicacile kwaye singenambala.
(2) I-Chloride <1.03>-Dibanisa i-0.5 g ye-Levodopa kwi-6 mLof dilute nitric acid, kwaye wongeze amanzi ukwenza i-50 mL.Yenza uvavanyo usebenzisa esi sisombululo njengesisombululo sovavanyo.Lungisa isisombululo sokulawula kunye ne-0.30 mL ye-0.01 mol / L hydrochloricacid VS (kungekho ngaphezu kwe-0.021%).
(3) Sulfate <1.14>-Dibanisa i-0.40 g ye-Levodopa kwi-1 mL ye-dilute hydrochloric acid kunye ne-30 mL yamanzi, kwaye yongeza amanzi ukwenza i-50 mL.Yenza uvavanyo usebenzisa esi sisombululo njengesisombululo sovavanyo.Lungiselela isisombululo sokulawula kunye ne-0.25 mL ye-0.005 mol / L i-sulfuric acid VS (kungekho ngaphezu kwe-0.030%).
(4) Iintsimbi ezinzima <1.07>-Qhubeka kunye ne-1.0 g yeLevodopa ngokweNdlela yesi-2, kwaye wenze uvavanyo.Lungiselela isisombululo solawulo kunye ne-2.0 mL yeSisombululo esiPhambili seNkokheli (kungekho ngaphezu kwe-20 ppm).
(5) I-Arsenic <1.11>-Dissolve 1.0 g yeLevodopa kwi-5 mLof ihlambulule i-hydrochloric acid, kwaye wenze uvavanyo kunye nesi sisombululo njengesisombululo sokuvavanya (kungekho ngaphezu kwe-2 ppm).
(6) Izinto ezihambelanayo-Dibanisa i-0.10 g ye-Levodopa kwi-10 mL ye-sodium disulfite TS, kwaye usebenzise esi sisombululo njengesisombululo sesampuli.Umbhobho we-1 mL wesisombululo sesampuli, yongeza i-sodium disulfite TS ukwenza i-25 mL ngqo.Umbhobho we-1 mL yesi sisombululo, yongeza i-sodium disulfite TS ukwenza kanye i-20 mL, kwaye usebenzise esi sisombululo njengesisombululo esiqhelekileyo.Yenza uvavanyo ngezi zisombululo njengoko kubhaliwe phantsi kwe-Thin-layer Chro-matography <2.03>.Indawo ye-5mL nganye yesisombululo sesampulu kunye nesisombululo esisemgangathweni kwipleyiti ye-cellulose ye-thin-layerchromatography.Phuhlisa ipleyiti ngomxube we-1-butanol, amanzi, i-acetic acid (100) kunye ne-methanol (10: 5: 5: 1) kumgama omalunga ne-10 cm, kunye ne-air-dry plate.Isisombululo se-sprayevenly se-ninhydrin kwi-acetone (i-1 ku-50) kwi-plate kunye nobushushu kwi-90 ℃ imizuzu eyi-10: amabala angaphandle kwendawo ephambili kwisisombululo sesampulu ayinamandla ngaphezu kwendawo evela kwisisombululo esiqhelekileyo.
Ilahleko ekomisweni <2.41> Akukho ngaphezu kwe-0.30% (1 g, 105℃,3 iiyure).
Intsalela kwi-Ignition <2.44> Akukho ngaphezu kwe-0.1% (1 g).
I-Assay Ukulinganisa ngokuchanekileyo malunga ne-0.3 g ye-Levodopa, eyomisiwe ngaphambili, inyibilika kwi-3 mL ye-formic acid, yongeza i-80 mL ye-acetic acid (100), kunye ne-titrate <2.50> kunye ne-0.1 mol / L perchloric acid VS de umbala wesisombululo utshintshe. ukusuka emfusa ukuya eluhlaza okwesibhakabhaka ukuya eluhlaza (isalathisi: amaconsi ama-3 e-crystalviolet TS).Yenza isigqibo esingenanto, kwaye wenze naluphi na ulungiso oluyimfuneko.
I-mL nganye ye-0.1 mol/L ye-perchloric acid VS＝19.72 mg ye-C9H11NO4
Imigqomo kunye nokugcinwa Izikhongozeli-Tight izikhongozeli.
Ugcino-Ukukhanya-resistant.