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

Optical Rotation [EP]
Qhala bongata bo lekanang le 0.200g ya ntho e dreied le 5g ya hexamethylenetetramine R ho 10ml ya 1mol/L hydrochloric acid mme o hlapolle ho 25.oml ka asiti e tshwanang.Lumella tharollo hore e eme e sirelelitsoe leseli bakeng sa 3h.Lehlakore la ho potoloha ha optical ke -1.27 ° ho -1.34 °
Ponahalo ea Tharollo
Tlosa 1.0g ho 1mol/L hydrochloric acid mme o hlapolle ho 25ml ka solvnet e tšoanang.Tharollo ha e na 'mala o matla ho feta tharollo ea BY6.
Lintho tse Amanang [EP]
Hlahloba ka chromatography ea lera le tšesaane, u sebelisa selulose bakeng sa chromatography R joalo ka ntho ea ho roala.
Tharollo ea teko-Hlakola 0.1g ea ntho e lokelang ho hlahlojoa ka 5ml ea anhydrous formic acid R le ho hlapolla ho 10ml ka methanol R. Lokisetsa hang-hang pele o sebelisoa.
Tharollo ea litšupiso (a) - Hlakola 0.5ml ea tharollo ea teko ho 100ml ka methanol R.
Reference solution (b) - Hlakola 30mg ea tyrosine R ka 1ml ea anhydrous formic acid R 'me u hlapolle ho 100ml ka methanol R. Kopanya 1ml ea tharollo ena le 1ml ea tharollo ea teko.
Etsa kopo ka thoko ho poleiti e le lihlopha tse bolelele ba 20mm, 1oμl ea tharollo ea teko, 10μl ea tharollo ea litšupiso (a) le 20μl ea tharollo ea litšupiso (b).Omella moyeng.Hlahisa ka tsela ea 15cm ho sebelisa motsoako oa 50 volume butanol R, 25 volumes ea glacial acetic acid R le 25 volume ea metsi.Omisa poleiti moeeng o futhumetseng 'me u fafatse ka motsoako o sa tsoa lokisoa oa tekanyo e lekanang ea 10 lekholong m / v tharollo ea ferric chloride R le 5% m / v tharollo ea postassium ferricyanide R. Hlahloba li-chromatoframs hang-hang.Sebaka sefe kapa sefe sa chromatogram se fumanoeng ka tharollo ea tlhahlobo, ntle le sebaka sa mantlha, ha se matla ho feta sebaka se ho chromatogram se fumanoeng ka tharollo ea (a) e bonts'ang.Teko ha e sebetse ntle le haeba chromatogram e fumanoeng ka tharollo ea litšupiso (b) e bonts'a, ka holim'a sebaka se seholo, sebaka se ikhethang se matla ho feta sebaka se ho chromatogram se fumanoeng ka tharollo ea litšupiso (a).
UV Spectrum [EP]
Disslove 30.0mg ho 0.1mol/L hydrochloric acid mme o hlapolle ho 100.oml ka asiti e tšoanang.Hlakola 10.0ml ea tharollo ena ho 100.0ml ka 0.1mol/L hydrochloric acid.Ha e hlahlojoa pakeng tsa 230nm le 350nm, tharollo e bontša tekanyo e le 'ngoe ea ho monya ho 280nm.Monyetla o khethehileng ka bongata bona ke 137 ho isa ho 147, e baloang ho ipapisitsoe le ntho e omisitsoeng.
Tahlehelo ka ho Omisa
Nka sehlahisoa sena, se omeletseng ho boima bo sa feleng ho 105 ° C, ho lahleheloa ke boima ha hoa lokela ho feta 1.0% (Molao o akaretsang 0831).
Residue on Ignition (Sulfated)
Nka l.0g ea Levodopa 'me u e hlahlobe ho ea ka molao (Molao o akaretsang 0841).Se setseng se setseng ha sea lokela ho feta 0.1%.
Litšepe tse boima
Masala a setseng tlas'a ntho ea ho nka mesaletsa ea ho khantša e ke ke ea e-ba le likarolo tse fetang 10 ho milione ea tšepe e boima ha e hlahlojoa ke molao (Melao-motheo e Akaretsang 0821, Molao oa II).
Tlhahlobo ea pH
0.10g ho 10ml ea H2O e sisinyeha ka metsotso e 15.
Boikemisetso ba litaba
Nka sehlahisoa sena ka 0.lg, boima bo nepahetseng, eketsa anhydrous formic acid 2ml ho qhibiliha, eketsa glacial acetic acid 20ml, sisinya, eketsa crystal violet indicator marotholi a 2, ka perchloric acid titration solution (0.1 mol / L) titration ho tharollo ke botala, mme sephetho sa titration se lokisoa ka tlhahlobo e se nang letho.E 'ngoe le e' ngoe ea 1 ml ea perchloric acid titration solution (0.1 mol / L) e lumellana le 19.72mg ea C9H11N04.

JP17 Mokhoa oa Teko

Levodopa, ha e omisitsoe, ha e na ka tlase ho 98.5% ea Levodopa (C9H11NO4).
Tlhaloso Levodopa e hlaha e le tšoeu kapa e bohlooho bo bosoeu hanyenyane, likristale kapa phofo ea kristale.Ha e na monko.E qhibiliha ka bolokolohi ka formic acid, e qhibiliha hanyane ka metsing, 'me e batla e sa qhibilihe ka har'a ethanol (95).E qhibiliha ka ho hlapolla hydrochloric acid.PH ea tharollo e tletseng ea Levodopa e pakeng tsa 5.0 le 6.5.Sebaka se qhibilihang: hoo e ka bang 275 ℃ (ka ho bola).
Boitsebiso
(1) Ho 5 ml ea tharollo ea Levodopa (1 ho 1000) eketsa 1mL ea ninhydrin TS, 'me u chese metsotso e 3 ka bateng ea metsi: 'mala o pherese oa hlaha.
(2) Ho 2 mL ea tharollo ea Levodopa (1 ho 5000) eketsa 10 mL ea 4-aminoantipyrine TS, 'me u sisinyehe: 'mala o mofubelu o hlaha.
(3) Hlakola 3 mg ea Levodopa ka 0.001 mol / L hydrochloric acid TS ho etsa 100 mL.Etsa qeto ea hore na tharollo ea tharollo e laoloa joang tlas'a Ultravioletvisible Spectrophotometry <2.24>, 'me u bapise sepakapaka le Reference Spectrum: ka bobeli li bonts'a matla a tšoanang a ho monya ka nako e tšoanang.
Absorbance <2.24> E 1%1cm (280 nm): 136-146 (kamora ho omisa, 30 mg, 0.001 mol/L hydrochloric acid TS, 1000 mL).
Optical Rotation <2.49> [a]20D:-11.5° ~-13.0°(kamora ho omisa, 2.5 g, 1 mol/L hydrochloric acid TS, 50 mL, 100 mm).
Bohloeki
(1) Ho hlaka le 'mala oa tharollo-Hlakola 1.0 g ea Levodopa ka 20 mL ea 1 mol / L hydrochloric acid TS: tharollo e hlakile ebile ha e na mebala.
(2) Chloride <1.03>-Hlakola 0.5 g ya Levodopa ka 6 mLof hlapolla nitric acid, mme o kenye metsi ho etsa 50 mL.Etsa tlhahlobo ka ho sebelisa tharollo ena e le tharollo ea teko.Lokisetsa tharollo ea taolo ka 0.30 mL ea 0.01 mol/L hydrochloricacid VS (e seng ho feta 0.021%).
(3) Sulfate <1.14>-Hlakola 0.40 g ya Levodopa ka 1 mL ya dilute hydrochloric acid le 30 ml ya metsi, mme o kenye metsi ho etsa 50 mL.Etsa tlhahlobo ka ho sebelisa tharollo ena e le tharollo ea teko.Lokisetsa tharollo ea taolo ka 0.25 mL ea 0.005 mol/L sulfuric acid VS (e seng ho feta 0.030%).
(4) Heavy Metals <1.07>-Tsoela pele ka 1.0 g ea Levodopa ho ea ka Method 2, 'me u etse tlhahlobo.Lokisetsa tharollo ea taolo ka 2.0 mL ea Standard Lead Solution (eseng ho feta 20 ppm).
(5) Arsenic <1.11> - Hlakola 1.0 g ea Levodopa ka 5 mLof hlapolla hydrochloric acid, 'me u etse tlhahlobo ka tharollo ena e le tharollo ea teko (eseng ho feta 2 ppm).
(6) Lintho tse amanang le tsona-Hlakola 0.10 g ea Levodopa ka 10 mL ea sodium disulfite TS, 'me u sebelise tharollo ena e le mohlala oa tharollo.Pipet 1 mL ea tharollo ea sampole, eketsa sodium disulfite TS ho etsa 25 mL hantle.Pipet 1 mL ea tharollo ena, eketsa sodium disulfite TS ho etsa 20 mL hantle, 'me u sebelise tharollo ena e le tharollo e tloaelehileng.Etsa tlhahlobo ka litharollo tsena joalo ka ha ho laetsoe tlasa Thin-layer Chro-matography<2.03>.Spot 5mL e 'ngoe le e 'ngoe ea tharollo ea sampole le tharollo e tloaelehileng poleiting ea selulose bakeng sa mokhoa o mosesane oa ho roka.Theha poleiti ka motsoako oa 1-butanol, metsi, acetic acid (100) le methanol (10:5:5:1) sebaka se ka bang 10 cm, 'me u omise poleiti ka moea.Motsoako oa "ninhydrin" ka har'a acetone (1 ho 50) ka poleiti le mocheso ka 90 ℃ metsotso e 10: matheba ntle le sebaka se ka sehloohong sa tharollo ea sampole ha a matla ho feta sebaka se tsoang tharollong e tloaelehileng.
Tahlehelo ha o Omisa <2.41> Ha e fete 0.30%(1 g, 105℃,3 lihora).
Masalla a ho Ignition <2.44> Ha a fete 0.1% (1 g).
Assay Beha boima bo nepahetseng ka 0.3 g ea Levodopa, e neng e omisitsoe pele, qhala ka 3 ml ea formic acid, eketsa 80 ml ea acetic acid (100), le titrate <2.50> ka 0.1 mol/L perchloric acid VS ho fihlela 'mala oa tharollo o fetoha. ho tloha ho pherese ho isa ho botala bo boputsoa ho isa ho botala (pontšo: marotholi a 3 a crystalviolet TS).Etsa qeto e se nang letho, 'me u etse tokiso e hlokahalang.
ML ka 'ngoe ea 0.1 mol/L perchloric acid VS＝19.72 mg ea C9H11NO4
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