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

Kutenderera kweOptical [EP]
Dissolve huwandu hwakaenzana ne0.200g yedreied substance uye 5g yehexamethylenetetramine R mu 10ml ye 1mol/L hydrochloric acid uye dilute kusvika 25.oml neasidhi yakafanana.Bvumira mhinduro kumira yakadzivirirwa kubva kuchiedza kwe3h.Iko kona ye optical rotation ndeye -1.27 ° kusvika -1.34 °
Kuonekwa kweSolution
Disslove 1.0g mu1mol/L hydrochloric acid uye diluve kusvika 25ml neiyo solvnet yakafanana.Mhinduro haina kunyanya kupenya kupfuura referensi mhinduro BY6.
Zvinhu zvinoenderana [EP]
Ongorora neyakaonda-layer chromatography, uchishandisa cellulose yechromatography R sechinhu chekuputira.
Test solution-Dissolve 0.1g yechinhu chinofanirwa kuongororwa mu5ml yeanhydrous formic acid R uye diluted kusvika 10ml nemethanol R. Gadzirira pakarepo usati washandisa.
Reference solution (a)-Dilute 0.5ml yebvunzo mhinduro ku100ml ine methanol R.
Reference solution (b) -Dissolve 30mg ye tyrosine R mu 1ml ye anhydrous formic acid R uye shandura kusvika 100ml ne methanol R. Sanganisa 1ml yeiyi mhinduro ne 1ml yemhinduro yekuedza.
Isa zvakaparadzana mundiro semabhandi 20mm kureba, 1oμl yemubvunzo mhinduro, 10μl yereferensi mhinduro (a) uye 20μl yereferenzi mhinduro (b).Dry mumhepo inoyerera.Gadzira pamusoro penzira od 15cm uchishandisa musanganiswa we50 mavhoriyamu ebutanol R, 25 mavhoriyamu eglacial acetic acid R uye makumi maviri nemashanu emvura.Pukuta ndiro mumhepo inodziya uye pfapfaidza nemusanganiswa uchangogadzirwa wakaenzana nehuwandu hwe10 muzana m/v mhinduro yeferric chloride R uye 5 muzana m/v mhinduro ye postassium ferricyanide R. Ongorora ma chromatoframs nekukasika.Chero nzvimbo muchromatogram yakawanikwa nemhinduro yebvunzo, kunze kwenzvimbo huru, haina kusimba kupfuura nzvimbo iri muchromatogram inobatwa nereferensi mhinduro (a) inoratidza.Muedzo haushande kunze kwekunge chromatogram yawanwa nereferensi mhinduro (b) inoratidza, pamusoro penzvimbo huru, nzvimbo yakasarudzika yakanyanyisa kupfuura nzvimbo iri muchromatogram yakawanikwa nereferensi mhinduro (a).
UV Spectrum [EP]
Disslove 30.0mg mu 0.1mol/L hydrochloric acid uye dilute kusvika 100.oml neasidhi yakafanana.Dilute 10.0ml yemushonga uyu kusvika pa100.0ml ne0.1mol/L hydrochloric acid.Yakaongororwa pakati pe230nm uye 350nm, mhinduro inoratidza kumwe kunyura kwakanyanya pa280nm.Iyo chaiyo yekunyura pane iyi yakakura ndeye 137 kusvika 147, yakaverengerwa inoenderana neyakaomeswa chinhu.
Kurasika paKuomesa
Tora chigadzirwa ichi, chakaoma kuti chirambe chichirema pa 105 ° C, kurasikirwa kwehuremu hakufaniri kudarika 1.0% (General rule 0831).
Residue paIgnition (Sulfated)
Tora l.0g yeLevodopa uye utarise maererano nemutemo (General mutemo 0841).Zvakasara zvakasara hazvifaniri kudarika 0.1%.
Heavy Metals
Zvakasara zvakasara pasi pechinhu chekutora zvakasara zvemoto hazvifaniri kuva nezvikamu zvinopfuura gumi pamamiriyoni eheavy metal kana zvichiongororwa nemutemo (General Principles 0821, Law II).
pH Test
0.10g mu10ml yeH2O ichizunza kwemaminetsi gumi nemashanu.
Kutsunga kwemukati
Tora chigadzirwa ichi nezve 0.lg, kunyatsoyera kuyera, kuwedzera anhydrous formic acid 2ml kuti iparadze, wedzera glacial acetic acid 20ml, zunza, wedzera crystal violet chiratidzo 2 madonhwe, ane perchloric acid titration solution (0.1 mol / L) titration kune mhinduro iri girini, uye mhedzisiro yetitration inogadziriswa nebvunzo isina chinhu.Imwe neimwe 1 ml ye perchloric acid titration solution (0.1 mol/L) inoenderana ne19.72mg yeC9H11N04.

JP17 Test Method

Levodopa, kana yakaomeswa, ine kwete pasi pe98.5% yeLevodopa (C9H11NO4).
Tsanangudzo Levodopa inoitika sechena kana zvishoma greyi chena, makristasi kana crystalline poda.Hainhuhwi.Iyo inonyungudika zvakasununguka muformic acid, inonyungudika zvishoma mumvura, uye isingagoneke mu ethanol (95).Inonyungudika mu dilute hydrochloric acid.Iyo pH yesaturated solution yeLevodopa iri pakati pe5.0 ne6.5.Nzvimbo yakanyungudika: inenge 275 ℃ (ine kuora).
Identification
(1) Ku5 mL yemushonga weLevodopa (1 mu1000) wedzera 1mL yeninhydrin TS, uye kupisa kwemaminetsi matatu mukugeza nemvura: ruvara rwepepuru runokura.
(2) Ku 2 mL yemushonga weLevodopa (1 mu5000) wedzera 10 mL ye4-aminoantipyrine TS, uye zunza: ruvara rutsvuku runokura.
(3) Dissolve 3 mg yeLevodopa mu 0.001 mol / L hydrochloric acid TS kuita 100 mL.Sarudza iyo absorption spectrum yemhinduro sekurairwa pasi peUltravioletvisible Spectrophotometry <2.24>, uye enzanisa iyo spectrum neReference Spectrum: ese ari maviri anoratidza kusimba kwakafanana kwekunyura paawavelengths akafanana.
Absorbance <2.24> E 1% 1cm (280 nm): 136-146 (mushure mekuoma, 30 mg, 0.001 mol/L hydrochloric acid TS, 1000 mL).
Optical Rotation <2.49> [a]20D:-11.5° ~-13.0°(mushure mekuoma, 2.5 g, 1 mol/L hydrochloric acid TS, 50 mL, 100 mm).
Kuchena
(1) Kujeka uye ruvara rwekugadzirisa-Dissolve 1.0 g yeLevodopa mu 20 mL ye 1 mol / L hydrochloric acid TS: mhinduro yakajeka uye isina ruvara.
(2) Chloride <1.03>-Dissolve 0.5 g yeLevodopa mu6 mLof dilute nitric acid, woisa mvura kuita 50 mL.Ita bvunzo uchishandisa iyi mhinduro seyeyedzo mhinduro.Gadzirira mhinduro yekudzora ne 0.30 mL ye0.01 mol/L hydrochloricacid VS (kwete kupfuura 0.021%).
(3) Sulfate <1.14>-Dissolve 0.40 g yeLevodopa mu1 mL ye dilute hydrochloric acid uye 30 mL yemvura, woisa mvura kuita 50 mL.Ita bvunzo uchishandisa iyi mhinduro seyeyedzo mhinduro.Gadzirira mhinduro yekudzora ne 0.25 mL ye0.005 mol/L sulfuric acid VS (kwete kupfuura 0.030%).
(4) Heavy Metals <1.07>-Rambai ne 1.0 g yeLevodopa maererano neMethod 2, uye ita muedzo.Gadzirira mhinduro yekudzora ne 2.0 mL yeStandard Lead Solution (kwete kupfuura 20 ppm).
(5) Arsenic <1.11> -Dissolve 1.0 g yeLevodopa mu 5 mLof dilute hydrochloric acid, uye ita muedzo nemhinduro iyi semhinduro yekuedza (kwete kupfuura 2 ppm).
(6) Zvinhu zvinoenderana-Dissolve 0.10 g yeLevodopa mu10 mL ye sodium disulfite TS, uye shandisa mhinduro iyi semuenzaniso wemhinduro.Pipet 1 mL yemhinduro yemuenzaniso, wedzera sodium disulfite TS kuti iite 25 mL chaiyo.Pipeti 1 mL yemhinduro iyi, wedzera sodium disulfite TS kugadzira chaizvo 20 mL, uye shandisa iyi mhinduro seyakajairwa mhinduro.Ita bvunzo nemhinduro idzi sekurairwa pasi peThin-layer Chro-matography <2.03>.Spot 5mL imwe neimwe yemuenzaniso mhinduro uye yakajairwa mhinduro pandiro ye cellulose kune yakaonda-layerchromatography.Gadzira ndiro nemusanganiswa we1-butanol, mvura, acetic acid (100) uye methanol (10:5:5:1) kureba ingangoita masendimita gumi, uye woomesa ndiro.Sprayevenly mhinduro yeninhydrin muacetone (1 mu50) mundiro uye kupisa pa90 ℃ kwemaminetsi gumi: makwapa kunze kwenzvimbo huru kubva kumuenzaniso mhinduro haana kusimba kupfuura nzvimbo kubva kune yakajairwa mhinduro.
Kurasikirwa paKuomesa <2.41> Kwete kupfuura 0.30% (1 g, 105℃,3 maawa).
Residue paIgnition <2.44> Kwete kupfuura 0.1% (1 g).
Assay Wema nemazvo nezve 0.3 g yeLevodopa, yakamboomeswa, nyungudika mu3 mL yeformic acid, wedzera 80 mL yeacetic acid (100), uye titrate <2.50> ne0.1 mol/L perchloric acid VS kusvika ruvara rwemushonga rwachinja. kubva kupepuru kuburikidza nebhuruu-girinhi kusvika kugirinhi (chiratidzo: 3 madonhwe ecrystalviolet TS).Ita chisungo chisina chinhu, uye ita chero gadziriso inodiwa.
Imwe mL ye0.1 mol/L perchloric acid VS＝19.72 mg yeC9H11NO4
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