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

Kuzungulira kwa Optical [EP]
Sungunulani kuchuluka kofanana ndi 0.200g ya dreied substance ndi 5g ya hexamethylenetetramine R mu 10ml ya 1mol/L hydrochloric acid ndi kuchepetsa mpaka 25.oml ndi asidi yemweyo.Lolani kuti yankho likhale lotetezedwa ku kuwala kwa 3h.Kuzungulira kwa kuwala ndi -1.27 ° mpaka -1.34 °
Mawonekedwe a Solution
Sungunulani 1.0g mu 1mol/L hydrochloric acid ndi kuchepetsa mpaka 25ml ndi solvnet yomweyo.Yankho lake silikhala lakuda kwambiri kuposa yankho la BY6.
Zofananira [EP]
Yang'anani ndi chromatography yopyapyala, pogwiritsa ntchito cellulose ya chromatography R ngati chinthu chopaka.
Sungunulani njira yothetsera 0.1g ya zinthu zomwe ziyenera kuyesedwa mu 5ml ya anhydrous formic acid R ndi kuchepetsa 10ml ndi methanol R. Konzani mwamsanga musanagwiritse ntchito.
Njira yothetsera (a) -Sungani 0.5ml ya njira yoyesera ku 100ml ndi methanol R.
Reference solution (b) -Sungani 30mg ya tyrosine R mu 1ml ya anhydrous formic acid R ndi kuchepetsa ku 100ml ndi methanol R. Sakanizani 1ml ya yankho ili ndi 1ml ya yankho loyesa.
Ikani padera ku mbale monga magulu 20mm kutalika, 1oμl ya yankho loyesera, 10μl ya yankho lachidziwitso (a) ndi 20μl ya yankho lachidziwitso (b).Yanikani mumphepo yamkuntho.Pangani panjira od 15cm pogwiritsa ntchito ma voliyumu 50 a butanol R, ma voliyumu 25 a glacial acetic acid R ndi ma voliyumu 25 amadzi.Yanikani mbaleyo mu mpweya wofunda ndikupopera ndi chisakanizo chokonzekera chatsopano cha 10 peresenti m/v yankho la ferric chloride R ndi 5 peresenti m/v yankho la postassium ferricyanide R. Yang'anani ma chromatoframs nthawi yomweyo.Malo aliwonse mu chromatogram yopezedwa ndi yankho loyesa, kupatula malo oyambira, sakhala okulirapo kuposa malo omwe ali mu chromatogram yopezeka ndi yankho lolozera (a) kuwonetsa.Kuyesako sikuli kovomerezeka pokhapokha ngati chromatogram yomwe yapezedwa ndi yankho lachidziwitso (b) ikuwonetsa, pamwamba pa malo oyamba, malo enaake omwe ndi olimba kwambiri kuposa malo omwe ali mu chromatogram yopezedwa ndi yankho lazofotokozera (a).
UV Spectrum [EP]
Disslove 30.0mg mu 0.1mol/L hydrochloric acid ndi kuchepetsa ku 100.oml ndi asidi yemweyo.Sungunulani 10.0ml ya yankho ili ku 100.0ml ndi 0.1mol/L hydrochloric acid.Kuyesedwa pakati pa 230nm ndi 350nm, yankho likuwonetsa kuyamwa kamodzi kokha pa 280nm.Zomwe zimayamwa pamlingo uwu ndi 137 mpaka 147, zowerengedwa potengera zinthu zouma.
Kutaya pa Kuyanika
Tengani mankhwalawa, owuma mpaka kulemera kosalekeza pa 105 ° C, kuwonda sikuyenera kupitirira 1.0% (General rule 0831).
Zotsalira pa Ignition (Sulfated)
Tengani l.0g ya Levodopa ndikuyiyang'ana molingana ndi lamulo (General Law 0841).Zotsalira zomwe zatsala siziyenera kupitirira 0.1%.
Zitsulo Zolemera
Zotsalira zomwe zatsala pansi pa chinthu chotengera chotsalira choyatsira sizikhala ndi magawo opitilira 10 pa miliyoni imodzi yazitsulo zolemera zikafufuzidwa ndi lamulo (General Principles 0821, Law II).
Mayeso a pH
0.10g mu 10ml ya H2O kugwedeza kwa mphindi 15.
Kutsimikiza kokhutira
Tengani mankhwalawa za 0.lg, masekeli olondola, onjezani anhydrous formic acid 2ml kuti asungunuke, onjezerani glacial acetic acid 20ml, gwedezani, onjezerani madontho a crystal violet 2, ndi perchloric acid titration solution (0.1 mol / L) titration yankho ndi yankho. wobiriwira, ndipo zotsatira za titration zimakonzedwa ndi mayeso opanda kanthu.1 ml iliyonse ya perchloric acid titration solution (0.1 mol/L) imafanana ndi 19.72mg ya C9H11N04.

Njira Yoyesera ya JP17

Levodopa, ikauma, imakhala yosachepera 98.5% ya Levodopa (C9H11NO4).
Kufotokozera Levodopa imapezeka ngati yoyera kapena yotuwira pang'ono yoyera, makhiristo kapena ufa wonyezimira.Palibe fungo.Imasungunuka momasuka mu formic acid, imasungunuka pang'ono m'madzi, ndipo imakhala yosasungunuka mu ethanol (95).Imasungunuka mu dilute hydrochloric acid.PH ya njira yodzaza ya Levodopa ili pakati pa 5.0 ndi 6.5.Malo osungunuka: pafupifupi 275 ℃ (ndi kuwonongeka).
Chizindikiritso
(1) Ku 5 ml ya yankho la Levodopa (1 mu 1000) onjezerani 1mL ya ninhydrin TS, ndi kutentha kwa mphindi 3 mukusamba kwamadzi: utoto wofiirira umatuluka.
(2) Ku 2 ml ya yankho la Levodopa (1 mu 5000) onjezerani 10 ml ya 4-aminoantipyrine TS, ndikugwedezani: mtundu wofiira umayamba.
(3) Sungunulani 3 mg wa Levodopa mu 0.001 mol/L hydrochloric acid TS kupanga 100 mL.Dziwani kuchuluka kwa mayamwidwe a yankho monga momwe amayankhidwira pansi pa Ultravioletvisible Spectrophotometry <2.24>, ndikuyerekeza mawonekedwewo ndi Reference Spectrum: mawonekedwe onsewa amawonetsa kulimba kofanana kwa kuyamwa pamafunde omwewo.
Absorbance <2.24> E 1% 1cm (280 nm): 136-146 (pambuyo kuyanika, 30 mg, 0.001 mol/L hydrochloric acid TS, 1000 mL).
Kasinthasintha wa Kuwala <2.49> [a]20D:-11.5° ~-13.0°(ataumitsa, 2.5 g, 1 mol/L hydrochloric acid TS, 50 mL, 100 mm).
Chiyero
(1) Kumveka bwino ndi mtundu wa yankho-Sungani 1.0 g ya Levodopa mu 20 ml ya 1 mol/L hydrochloric acid TS: yankho ndi lomveka komanso lopanda mtundu.
(2) Chloride <1.03>-Sungani 0.5 g ya Levodopa mu 6 mLof dilute nitric acid, ndi kuwonjezera madzi kupanga 50 mL.Yesani kugwiritsa ntchito yankho ili ngati yankho loyesa.Konzani njira yowongolera ndi 0.30 mL ya 0.01 mol/L hydrochloricacid VS (osapitirira 0.021%).
(3) Sulfate <1.14>-Sula 0.40 g ya Levodopa mu 1 mL ya dilute hydrochloric acid ndi 30 ml ya madzi, ndikuwonjezera madzi kupanga 50 ml.Yesani kugwiritsa ntchito yankho ili ngati yankho loyesa.Konzani njira yowongolera ndi 0.25 mL ya 0.005 mol/L sulfuric acid VS (osapitirira 0.030%).
(4) Zitsulo Zolemera <1.07>-Pitirizani ndi 1.0 g ya Levodopa molingana ndi Njira 2, ndikuchita mayeso.Konzani njira yowongolera ndi 2.0 mL ya Standard Lead Solution (osapitirira 20 ppm).
(5) Arsenic <1.11> -Sungani 1.0 g ya Levodopa mu 5 mLof kuchepetsa hydrochloric acid, ndikuchita mayeso ndi yankho ili ngati njira yothetsera (osapitirira 2 ppm).
(6) Related zinthu-Sungani 0,10 g wa Levodopa mu10 mL wa sodium disulfite TS, ndi ntchito njira yothetsera chitsanzo.Chitoliro 1 mL cha yankho lachitsanzo, onjezerani sodium disulfite TS kuti mupange ndendende 25 ml.Pipeti 1 mL ya yankho ili, onjezani sodium disulfite TS kuti mupange ndendende 20 mL, ndipo gwiritsani ntchito yankholi ngati yankho lokhazikika.Chitani mayeso ndi mayankho awa monga momwe akuwongolera pansi pa Thin-layer Chro-matography <2.03>.Ikani 5mL iliyonse ya yankho lachitsanzo ndi yankho lokhazikika pa mbale ya cellulose ya thin-layerchromatography.Pangani mbale ndi osakaniza 1-butanol, madzi, asidi asidi (100) ndi methanol (10:5:5:1) mtunda wa pafupifupi 10 cm, ndi mpweya wowumitsa mbale.Njira yothetsera ninhydrin mu acetone (1 mu 50) m'mbale ndi kutentha kwa 90 ℃ kwa mphindi 10: madontho ena kupatula malo ofunikira kuchokera ku yankho lachitsanzo sali olimba kuposa malo omwe amachokera ku yankho lokhazikika.
Kutaya pa Kuyanika <2.41> Osapitirira 0.30% (1 g, 105 ℃,3 maola).
Zotsalira pakuyatsa <2.44> Osapitirira 0.1% (1 g).
Kuyesa Kuyeza molondola za 0.3 g ya Levodopa, yowumitsidwa kale, sungunulani mu 3 ml ya formic acid, onjezerani 80 mL ya acetic acid (100), ndi titrate <2.50> ndi 0.1 mol/L perchloric acid VS mpaka mtundu wa yankho usinthe. kuyambira wofiirira mpaka wobiriwira wobiriwira mpaka wobiriwira (chizindikiro: madontho atatu a crystalviolet TS).Chitani chitsimikiziro chopanda kanthu, ndipo pangani kukonza kulikonse kofunikira.
ML iliyonse ya 0.1 mol/L perchloric acid VS＝19.72 mg ya C9H11NO4
Zotengera ndi zosungirako Zotengera-Zolimba zolimba.
Kusunga-Kuwala zosagwira.