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

Kev sib hloov kho qhov muag [EP]
Dissolve ib tug kom muaj nuj nqis sib npaug rau 0.200g ntawm dreied tshuaj thiab 5g ntawm hexamethylenetetramine R nyob rau hauv 10ml ntawm 1mol / L hydrochloric acid thiab dilute mus rau 25.oml nrog tib cov kua qaub.Cia qhov kev daws teeb meem los tiv thaiv lub teeb rau 3h.Lub kaum sab xis ntawm kev sib hloov kho qhov muag yog -1.27 ° txog -1.34 °
Qhov tshwm sim ntawm kev daws teeb meem
Disslove 1.0g hauv 1mol / L hydrochloric acid thiab dilute mus rau 25ml nrog tib solvnet.Cov tshuaj tsis muaj xim ntau dua li kev siv tshuaj BY6.
Related Substances [EP]
Tshawb xyuas los ntawm nyias txheej chromatography, siv cellulose rau chromatography R ua cov txheej txheem.
Test tov-Dissolve 0.1g ntawm cov tshuaj yuav tsum tau kuaj nyob rau hauv 5ml ntawm anhydrous formic acid R thiab dilute mus rau 10ml nrog methanol R. Npaj tam sim ua ntej siv.
Kev siv tshuaj (a)-Dilute 0.5ml ntawm cov tshuaj ntsuam xyuas rau 100ml nrog methanol R.
Reference solution (b)-Dissolve 30mg of tyrosine R in 1ml of anhydrous formic acid R thiab dilute to 100ml with methanol R. Mix 1ml of this solution with 1ml of the test solution.
Siv nyias rau lub phaj li bands 20mm ntev, 1oμl ntawm cov tshuaj ntsuam xyuas, 10μl ntawm kev siv tshuaj (a) thiab 20μl ntawm kev siv tshuaj (b).Qhuav nyob rau hauv ib tug tam sim no ntawm huab cua.Tsim ib txoj kev od 15cm siv sib tov ntawm 50 ntim ntawm butanol R, 25 ntim ntawm glacial acetic acid R thiab 25 ntim dej.Qhuav lub phaj nyob rau hauv ib tug tam sim no ntawm huab cua sov thiab tshuaj tsuag nrog ib tug freshly npaj sib tov ntawm sib npaug volumed ntawm 10 feem pua ​​m/v tov ntawm ferric chloride R thiab ib tug 5 feem pua ​​m/v tov ntawm postassium ferricyanide R. Tshawb xyuas cov chromatoframs tam sim ntawd.Txhua qhov chaw hauv chromatogram tau txais nrog cov tshuaj ntsuam xyuas, sib nrug los ntawm qhov chaw tseem ceeb, tsis yog khaus ntau dua li qhov chaw hauv chromatogram ibtained nrog kev siv tshuaj (a) qhia.Qhov kev ntsuam xyuas tsis siv tau tshwj tsis yog tias cov chromatogram tau txais nrog kev siv tshuaj (b) qhia tau hais tias, saum toj no lub hauv paus chaw, ib qho chaw sib txawv uas yog khaus tshaj qhov chaw hauv chromatogram tau nrog kev siv tshuaj (a).
UV Spectrum [EP]
Disslove 30.0mg hauv 0.1mol / L hydrochloric acid thiab dilute rau 100.oml nrog tib cov kua qaub.Dilute 10.0ml ntawm cov tshuaj no rau 100.0ml nrog 0.1mol / L hydrochloric acid.Kev tshuaj xyuas ntawm 230nm thiab 350nm, cov tshuaj qhia tau hais tias ib qho kev nqus siab tshaj plaws ntawm 280nm.Qhov tshwj xeeb absorbance ntawm qhov siab tshaj plaws no yog 137 txog 147, suav nrog siv rau cov khoom qhuav.
Poob rau ziab
Noj cov khoom no, qhuav mus tas li qhov hnyav ntawm 105 ° C, qhov hnyav poob yuav tsum tsis pub tshaj 1.0% (Txoj cai 0831).
Residue ntawm Ignition (Sulfated)
Noj l.0g ntawm Levodopa thiab xyuas nws raws li txoj cai (Txoj cai 0841).Cov seem seem yuav tsum tsis pub tshaj 0.1%.
Hnyav Hlau
Cov seem tshuav nyob rau hauv cov khoom ntawm kev noj cov khoom siv hluav taws xob yuav tsum tsis txhob muaj ntau tshaj 10 feem ntawm ib lab ntawm cov hlau hnyav thaum kuaj xyuas los ntawm txoj cai lij choj (General Principles 0821, Law II).
pH Test
0.10g hauv 10ml ntawm H2O co rau 15 feeb.
Kev txiav txim siab txog cov ntsiab lus
Noj cov khoom no txog 0.lg, precision hnyav, ntxiv anhydrous formic acid 2ml kom yaj, ntxiv glacial acetic acid 20ml, co, ntxiv crystal violet qhia 2 tee, nrog perchloric acid titration tov (0.1 mol / L) titration rau cov tshuaj yog ntsuab, thiab qhov tshwm sim ntawm titration yog kho nrog ib qho kev kuaj dawb paug.Txhua 1 ml ntawm perchloric acid titration tov (0.1 mol / L) sib raug rau 19.72mg ntawm C9H11N04.

JP17 Test Method

Levodopa, thaum qhuav, muaj tsawg dua 98.5% ntawm Levodopa (C9H11NO4).
Kev piav qhia Levodopa tshwm sim dawb los yog me ntsis greyish dawb, muaju los yog crystalline hmoov.Nws yog tsw ntxhiab.Nws yog dawb do soluble nyob rau hauv formic acid, me ntsis soluble nyob rau hauv dej, thiab xyaum insoluble nyob rau hauv ethanol (95).Nws dissolves nyob rau hauv dilute hydrochloric acid.Cov pH ntawm cov kua dej txaus ntawm Levodopa yog nyob nruab nrab ntawm 5.0 thiab 6.5.Melting point: txog 275 ℃ (nrog decomposition).
Kev txheeb xyuas
(1) Rau 5 mL ntawm ib qho kev daws ntawm Levodopa (1 ntawm 1000) ntxiv 1mL ntawm ninhydrin TS, thiab cua sov rau 3 feeb hauv dej da dej: xim liab.
(2) Rau 2 mL ntawm kev daws ntawm Levodopa (1 hauv 5000) ntxiv 10 mL ntawm 4-aminoantipyrine TS, thiab co: xim liab tsim.
(3) Dissolve 3 mg ntawm Levodopa hauv 0.001 mol / L hydrochloric acid TS kom 100 mL.Txiav txim siab qhov nqus spectrum ntawm cov tshuaj raws li qhia nyob rau hauv Ultravioletvisible Spectrophotometry <2.24>, thiab sib piv cov spectrum nrog Reference Spectrum: ob qho tib si spectrum qhia zoo sib xws ntawm kev nqus ntawm tib lub wavelengths.
Absorbance <2.24> E 1% 1cm (280 nm): 136-146 (tom qab ziab, 30 mg, 0.001 mol/L hydrochloric acid TS, 1000 mL).
Optical Rotation <2.49> [a]20D:-11.5° ~-13.0° (tom qab ziab, 2.5 g, 1 mol/L hydrochloric acid TS, 50 mL, 100 mm).
Purity
(1) Clarity thiab xim ntawm cov kua - Dissolve 1.0 g ntawm Levodopa nyob rau hauv 20 mL ntawm 1 mol / L hydrochloric acid TS: cov tshuaj yog ntshiab thiab tsis muaj xim.
(2) Chloride <1.03>- Dissolve 0.5 g ntawm Levodopa hauv 6 mLof dilute nitric acid, thiab ntxiv dej kom 50 mL.Ua qhov kev sim siv qhov kev daws teeb meem no raws li qhov kev sim tshuaj.Npaj cov tshuaj tswj nrog 0.30 mL ntawm 0.01 mol / L hydrochloricacid VS (tsis ntau tshaj 0.021%).
(3) Sulfate <1.14>- Dissolve 0.40 g ntawm Levodopa hauv 1 mL ntawm dilute hydrochloric acid thiab 30 mL dej, thiab ntxiv dej kom 50 mL.Ua qhov kev sim siv qhov kev daws teeb meem no raws li qhov kev sim tshuaj.Npaj cov tshuaj tswj nrog 0.25 mL ntawm 0.005 mol / L sulfuric acid VS (tsis ntau tshaj 0.030%).
(4) Heavy Metals <1.07>-Tau nrog 1.0 g ntawm Levodopa raws li Txoj Kev 2, thiab ua qhov kev sim.Npaj cov tshuaj tswj nrog 2.0 mL ntawm Standard Lead Solution (tsis ntau tshaj 20 ppm).
(5) Arsenic <1.11>-Dissolve 1.0 g ntawm Levodopa hauv 5 mLof dilute hydrochloric acid, thiab ua qhov kev sim nrog cov tshuaj no raws li cov tshuaj ntsuam xyuas (tsis ntau tshaj 2 ppm).
(6) Lwm yam tshuaj-Dissolve 0.10 g ntawm Levodopa hauv 10 mL ntawm sodium disulfite TS, thiab siv cov tshuaj no ua cov qauv tshuaj.Pipet 1 mL ntawm cov qauv tov, ntxiv sodium disulfite TS kom raws nraim 25 mL.Pipet 1 mL ntawm cov tshuaj no, ntxiv sodium disulfite TS ua raws nraim 20 mL, thiab siv cov tshuaj no raws li cov qauv kev daws teeb meem.Ua qhov kev sim nrog cov kev daws teeb meem no raws li qhia hauv Thin-txheej Chro-matography <2.03>.Spot 5mL txhua tus qauv tov thiab cov txheej txheem tov rau ntawm ib phaj ntawm cellulose rau nyias-layerchromatography.Tsim lub phaj nrog kev sib xyaw ntawm 1-butanol, dej, acetic acid (100) thiab methanol (10: 5: 5: 1) mus rau qhov deb li ntawm 10 cm, thiab cua qhuav lub phaj.Txau ib qho kev daws teeb meem ntawm ninhydrin hauv acetone (1 hauv 50) ntawm lub phaj thiab cua sov ntawm 90 ℃ rau 10 feeb: cov chaw uas tsis yog qhov chaw tseem ceeb ntawm cov qauv tshuaj tsis yog khaus ntau dua li qhov chaw los ntawm cov txheej txheem kev daws teeb meem.
Poob rau ziab <2.41> Tsis ntau tshaj 0.30% (1 g, 105 ℃, 3 teev).
Residue ntawm Ignition <2.44> Tsis ntau tshaj 0.1% (1 g).
Kev ntsuas qhov hnyav yog kwv yees li 0.3 g ntawm Levodopa, yav tas los qhuav, yaj hauv 3 mL ntawm formic acid, ntxiv 80 mL ntawm acetic acid (100), thiab titrate <2.50> nrog 0.1 mol / L perchloric acid VS kom txog thaum cov xim hloov pauv. los ntawm ntshav los ntawm xiav-ntsuab mus rau ntsuab (qhov taw qhia: 3 tee ntawm crystalviolet TS).Ua ib qho kev txiav txim siab dawb paug, thiab kho qhov tsim nyog.
Txhua mL ntawm 0.1 mol / L perchloric acid VS ＝19.72 mg ntawm C9H11NO4
Containers thiab cia Containers-Tight containers.
Cia-Lub teeb-resistant.