Levodopa (L-DOPA) CAS 59-92-7 99.0~100.5% USP BP EP Paerewa Mate Anti-Parkinson Te Pure

Hurihuri Matapihi [EP]
Whakarewahia te rahinga e rite ana ki te 0.200g o te matū kua maroke me te 5g o te hexamethylenetetramine R ki te 10ml o te 1mol/L waikawa pūhaumāota ka waimeha ki te 25.oml me te waikawa rite.Tukua te otinga kia tu maru i te marama mo te 3 haora.Ko te koki o te hurihanga whatu ko -1.27° ki te -1.34°
Te ahua o te otinga
Wewetehia te 1.0g ki te 1mol/L waikawa pūhaumāota me te waimeha ki te 25ml ki te solvnet taua.Ko te otinga kaore i te kaha ake te tae ki te otinga tohutoro BY6.
Nga matū e pa ana [EP]
Ka tirohia ma te whakamaarama papa angiangi, ma te whakamahi i te cellulose mo te chromatography R hei matū paninga.
Te otinga whakamatautau-Tarekahia te 0.1g o te matū ka tirohia ki te 5ml o te waikawa waikawa R ka waimeha ki te 10ml ki te methanol R. Whakaritea i mua tonu i te whakamahinga.
Wairewa tohutoro (a)-Warekahia te 0.5ml o te otinga whakamatautau ki te 100ml me te mewaro R.
Wairewa tohutoro (b)-Warekahia te 30mg o te tyrosine R ki te 1ml o te waikawa puka R ka waimeha ki te 100ml me te methanol R. Whakaranuhia te 1ml o tenei otinga ki te 1ml o te wairewa whakamatautau.
Hoatu motuhake ki te pereti hei roopu 20mm te roa, 1oμl o te otinga whakamatautau, 10μl o te otinga tohutoro (a) me te 20μl o te otinga tohutoro (b).Ka maroke i roto i te ia o te hau.Whakawhanakehia ki runga i te ara o te 15cm ma te whakamahi i te ranunga o te 50 pukapuka o te butanol R, te 25 o te waikawa ahetiki huka R me te 25 o te wai.Me whakamaroke te pereti ki roto i te hau mahana ka rehuhia ki te ranunga hou kua rite te ruri o te 10 paiheneti m/v otinga o te ferric chloride R me te 5 paiheneti m/v wairewa o postassium ferricyanide R. Tirohia nga chromatoframs tonu.Ko nga waahi katoa o te chromatogram i whiwhi ki te otinga whakamatautau, haunga te waahi matua, kaore i te kaha ake i te waahi o te chromatogram i whiwhi me te otinga tohutoro (a).Karekau te whakamatautau i te whaimana mena ka whakaatuhia e te chromatogram me te otinga tohutoro (b), kei runga ake i te waahi matua, he waahi motuhake ka kaha ake i te waahi o te chromatogram i whiwhi ki te otinga tohutoro (a).
Hiranga UV [EP]
Whakakorehia te 30.0mg ki te 0.1mol/L waikawa pūmāota me te waimeha ki te 100.oml me te waikawa rite.Ringihia te 10.0ml o tenei wairewa ki te 100.0ml me te 0.1mol/L waikawa pūhaumāota.Ka tirohia i waenga i te 230nm me te 350nm, ko te otinga e whakaatu ana i te morahi whakaurunga kotahi ki te 280nm.Ko te 137 ki te 147 te whakaurunga motuhake i tenei morahi, ka tatauhia me te tohutoro ki te matū maroke.
Ngaronga i te whakamaroke
Tangohia tenei hua, maroke ki te taumaha tonu i te 105°C, kaua e neke ake te mate taimaha i te 1.0% (Ture Whanui 0831).
Te toenga i runga i te mura (Sulfated)
Tangohia te l.0g o Levodopa ka tirohia kia rite ki te ture (Ture whanui 0841).Ko te toenga e toe ana kaua e neke ake i te 0.1%.
Nga Korewa Taamaha
Ko te toenga e waiho ana i raro i te mea tango i te toenga mura kia kaua e neke ake i te 10 nga wahanga mo ia miriona o te konganuku taumaha ina tirohia e te ture (General Principles 0821, Ture II).
Whakamātautau pH
0.10g i roto i te 10ml o H2O ruru mo te 15 meneti.
Te whakatau ihirangi
Tangohia tenei hua e pā ana ki te 0.lg, te taimaha tika, tāpirihia te waikawa formic anhydrous 2ml ki te memeha, tāpiri waikawa acettic glacial 20ml, ruru, tāpiri tohu puru karaihe 2 pata, ki te wairewa titration waikawa perchloric (0.1 mol/L) titration ki te otinga ko kakariki, ka whakatikahia te hua o te titration me te whakamatautau paratea.Ia 1 ml o te wairewa titration waikawa perchloric (0.1 mol/L) e rite ana ki te 19.72mg o C9H11N04.

JP17 Tikanga Whakamatau

Levodopa, ina whakamaroke, kaua e iti iho i te 98.5% o Levodopa (C9H11NO4).
Whakaahuatanga Ko te Levodopa he ma, he paku hina, he kiripiri, he paura tioata ranei.He haungakore.He memeha noa i roto i te waikawa formic, he paku whakarewa ki te wai, he kore noa ki te waiwaro (95).Ka memeha ki roto i te waikawa puota waimeha.Kei waenganui i te 5.0 me te 6.5 te pH o te wairewa kukū o Levodopa.Ira whakarewa: tata ki te 275 ℃ (me te pirau).
Tautuhinga
(1) Ki te 5 mL o te otinga o Levodopa (1 i roto i te 1000) tāpirihia te 1mL o te ninhydrin TS, ka whakamahana mo te 3 meneti i roto i te pati wai: ka puta he tae papura.
(2) Ki te 2 mL o te otinga o Levodopa (1 i roto i te 5000) tāpirihia te 10 mL o te 4-aminoantipyrine TS, ka wiri: ka puta he tae whero.
(3) Whakarewahia te 3 mg o Levodopa ki te 0.001 mol/L waikawa pūhaumāota TS hei hanga 100 mL.Whakatauhia te tuāwhiorangi horomanga o te otinga i raro i te Ultravioletvisible Spectrophotometry <2.24>, ka whakatairitehia te tuāwhiorangi ki te Tohu Tohutoro: e whakaatu ana nga tuāwhiorangi e rua i te kaha o te horomanga i nga roangaru kotahi.
Absorbance <2.24> E 1%1cm (280 nm): 136-146 (i muri i te whakamaroketanga, 30 mg, 0.001 mol/L waikawa pūmāota TS, 1000 mL).
Te hurihanga Optical <2.49> [a]20D:-11.5° ~-13.0°(i muri i te whakamaroketanga, 2.5 g, 1 mol/L waikawa pūhaumāota TS, 50 mL, 100 mm).
Maamaa
(1) Te marama me te tae o te wairewa-Warekahia te 1.0 g Levodopa ki te 20 mL o te 1 mol/L waikawa pūhaumāota TS: he maama te otinga, he kore tae.
(2) Chloride <1.03>-Warekahia te 0.5 g o Levodopa ki te 6 mLof waimeha waikawa nitric, ka tapirihia he wai kia 50 mL.Mahia te whakamatautau ma te whakamahi i tenei otinga hei otinga whakamatautau.Whakaritehia te otinga whakahaere me te 0.30 mL o te 0.01 mol/L hydrochloricacid VS (kaua e neke ake i te 0.021%).
(3) Sulfate <1.14>-Whakarewahia te 0.40 g o Levodopa ki te 1 mL o te waikawa maaota waimeha me te 30 mL wai, ka tapirihia he wai kia 50 mL.Mahia te whakamatautau ma te whakamahi i tenei otinga hei otinga whakamatautau.Whakapaia te otinga mana me te 0.25 mL o te 0.005 mol/L waikawa pungatara VS (kaore e neke ake i te 0.030%).
(4) Heavy Metals <1.07>-Haere ki te 1.0 g o Levodopa kia rite ki te Tikanga 2, ka mahi i te whakamatautau.Whakaritehia te otinga mana me te 2.0 mL o te Wairewa Matarahi Paerewa (kaua e neke ake i te 20 ppm).
(5) Arsenic <1.11>-Warekahia te 1.0 g o Levodopa ki roto i te 5 mLof waimeha waikawa maata, ka mahia te whakamatautau me tenei otinga hei otinga whakamatautau (kaua e neke ake i te 2 ppm).
(6) Nga matū e pa ana-Whakarewa 0.10 g Levodopa ki te 10 mL o te konutai disulfite TS, ka whakamahi i tenei otinga hei tauira otinga.Pipeto 1 mL o te tauira otinga, tāpirihia te konutai disulfite TS kia rite te 25 mL.Pipeto 1 mL o tenei wairewa, tapirihia te konutai disulfite TS kia rite te 20 mL, ka whakamahi i tenei otinga hei otinga paerewa.Mahia te whakamatautau me enei otinga i raro i te Tohu-papa angiangi Chro-matography<2.03>.Tuhia te 5mL o ia tauira otinga me te otinga paerewa ki runga i te pereti cellulose mo te chromatography paparanga angiangi.Whakawhanakehia te pereti me te ranunga o te 1-butanol, te wai, te waikawa acetic (100) me te mewaro (10:5:5:1) ki te 10 cm te tawhiti, ka whakamarokehia te pereti.Ringihia he wairewa ninhydrin i roto i te acetone (1 i roto i te 50) ki runga i te pereti me te whakamahana i te 90 ℃ mo te 10 meneti: ko nga wahi i tua atu i te waahi matua mai i te tauira otinga kaore i te kaha ake i te waahi mai i te otinga paerewa.
Ngaronga i te whakamaroke <2.41> Kaua e neke ake i te 0.30%(1 g, 105℃,3 haora).
Te toenga i runga i te mura <2.44> Kaua e neke ake i te 0.1% (1 g).
Whakatauhia te pauna tika mo te 0.3 g o Levodopa, kua maroke i mua, memeha ki te 3 mL o te waikawa formic, tāpirihia te 80 mL o te waikawa ahetiki (100), ka titrate <2.50> ki te 0.1 mol/L perchloric acid VS tae noa ki te rereke o te tae o te otinga. mai i te papura mai i te puru-matomato ki te kaakaariki (tohu: 3 nga pata o te crystalviolet TS).Whakaritehia he whakatau patea, ka whakatikahia.
Ia mL o te 0.1 mol/L waikawa perchloric VS＝19.72 mg o C9H11NO4
Ipu me te rokiroki Ipu-Tight ipu.
Rokiroki-Marama-aukati.