D-Phenylalanine CAS 673-06-3 (HD-Phe-OH) Assay 98.0~102.0% Factory 50MT/Mwezi

1. Maonekedwe-- Kuyang'ana kowoneka
2. Kuzungulira kwachindunji-- Kuzungulira kwapadera kumayesedwa molingana ndi GB/T613-1988
Kukonzekera kwachitsanzo: Yezerani bwino chitsanzo cha 0.5000g ndikusunthira ku botolo loyera ndi louma la 50ml voliyumu, onjezerani madzi 20ml, kuphimba botolo, kuligwedeza kuti lisungunuke, ndiyeno tsitsani pa sikelo ndi madzi.
Mayeso: Sinthani zero ya gyroscope mayeso asanayesedwe, kenaka tsitsani chubu choyesera ndi yankho lachitsanzo, lembani ngodya yozungulira, ndikuwerengera kusinthasintha kwachitsanzo ndi formula iyi.
[а]D20 = (r×50) ÷(L×W)
Kumene:
[а]D20: Kusintha kwapadera kwa kuwala kwa 20 ℃ ya chitsanzo cha yankho
r: Kuzungulira kwa kuwala komwe kumawonedwa pa 20 ℃ kwa yankho lachitsanzo
50: Voliyumu yachitsanzo chokonzekera (ml)
w: kulemera kwachitsanzo (g)
L: Kutalika kwa chubu chozungulira (dm)
3. Kuwotcha zotsalira
Tengani pafupifupi 1g ya mankhwalawa ndikuwotchera pa 600 ℃, tenthetsani mpaka phulusa lathunthu molingana ndi lamulo la Zowonjezera Ⅷ N wa Gawo II la CP2010 Edition, onjezerani 0.5-1.0ml wa sulfuric acid ndikuwotcha (700 ℃ - 800 ℃) kulemera kosalekeza.
3.1 "Zotsalira za incandescent" mu Njira iyi (Chinese Pharmacopoeia Edition 2005, Gawo II Zowonjezera Ⅷ N) zimatanthawuza ma oxides achitsulo kapena sulfate otsala pambuyo potenthetsa mankhwala (makamaka organic) mpaka phulusa lathunthu, kenako sulfuric acid imawonjezeredwa 0.5 ~ 1.0ml ndi incandesced (700 ~ 800 ℃) kulemera kosalekeza.
4 Chiral purity (HPLC)
Zida: High performance liquid chromatography, PDA chowunikira.Electronic analytical balance, reagent;Mlingo wa chromatography
Makhalidwe a Chromatographic: Mzere: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm, 5ul, kutalika kwa kutalika kwa kutalika, kuthamanga, kukula kwa chitsanzo : 10 u L (reference) woonda: madzi, nthawi yosonkhanitsa deta :20.00min.
Kutsimikiza kwachitsanzo: Chitsanzocho chinawunikidwa motsatira ndondomeko zotsatirazi: singano ya 1 yopanda kanthu ndi singano ya 1 ya DL-phenylalanine reference.
1 chitsanzo cha singano yankho,
Kuwerengera Zotsatira: Zomwe zili mu HPLC zidatsimikizika kukhala zosakwana 0.5% kutengera kukhazikika kwamalo okhazikika komanso kuchotsera opanda kanthu.
5. Zouma ndi zopanda kulemera
5.1 Zida:
Thermostatic kuyanika uvuni, 1/10,000 bwino.
5.2 Ndondomeko:
Mu botolo loyezera lathyathyathya lokhala ndi kulemera kosalekeza ndi chivundikiro cha pakamwa chowuma kwambiri, yezani 1 gramu (yolondola mpaka 0.0001 gramu) ya chitsanzo.Zitsanzo ziyenera kufalikira pansi pa botolo lolemera ndi makulidwe osapitirira 10mm, kuyika mu uvuni wamagetsi wa thermostatic, wouma pa 105-110 ℃ kwa maola 3, kenako ndikulowa m'chipinda choyanika kuti muzizizira. kutentha kwa chipinda poyeza.
Kuwerengera: Kutaya kuwonda %= (M1-M2) ÷M×100
Kumene: M1: kuchuluka kwa zitsanzo ndi botolo loyezera musanayanike, magalamu
M2: Unyinji wa zitsanzo ndi botolo loyezera mutatha kuyanika, mu magalamu
M: Zitsanzo za kulemera, magalamu
Gawo 6: Zamkatimu
6.1 Zida
High performance liquid chromatography, PDA chowunikira.
Electronic analytical balance
6.2 Reagents
Acetonitrile (chromatographic grade), TFA (chromatographic grade)
6.3 Chromatographic Conditions
6.3.1 Mzere: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Kutalika kwa mawonekedwe: INC220nm
Kuthamanga: 1.0mL / min
Kukula kwachitsanzo: 10μL (zofotokozera)
Wochepa thupi: Acetonitrile
Nthawi yosonkhanitsa deta: 20.00min
6.4 Kukonzekera gawo la mafoni
Mobile gawo A (0.1% trifluoroacetic acid madzi): mwatsatanetsatane mayamwidwe 2. Sungunulani Oml trifluoroacetic asidi ndi madzi 2000m1, sakanizani bwino, ndi degas;
Mobile gawo B (0.1% acetonitrile trifluoroacetic acid): mayamwidwe enieni 2.Oml trifluoroacetic asidi anachepetsedwa kuti 2000m1 ndi acetonitrile, wosakaniza ndi deggated;
Pulogalamu ya 6.5 Mobile phase gradient
Nthawi (mphindi) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Kukonzekera chitsanzo cha yankho
Yesani ndi kusungunula chitsanzo cha 0.1g ndi acetonitrile, tsitsani mpaka 100m1, gwedezani bwino kuti mugwiritse ntchito, kapena ndende yomweyo.Konzani zitsanzo ziwiri zofanana.
6.7 Kutsimikiza Kwachitsanzo
Sankhulani chitsanzocho motsatira njira zotsatirazi:
Kupitilira 1 jekeseni wopanda kanthu
1 chitsanzo cha singano yankho 1#
1 singano chitsanzo yankho 2#
6.8 Kuwerengera zotsatira
2.8.1 Njira yokhazikika yamalo okhazikika idagwiritsidwa ntchito kuwerengera chiyero cha HPLC pochotsa malo opanda kanthu.
2.8.2 Chibale chikutanthauza kupatuka kwa chiyero cha singano ziwiri sikuyenera kukhala wamkulu kuposa 1%
2.8.3 Ngati zotsatira za majekeseni onsewa zikugwirizana ndi zovomerezeka, chiyero chapakati chimatengedwa ngati chotsatira chomaliza.