D-Phenylalanine CAS 673-06-3 (HD-Phe-OH) Qiimaynta 98.0~102.0% Warshada 50MT/Bishii

1. Muuqashada-- Kormeerka muuqaalka
2. Wareeg gaar ah --wareejin gaar ah ayaa lagu cabbiraa si waafaqsan GB/T613-1988
Tusaalaha diyaarinta: Si sax ah u miisaam muunada 0.5000g oo u guuri dhalada mug leh ee 50ml nadiif ah oo qalalan, ku dar 20ml biyo ah, dabool dhalada, rux si ay u milanto,kadibna miisaanka ku qas biyo.
Tijaabi: Ku hagaaji eber gyroscope-ka tijaabada ka hor, ka dibna ku shub tuubada tijaabada xalka muunada, duub xagasha wareega, oo ku xisaabi wareega gaarka ah ee muunada adigoo isticmaalaya qaacidada soo socota.
[а] D20 = (r×50) ÷(L×W)
Halkee:
[а] D20: Wareegga indhaha ee gaarka ah ee 20℃ ee xalka muunada
r: wareegga indhaha ee lagu arkay 20 ℃ ee xalka muunada
50: Mugga xal muunad la diyaariyey (ml)
w: Tusaalaha miisaanka (g)
L: Dhererka tuubada wareegga indhaha (dm)
3. Hadhaaga gubanaya
Qaado qiyaastii 1g oo alaabtan ah oo kuleyl 600 ℃, kuleyli ilaa ay gebi ahaanba dambaska ka noqoto sida waafaqsan xeerka Lifaaqa Ⅷ N ee Qaybta II ee daabacaadda CP2010, ku dar 0.5-1.0ml sulfuric acid oo xoog leh oo kuleyli (700 ℃- 800 ℃) miisaan joogto ah.
3.1 "Hadhaaga Incandescent" ee Habkan (Pharmacopoeia Chinese 2005 Edition, Qaybta II Lifaaqa Ⅷ N) waxaa loola jeedaa oxides birta ama sulfates ka dib marka daawooyinka (inta badan xeryahooda organic) la kululeeyo ilaa gebi ahaan ash, ka dibna sulfuric acid lagu daray 0.5 ~ 1.0ml iyo incandesced (700 ~ 800 ℃) miisaan joogto ah.
4 Nadiifnimada Chiral (HPLC)
Qalabka: chromatography dareeraha waxqabadka sare, baaraha PDA.Isku dheelitirka falanqaynta elegtarooniga ah, reagent;Heerka chromatography
Xaaladaha Chromatographic: Column: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm,5ul, mowjadaha ogaanshaha, heerka socodka, cabbirka muunada: 10 u L (tixraac) khafiif ah: biyaha, wakhtiga ururinta xogta: 20.00min.
Go'aaminta muunada: Muunadda ayaa loo falanqeeyay iyadoo la raacayo nidaamka muunad ee soo socda: 1 irbad xal madhan iyo 1 irbad tixraac DL-phenylalanine ah.
1 xal muunad irbad,
Xisaabinta Natiijooyinka: Waxa ku jira HPLC waxaa la go'aamiyay in ay ka yar tahay 0.5% iyadoo loo eegayo aagga caadiga ah ee ugu sarreeya iyo ka-goynta bannaan.
5. Qalalan oo aan miisaan lahayn
5.1 Qalabka:
Foornada kuleylka kuleylka, 1/10,000 dheelitirnaan.
5.2 Habka:
Dhalo miisaankeedu siman yahay oo leh miisaan joogto ah iyo daboolka afka dhulka oo aad u engegan, miisaan 1 garaam (sax ah ilaa 0.0001 garaam) ee muunada.Muunada waa in si siman loogu faafiyaa gunta dhalada miisaanka oo dhumucdiisu aanay ka badnayn 10mm, waa in lagu ridaa foorno heerkulbeeg ah oo koronto ah, qallaji 105-110 ℃ 3 saacadood, ka dibna u gudub qolka qalajinta si aad u qaboojiso heerkulka qolka ee miisaanka.
Xisaabinta: Miisaanka qallalan %= (M1-M2) ÷M×100
Halka: M1: cufnaanta muunadda iyo dhalada cabbirka ka hor inta aan la qalajin, garaam
M2: Cuf muunad iyo dhalada cabbiraadda qallajinta ka dib, garaam
M: Tirada muunad, garaam
Tallaabada 6: Waxa ku jira
6.1 Qalabka
chromatography dareere waxqabadka sare leh, PDA detector.
Isku dheelitirka falanqaynta elegtarooniga ah
6.2 Reagent
Acetonitrile (darajada chromatographic), TFA (darajada chromatographic)
6.3 Xaaladaha Chromatographic
6.3.1 Tiirka: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Dhererka mowjadda ogaanshaha: INC220nm
Heerka socodka:1.0ml/min
Cabbirka Tusaalaha: 10μL (Tixraac)
Khafiifsan: Acetonitrile
Waqtiga aruurinta xogta: 20.00min
6.4 diyaarinta wajiga wareega
Marxaladda wareega A (0.1% trifluoroacetic acid water): nuugista saxda ah 2. Ku qas Oml trifluoroacetic acid biyo ilaa 2000m1, si fiican isku qas, iyo degas;
Marxaladda wareega B (0.1% acetonitrile trifluoroacetic acid): nuugista saxda ah ee 2.Oml trifluoroacetic acid ayaa lagu qasi jiray 2000m1 oo leh acetonitrile, isku dhafan oo hoos u dhacay;
6.5 barnaamijka gradient wajiga mobile
Waqtiga (daqiiqo) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Diyaarinta xal muunad
Miisaam oo milaan 0.1g muunadda leh acetonitrile, ku milo 100m1, si fiican u rux si aad u isticmaasho, ama isku-fiirsasho isku mid ah.U diyaari laba muunado oo isbarbar socda.
6.7 Tusaalaha Go'aaminta
U falanqeyso muunada iyadoo la raacayo nidaamka muunada ee soo socota:
In ka badan 1 duritaan oo xal maran
1 muunada muunada irbadda 1#
1 muunada muunada irbadda 2#
6.8 Natiijooyinka Xisaabinta
2.8.1 Habka caadiga ah ee aagga ugu sarreeya ayaa la isticmaalay si loo xisaabiyo nadiifinta HPLC iyada oo laga jarayo meel bannaan.
2.8.2 Macnaha qaraabo leexinta nadiifinta laba irbadood waa in aanu ka badnayn 1%
2.8.3 Haddii natiijooyinka labada irbadood ay buuxiyaan shuruudaha aqbalaadda, celceliska nadiifinta ayaa loo qaataa natiijada kama dambaysta ah.