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

1. Te ahua-- Tirotiro tirohanga
2. Te hurihanga motuhake-- Ka inehia te hurihanga motuhake i runga i te GB/T613-1988
Te whakarite tauira: Me ata paunatia te tauira 0.5000g ka nukuhia ki te pounamu volumetric 50ml ma, maroke hoki, ka tapirihia te wai 20ml, ka hipoki i te pounamu, ka ruia kia memeha, katahi ka waimeha ki te tauine ki te wai.
Whakamātautau: Whakaritea te kore o te gyroscope i mua i te whakamatautau, ka utaina te ipuipu whakamatautau me te otinga tauira, tuhia te Koki hurihuri, ka tatau i te hurihanga motuhake o te tauira me te tauira e whai ake nei.
[а]D20 = (r×50) ÷(L×W)
Kei hea:
[a]D20: Te hurihanga whatu motuhake i te 20 ℃ o te otinga tauira
r: Ka kitea te hurihanga mata i te 20 ℃ mo te otinga tauira
50: Rōrahi o te otinga tauira kua rite (ml)
w: Tauira taumaha (g)
L: Roa ngongo hurihuri whatu (dm)
3. Te tahu toenga
Tangohia kia 1 karamu o tenei hua ka whakamahana ki te 600 ℃, whakamahana kia tino pungarehu kia rite ki te ture o te Apiti Ⅷ N o te Wahanga II o te Putanga CP2010, tāpirihia te 0.5-1.0ml waikawa pungatara me te whakamahana (700℃-). 800 ℃) ki te taumaha tonu.
3.1 "Ko te toenga o te rama" i roto i tenei tikanga (Hainamana Pharmacopoeia 2005 Putanga, Wāhanga II Tāpiritanga Ⅷ N) e pā ana ki te waikura whakarewa, pūkawa ngāwha ranei i toe mai i muri i te whakamahanatanga o nga raau taero (te nuinga o nga pūhui waro) tae noa ki te pungarehu, katahi ka taapirihia te waikawa sulfuric 0.5 ~ 1.0ml me te incandesced (700 ~ 800 ℃) ki te taumaha tonu.
4 Pure kirikiri (HPLC)
Nga Taonga: Ko te chromatography wai mahi teitei, te kaitirotiro PDA.Taurite tātari hiko, reagent;Te taumata o te chromatography
Tikanga Chromatographic: Tīwae: Astec CHIROBIOTICTMT HPLC Tīwae 250X4.6mm,5ul, roangaru rapunga, tere rere, rahi tauira:10 u L(tohutohu) kikokore: wai, wa kohinga raraunga :20.00min.
Te whakatau tauira: I wetewetehia te tauira i runga i te tikanga tauira e whai ake nei:1 ngira o te otinga patea me te 1 ngira o te tohutoro DL-phenylalanine.
1 wairewa tauira ngira,
Te Tatautanga Hua: Ko te ihirangi HPLC i whakatauhia kia iti iho i te 0.5% e ai ki te ahua o te waahi teitei me te tangohanga patea.
5. He maroke me te kore taumaha
5.1 Taputapu:
Umu whakamaroke Thermostatic, 1/10,000 toenga.
5.2 Tikanga:
I roto i te pounamu pauna he rite tonu te taumaha me te whakamaroke o te waha o te waha o te whenua, paunatia te 1 karamu (tika ki te 0.0001 karamu) o te tauira.Ko te tauira kia horahia ki raro o te pounamu pauna me te matotoru kaua e neke atu i te 10mm, ka maka ki roto i te oumu whakamaroke hiko whakamaroke, whakamaroke ki te 105-110 ℃ mo te 3 haora, katahi ka neke ki roto i te ruma whakamaroke ki te whakamatao te pāmahana rūma mo te pauna.
Tātaitanga: Te mate taimaha maroke %= (M1-M2) ÷M×100
Kei hea: M1: te papatipu tauira me te pounamu ine i mua i te whakamaroke, karamu
M2: Te papatipu o te tauira me te pounamu ine i muri i te whakamaroketanga, ki te karamu
M: Tauira papatipu, karamu
Hipanga 6: Ihirangi
6.1 Taputapu
Ko te chromatography wai mahi teitei, te kaitirotiro PDA.
Taurite tātari hiko
6.2 Reagents
Acetonitrile (kōeke chromatographic), TFA(kōeke chromatographic)
6.3 Tikanga Chromatographic
6.3.1 Tīwae: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Te roangaru rapu: INC220nm
Rere Rere :1.0mL/min
Rahi tauira: 10μL(mo te tohutoro)
He angiangi: Acetonitrile
Te wa kohikohi raraunga: 20.00min
6.4 Whakaritenga wahanga pūkoro
Waahanga pūkoro A (0.1% te wai waikawa trifluoroacetic): te whakauru tika 2. Whakakorehia te waikawa trifluoroacetic Oml ki te wai ki te 2000m1, uru pai, me te degas;
Wāhanga pūkoro B(0.1% acetonitrile trifluoroacetic acid): te absorption pū 2.Oml trifluoroacetic acid was diluted to 2000m1 with acetonitrile, mixed and deggated;
6.5 Hotaka rōnaki wāhanga pūkoro
Wā (min) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Te whakarite tauira otinga
Paunatia me te whakakore i te tauira 0.1g me te acetonitrile, waimeha ki te 100m1, ruru pai mo te whakamahi, kia rite ranei te kukū.Whakaritea kia rua nga tauira hei whakarara.
6.7 Tauira Whakatau
Tātarihia te tauira kia rite ki te tikanga tauira e whai ake nei:
Neke atu i te 1 werohanga o te otinga patea
1 wairewa tauira ngira 1#
1 wairewa tauira ngira 2#
6.8 Te Tatautanga Hua
2.8.1 I whakamahia te tikanga whakatikatika rohe tihi ki te tatau i te pokekore o te HPLC ma te tango i te waahi tuwhera.
2.8.2 Kaua e nui ake i te 1%.
2.8.3 Mena ka tutuki nga hua o nga werohanga e rua ki nga paearu whakaae, ka riro te maatanga toharite hei hua whakamutunga.