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

1. Chitarisiko-- Kuongorora kwekuona
2. Kutenderera chaiko-- Kutenderera chaiko kunoyerwa zvinoenderana neGB/T613-1988
Kugadzirira kwemuenzaniso: Nyatsoyera 0.5000g sampuli uye woifambisa kune yakachena uye yakaoma 50ml volumetric bhodhoro, wedzera 20ml mvura, vhara bhodhoro, rizununguse kuti rinyunguduke, uye wobva warideredza pachiyero nemvura.
Muedzo: Gadzirisa zero yegyroscope isati yaedzwa, wobva waisa chubhu yebvunzo nemhinduro yemuenzaniso, rekodha Angle yekutenderera, uye verenga kutenderera chaiko kwesample neinotevera formula.
[а]D20 = (r×50) ÷(L×W)
Kupi:
[а]D20: Yakananga optical kutenderera pa20 ℃ yemuenzaniso mhinduro
r: Kutenderera kweOptical kunoonekwa pa20 ℃ kune mhinduro yemuenzaniso
50: Vhoriyamu yeyakagadzirirwa sampuli mhinduro (ml)
w: uremu hwemuenzaniso (g)
L: Optical kutenderera chubhu kureba (dm)
3. Kupisa zvisaririra
Tora inenge 1g yechigadzirwa ichi uye upise pa600 ℃, upise kusvika yave dota zvachose maererano nemutemo weAppendix Ⅷ N yeChikamu II cheCP2010 Edition, wedzera 0.5-1.0ml yakagadziriswa sulfuric acid uye inopisa (700 ℃ - 800 ℃) kuhuremu hunogara huripo.
3.1 "Incandescent residue" muNzira iyi (Chinese Pharmacopoeia 2005 Edition, Chikamu II Appendix Ⅷ N) inoreva masimbi oxides kana sulfates anosara mushure mokunge mishonga (kunyanya organic compounds) yapisa kusvikira madota akazara, ipapo sulfuric acid inowedzerwa 0.5 ~ 1.0ml uye incandesced (700 ~ 800 ℃) kuti irambe ichirema.
4 Chiral kuchena (HPLC)
Zvishandiso: Yakakwira performance liquid chromatography, PDA detector.Electronic analytical balance, reagent;Nhamba yechromatography
Chromatographic mamiriro: Column: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm, 5ul, kuonekwa wavelength, kuyerera kwehuwandu, saizi yemuenzaniso :10 u L (referensi) yakaonda: mvura, nguva yekuunganidza data :20.00min.
Sample kutsunga: Sample yakaongororwa maererano neanotevera sampling maitiro: 1 tsono yemushonga usina chinhu uye 1 tsono yeDL-phenylalanine referensi.
1 tsono sampuli mhinduro,
Mhedzisiro Kuverengera: HPLC yemukati yakatemerwa kuve isingasviki 0.5% zvichienderana nepamusoro penzvimbo normalization uye isina kubviswa.
5. Yakaoma uye isina uremu
5.1 Zvishandiso:
Thermostatic drying oven, 1/10,000 chiyero.
5.2 Maitiro:
Mubhodhoro rehuremu rakafuratira rine huremu hunoramba huchiwedzera uye kuoma-kuoma kwevhu rakavhara muromo, kuyera 1 gramu (yakarurama kusvika 0.0001 gramu) yemuenzaniso.Sample inofanira kuparadzirwa zvakaenzana pazasi pebhodhoro rekuyeresa nehupamhi husingapfuure 10mm, isa muovheni yekuomesera yemagetsi, yakaoma pa105-110 ℃ kwemaawa matatu, uye wozoenda muimba yekuomesa kuti utonhorere. kamuri tembiricha yekuyera.
Kuverenga: Dry uremu kurasikirwa %= (M1-M2) ÷M×100
Ikoko: M1: huwandu hwesample uye bhodhoro rekuyeresa risati raoma, magiramu
M2: Misa yemuenzaniso uye bhodhoro rekuyeresa mushure mekuoma, mumagiramu
M: Sample mass, magiramu
Danho rechitanhatu: Zviri mukati
6.1 Zviridzwa
Yakakwira performance liquid chromatography, PDA detector.
Electronic analytical balance
6.2 Reagents
Acetonitrile (chromatographic giredhi), TFA (chromatographic giredhi)
6.3 Chromatographic Conditions
6.3.1 Koramu: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Kuona wavelength: INC220nm
Kuyerera kweyero: 1.0mL/min
Saizi yemuenzaniso: 10μL (yekutarisa)
Mutete: Acetonitrile
Nguva yekuunganidza data: 20.00min
6.4 Kugadzirira kwechikamu chenhare
Nharembozha chikamu A (0.1% trifluoroacetic acid mvura): kunyatsotora 2. Dilute Oml trifluoroacetic acid nemvura kusvika 2000m1, sanganisa zvakanaka, uye degas;
Nharembozha yechikamu B (0.1% acetonitrile trifluoroacetic acid): kunyatsotora 2.Oml trifluoroacetic acid yakaderedzwa kusvika 2000m1 neacetonitrile, yakasanganiswa uye yakasvibiswa;
6.5 Mobile chikamu gradient chirongwa
Nguva (miniti) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Kugadzirira kwemuenzaniso mhinduro
Weresa uye nyungudutsa 0.1g sampu ine acetonitrile, dilute kusvika 100m1, zunza zvakanaka kuti ushandiswe, kana iyo yakafanana fungidziro.Gadzirira sampuli mbiri dzakafanana.
6.7 Sample Kutsunga
Ongorora sampuli maererano neanotevera sampling maitiro:
Kupfuura jekiseni 1 remhinduro isina chinhu
1 tsono muenzaniso mhinduro 1#
1 tsono muenzaniso mhinduro 2#
6.8 Mhedzisiro Kuverenga
2.8.1 Peak area normalization nzira yakashandiswa kuverenga kuchena kweHPLC nekubvisa nzvimbo isina chinhu.
2.8.2 Iyo hama inoreva kutsauka kwekuchena kwetsono mbiri haifaniri kudarika 1%
2.8.3 Kana mhedzisiro yemajekiseni ese ari maviri akazadzisa maitiro ekugamuchirwa, avhareji yekuchena inotorwa semhedzisiro yekupedzisira.