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

1. Bayyanar-- Duban gani
2. Takamaiman juyawa-- Ana auna ƙayyadaddun juyawa daidai da GB/T613-1988
Shirye-shiryen samfurin: Daidai auna samfurin 0.5000g kuma motsa shi zuwa kwalban 50ml mai tsabta mai tsabta da bushe, ƙara ruwa 20ml, rufe kwalban, girgiza shi don narkewa, sa'an nan kuma tsoma shi zuwa sikelin da ruwa.
Gwaji: Daidaita sifilin gyroscope kafin gwajin, sannan ɗora bututun gwajin tare da maganin samfurin, yi rikodin kusurwar juyawa, kuma ƙididdige takamaiman juyawa na samfurin tare da dabara mai zuwa.
[a] D20 = (r×50) ÷(L×W)
Inda:
[a] D20: Takamaiman juyawa na gani a 20 ℃ na maganin samfurin
r: Juyawa na gani da aka lura a 20 ℃ don maganin samfurin
50: Girman maganin samfurin da aka shirya (ml)
w: Misalin nauyi (g)
L: Tsawon bututun juyawa na gani (dm)
3. Rago mai ƙonewa
Ɗauki kimanin 1g na wannan samfurin sai a daɗa shi a zafin jiki na 600 ℃, zazzage shi har sai ya zama toka kamar yadda ka'idar Shafi Ⅷ N na Part II na CP2010 Edition, ƙara 0.5-1.0ml concentrated sulfuric acid da kuma zafi shi (700 ℃-). 800 ℃) zuwa nauyi akai-akai.
3.1 "Sauran Incandescent" a cikin wannan Hanyar (Pharmacopoeia na kasar Sin 2005 Edition, Sashe na II Shafi Ⅷ N) yana nufin karfe oxides ko sulfates da suka rage bayan da kwayoyi (mafi yawan mahadi) suna mai tsanani har sai ash, sa'an nan kuma sulfuric acid an kara 0.5 ~ 1.0ml da incandesced (700 ~ 800 ℃) zuwa m nauyi.
4 Tsabtace Tsabtace (HPLC)
Kayan aiki: Babban aikin chromatography ruwa, mai gano PDA.Electronic Analytical balance, reagent;Matsayin chromatography
Yanayi na chromatographic: Rukunin: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm,5ul, tsayin tsayin tsinkaya, ƙimar kwarara, girman samfurin: 10 u L (magana) bakin ciki: ruwa, lokacin tattara bayanai: 20.00min.
Ƙaddamar da samfurin: An bincika samfurin bisa ga tsarin samfurin mai zuwa: 1 allura na bayani mara kyau da 1 allura na DL-phenylalanine.
1 samfurin maganin allura,
Lissafin sakamako: Abubuwan da ke cikin HPLC an ƙaddara su zama ƙasa da 0.5% bisa ga daidaitaccen yanki na kololuwa da cirewa mara kyau.
5. Bushewa da nauyi
5.1 Kayan aiki:
Tanda bushewar thermostatic, ma'auni 1/10,000.
5.2 Tsari:
A cikin kwalabe mai nauyi tare da madaidaicin nauyi da murfin bakin ƙasa mai bushewa, auna gram 1 (daidai zuwa gram 0.0001) na samfurin.Samfurin ya kamata a yada a ko'ina a kasan kwalban auna tare da kauri ba fiye da 10mm ba, a saka shi a cikin tanda bushewar wutar lantarki mai zafi, bushe a 105-110 ℃ na 3 hours, sa'an nan kuma matsawa cikin ɗakin bushewa don kwantar da hankali. zafin dakin don aunawa.
Lissafi: Busassun nauyi %= (M1-M2) ÷M×100
Inda: M1: yawan samfurin da kwalban aunawa kafin bushewa, grams
M2: Yawan samfuri da kwalbar aunawa bayan bushewa, a cikin grams
M: Samfurin taro, grams
Mataki 6: Abun ciki
6.1 Kayan aiki
Babban aikin chromatography ruwa, mai gano PDA.
Ma'aunin nazari na lantarki
6.2 Reagents
Acetonitrile (makin chromatographic), TFA (jin chromatographic)
6.3 Yanayi na Chromatographic
6.3.1 Rukunin: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Tsawon Gano: INC220nm
Yawan kwarara: 1.0ml/min
Girman samfurin: 10μL (don tunani)
Mai bakin ciki: acetonitrile
Lokacin tattara bayanai: 20.00min
6.4 Shirye-shiryen lokaci na wayar hannu
Wayar hannu lokaci A (0.1% ruwa mai trifluoroacetic acid): daidaitaccen sha 2. Dilute Oml trifluoroacetic acid da ruwa zuwa 2000m1, haɗuwa da kyau, da degas;
Wayar hannu B (0.1% acetonitrile trifluoroacetic acid): daidaitaccen sha 2.Oml trifluoroacetic acid an diluted zuwa 2000m1 tare da acetonitrile, gauraye da kuma lalata;
6.5 Shirin gradient lokaci na wayar hannu
Lokaci (min) A% B%
0.0090 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Shiri na samfurin bayani
Yi nauyi da narkar da samfurin 0.1g tare da acetonitrile, tsarma zuwa 100m1, girgiza da kyau don amfani, ko taro iri ɗaya.Shirya samfurori guda biyu a layi daya.
6.7 Samfurin Ƙaddamarwa
Yi nazarin samfurin bisa ga tsarin samfur mai zuwa:
Fiye da allura 1 na bayani mara kyau
Maganin samfurin allura 1 1#
Maganin samfurin allura 1 2#
6.8 Kididdigar sakamako
2.8.1 An yi amfani da hanyar daidaita yanayin yanki mafi girma don ƙididdige tsaftar HPLC ta hanyar cire sarari mara kyau.
2.8.2 Ma'anar ma'anar ma'anar tsarkin allura biyu ba za ta fi 1% ba.
2.8.3 Idan sakamakon alluran biyu sun cika ka'idojin yarda, ana ɗaukar matsakaicin tsafta azaman sakamako na ƙarshe.