D-Phenylalanine CAS 673-06-3 (HD-Phe-OH) Nyocha 98.0 ~ 102.0% Ụlọ ọrụ 50MT / ọnwa

1. Ọdịdị-- nlele anya
2. Ntugharị pụrụ iche-- A na-atụle ntụgharị dị iche iche dịka GB/T613-1988 si dị.
Nkwadebe ihe atụ: Jiri nlezianya tụọ ihe nlele 0.5000g ma bugharịa ya na karama volumetric 50ml dị ọcha ma kpọọ nkụ, tinye mmiri 20ml, kpuchie karama ahụ, gbanye ya ka ọ gbazee, wee gbanye ya na mmiri.
Nnwale: Gbanwee efu nke gyroscope tupu ule ahụ, wee buo tube ule ahụ na ngwọta nlele, dekọọ akụkụ ntụgharị, wee gbakọọ ntụgharị a kapịrị ọnụ nke nlele ahụ na usoro a.
[a]D20 = (r×50) ÷(L×W)
Ebe:
[а] D20: Ntugharị ngwa anya akọwapụtara na 20 ℃ nke ngwọta nlele
r: Ntugharị anya hụrụ na 20 ℃ maka ngwọta nlele
50: Mpịakọta nke ngwọta sample akwadoro (ml)
w: Nlereanya arọ (g)
L: Ogologo tube ntụgharị anya (dm)
3. Ihe fọdụrụ na-ere ọkụ
Were ihe dị ka 1g nke ngwaahịa a wee kpoo ya na 600 ℃, kpoo ya ruo mgbe ọ ga-abụ ntụ zuru oke dịka ụkpụrụ nke ihe mgbakwunye Ⅷ N nke akụkụ II nke mbipụta CP2010, tinye 0.5-1.0ml concentrated sulfuric acid na kpoo ya (700℃- 800 ℃) na ịdị arọ mgbe niile.
3.1 "Incandescent residue" na usoro a (Chinese Pharmacopoeia 2005 Edition, Part II Appendix Ⅷ N) na-ezo aka na metal oxides ma ọ bụ sulfates fọdụrụ mgbe ọgwụ (ọtụtụ ogige organic) na-ekpo ọkụ ruo mgbe ash, mgbe ahụ, sulfuric acid na-agbakwunye 0.5 ~ 1.0ml na incandesced (700 ~ 800 ℃) na-adị arọ mgbe nile.
4 Chiral ịdị ọcha (HPLC)
Ngwa: chromatography mmiri na-arụ ọrụ dị elu, ihe nchọpụta PDA.Eletrọnịkị nyocha itule, reagent;Ọkwa nke chromatography
Ọnọdụ Chromatographic: Kọlụm: Astec CHIROBIOTICTMT HPLC Kọlụm 250X4.6mm,5ul, ogologo ogologo oge nchọpụta, ọnụego nrịba, nha nha: 10 u L (ntụgharị aka) thinner: mmiri, oge nchịkọta data: 20.00min.
Nnwale mkpebi siri ike: A na-enyocha ihe nlele ahụ dị ka usoro nlele ndị a si dị: 1 agịga nke ngwọta efu na 1 agịga nke DL-phenylalanine.
1 agịga sample ngwọta,
Mgbakọ nsonaazụ: Achọpụtara ọdịnaya HPLC ka ọ na-erughị 0.5% dabere na nhazi mpaghara kacha elu yana mwepu oghere.
5. Akọrọ na enweghị ibu
5.1 Ngwa:
Igwe ọkụ ọkụ ọkụ, nguzozi 1/10,000.
5.2 Usoro:
N'ime karama na-atụ ihe dị larịị nke nwere ịdị arọ mgbe niile yana mkpuchi ọnụ ala na-akpọnwụ, tụọ gram 1 (nke ruru 0.0001 gram) nke nlele.Ekwesịrị ịgbasa ihe nlele ahụ n'otu n'otu na ala nke karama na-atụ ya na ọkpụrụkpụ nke na-erughị 10mm, tinye ya na oven ọkụ ọkụ ọkụ, kpoo na 105-110 ℃ maka awa 3, wee banye n'ime ụlọ ihicha ka ọ dị jụụ. ọnụ ụlọ okpomọkụ maka ịtụ.
Ngụkọta: Mbelata arọ akọrọ %= (M1-M2) ÷M×100
Ebe: M1: uka nke sample na karama atụ tupu ihicha, gram
M2: Mass nke sample na karama atụ mgbe akpọchara, na gram
Nna-ukwu: Ihe atụ, gram
Nzọụkwụ 6: Ọdịnaya
6.1 Ngwa
chromatography mmiri mmiri na-arụ ọrụ dị elu, ihe nchọpụta PDA.
Ntụle nyocha eletrọnịkị
6.2 Reagent
Acetonitrile (ọkwa chromatographic), TFA (ọkwa chromatographic)
6.3 Ọnọdụ Chromatographic
6.3.1 Ogidi: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Ogologo nchọta: INC220nm
Ọnụego mmiri: 1.0ml/min
Nlele nha: 10μL (maka ntụaka)
Nke dị mkpa: acetonitrile
Oge nchịkọta data: 20.00min
6.4 Mobile usoro nkwadebe
Usoro mkpanaka A (0.1% mmiri trifluoroacetic acid): nnabata ziri ezi 2. Dilute Oml trifluoroacetic acid na mmiri na 2000m1, jikọta nke ọma, na degas;
Usoro mkpanaaka B (0.1% acetonitrile trifluoroacetic acid): absorption ziri ezi 2.Oml trifluoroacetic acid e diluted na 2000m1 na acetonitrile, agwakọta na deggated;
6.5 Mmemme gradient usoro mkpanaaka
Oge (nkeji) A% B%
0.00 90 10
12.00 10 90
15.00 10 90
15.01 90 10
20.00 90 10
6.6 Nkwadebe nke ngwọta sample
Tuo ma gbarie 0.1g sample na acetonitrile, itughari ka 100m1, maa jijiji nke ọma maka ojiji, ma ọ bụ otu itinye uche.Kwadebe ihe atụ abụọ n'otu aka ahụ.
6.7 Mkpebi nlele
Nyochaa ihe nlele ahụ dịka usoro nlele ndị a si dị:
Ihe kariri ogwu ogwu efu 1
1 ihe ngwọta nke agịga 1 #
1 ihe ngwọta nke agịga 2 #
6.8 Mgbakọ nsonaazụ
2.8.1 A na-eji usoro nhazi nke mpaghara kacha elu iji gbakọọ ịdị ọcha HPLC site n'iwepụ oghere oghere.
2.8.2 Ntugharị ikwu nke ịdị ọcha nke agịga abụọ agaghị adị karịa 1%
2.8.3 Ọ bụrụ na nsonaazụ nke injections abụọ ahụ na-agbaso ụkpụrụ nnabata, a na-ewere nkezi ịdị ọcha dị ka nsonaazụ ikpeazụ.