D-Phenylalanine CAS 673-06-3 (HD-Phe-OH) Hōʻike 98.0~102.0% Hale Hana 50MT/Mahina

1. Nani-- Nana nana
2. Ho'ololi kiko'ī-- Ana 'ia ka ho'ololi kiko'ī e like me GB/T613-1988
Hoʻomākaukau laʻana: E kaupaona pololei i ka hāpana 0.5000g a hoʻoneʻe iā ia i kahi ʻōmole volumetric 50ml maʻemaʻe a maloʻo, e hoʻohui i ka wai 20ml, e uhi i ka ʻōmole, e hoʻoluliluli a hoʻoheheʻe ʻia, a laila e hoʻoheheʻe i ka paona me ka wai.
Ho'āʻo: E hoʻololi i ka zero o ka gyroscope ma mua o ka hoʻāʻo ʻana, a laila e hoʻouka i ka paipu hoʻāʻo me ka hāpana hāpana, e hoʻopaʻa i ka Angle rotation, a helu i ka ʻōwili kikoʻī o ka hāpana me ke ʻano ma lalo.
[a]D20 = (r×50) ÷(L×W)
Ma hea:
[a]D20: Ka huli ʻana o ka ʻike maka ma 20 ℃ o ka hāpana hāpana
r: ʻIke ʻia ka huli ʻana ma 20 ℃ no ka hāpana hāpana
50: Ka nui o ka hāpana hāpana i hoʻomākaukau ʻia (ml)
w: Kaumaha laʻana (g)
L: ʻO ka lōʻihi o ka paipu hoʻololi ʻana (dm)
3. Puhi koena
E lawe ma kahi o 1g o kēia huahana a wela iā 600 ℃, wela a hiki i ka lehu piha e like me ka hoʻoponopono o Appendix Ⅷ N o ka Māhele II o CP2010 Edition, e hoʻohui i ka 0.5-1.0ml concentrated sulfuric acid a wela iā ia (700 ℃- 800 ℃) i ke kaumaha mau.
3.1 "Ke koena incandescent" i kēia ʻano (Chinese Pharmacopoeia 2005 Edition, Part II Appendix Ⅷ N) e pili ana i nā mea hao a i ʻole sulfate i koe ma hope o ka hoʻomehana ʻia ʻana o nā lāʻau (ʻoi aku ka nui o nā mea kūlohelohe) a hiki i ka lehu, a laila hoʻohui ʻia ka sulfuric acid 0.5 ~ 1.0ml a incandesced (700 ~ 800 ℃) i ke kaumaha mau.
4 Hoʻomaʻemaʻe Chiral (HPLC)
Mea hana: High performance liquid chromatography, PDA detector.Ke kaulike analytical uila, reagent;Ka pae o ka chromatography
Nā kūlana Chromatographic: Column: Astec CHIROBIOTICTMT HPLC Column 250X4.6mm, 5ul, ka lōʻihi o ka nalu ʻike, kahe kahe, ka nui o ka laʻana: 10 u L(kuʻi) ʻoi aku ka lahilahi: wai, manawa hōʻiliʻili ʻikepili: 20.00min.
Hoʻoholo laʻana: Ua kālailai ʻia ka hāpana e like me ke kaʻina hana laʻana: 1 nila o ka solution blank a me 1 nila o ka DL-phenylalanine reference.
1 hāpana hāpana nila,
Ka helu ʻana i nā hopena: Ua hoʻoholo ʻia ka ʻike HPLC ma lalo o 0.5% e like me ka hoʻomaʻamaʻa ʻana o ka wahi kiʻekiʻe a me ka wehe ʻole ʻana.
5. Maloo a kaumaha ole
5.1 Nā mea kani:
ʻO ka umu hoʻomaloʻo Thermostatic, 1/10,000 koena.
5.2 Kaʻina hana:
I loko o ka omole kaumaha palahalaha me ka paona mau a me ka maloo nui o ka uhi waha o ka lepo, e kaupaona i 1 gram (pololei i ka 0.0001 gram) o ka laana.Pono e hohola ʻia ka hāpana ma lalo o ka ʻōmole kaupaona me ka mānoanoa ʻaʻole i ʻoi aku ma mua o 10mm, e hoʻokomo i loko o ka umu hoʻomaloʻo uila thermostatic, maloʻo ma 105-110 ℃ no 3 mau hola, a laila e neʻe i loko o ka lumi maloʻo e hoʻomaloʻo ai. lumi wela no ke kaupaona ana.
Heluhelu: Pohō kaumaha maloʻo %= (M1-M2) ÷M×100
Kahi: M1: ka nui o ka la'ana a me ke ana omole ma mua o ka malo'o 'ana, grams
M2: Ka nui o ka la'ana a me ke ana omole ma hope o ka maloo ana, ma ka grama
M: Laʻana nuipa, grams
KaʻAnuʻu Hana 6: Maʻiʻo
6.1 Mea Hana
Kiʻekiʻe hana wai chromatography, PDA detector.
Kaulike analytical electronic
6.2 Reagents
Acetonitrile (papa chromatographic), TFA (papa chromatographic)
6.3 Nā Kūlana Chromatographic
6.3.1 kolamu: YMC-ODS-AM, 5 μL, 150x4.6 mm
6.3.2 Ka lōʻihi nalu ʻike: INC220nm
Kawai kahe:1.0mL/min
Laʻana nui: 10μL (no ka ʻike)
ʻOi aku: Acetonitrile
Ka manawa ohi ʻikepili: 20.00min
6.4 Ka hoʻomākaukau ʻana o ka pae kelepona
Mobile pae A (0.1% trifluoroacetic waiʻakika): precision absorption 2. Dilute Oml trifluoroacetic acid me ka wai i 2000m1, hui maikai, a me ka degas;
Mobile phase B(0.1% acetonitrile trifluoroacetic acid): pololei absorption 2.Oml trifluoroacetic acid ua hoʻoheheʻe ʻia i 2000m1 me ka acetonitrile, hui ʻia a hoʻohaʻahaʻa ʻia;
6.5 Polokalamu gradient pae paʻalima
Manawa (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 Hoʻomākaukau i ka hāpana hāpana
Kauona a hoʻoheheʻe i ka laʻana 0.1g me ka acetonitrile, hoʻoheheʻe ʻia i 100m1, lulu maikaʻi no ka hoʻohana ʻana, a i ʻole ka manaʻo like.E hoʻomākaukau i ʻelua laʻana i ka like.
6.7 Hoʻoholo Laʻana
E noʻonoʻo i ka hāpana e like me ke kaʻina hana laʻana:
ʻOi aku ma mua o 1 hoʻoheheʻe ʻia o ka hopena blank
1 hāpana hāpana nila 1#
1 hāpana hāpana nila 2#
6.8 Helu Huahelu
2.8.1 Ua hoʻohana ʻia ke ʻano o ka hoʻomaʻemaʻe ʻana o ka ʻāpana kiʻekiʻe no ka helu ʻana i ka maʻemaʻe HPLC ma ka unuhi ʻana i kahi hakahaka.
2.8.2 ʻAʻole ʻoi aku ka nui ma mua o 1% ka ʻokoʻa o ka maʻemaʻe o nā nila ʻelua.
2.8.3 Inā hoʻokō nā hopena o nā injections ʻelua i nā koina ʻae, lawe ʻia ka maʻemaʻe maʻemaʻe ma ke ʻano he hopena hope loa.